The modification of NCM cathode material prepared by hydrothermal method under pulsed high magnetic field

The modification of NCM cathode material prepared by hydrothermal method under pulsed high magnetic field | 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 The modification of NCM cathode material prepared by hydrothermal method under pulsed high magnetic field Wenrui Sun, Genwen Lin, Xueqian Zhang, Hongming Jin, Mingyuan Zhu, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-5443801/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract High magnetic field serves as a unique technique for the materials preparation which is more applied in the magnetic materials, but seldom in the electrode materials. In this study, the pulsed high magnetic field was employed during the hydrothermal synthesis of the NCM523 precursor. And the electrochemical performances of NCM523 are researched: at a high cut-off voltage range from 3V to 4.5V and current density set at 1C = 180 mA/g, an initial specific discharge capacity is 190.4 mAh/g which is 12.1 mAh/g increased, and after 200 cycles both specific discharge capacity and capacity retention rate increased by 24.4 mAh/g and 8.5%, respectively, comparing to the sample prepared without magnetic field. The mechanism should be that the high magnetic field applied in the formation and growth of NCM crystal could improve its micro-structure such as layer structural, result in the mitigate Li + /Ni 2+ mixed-arrangement phenomenon and increase the Li + diffusion rate. Pulsed high magnetic field hydrothermal method NCM523 High voltage Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 1. Introduction As a typical cathode material, LiNi 0.5 Co 0.2 Mn 0.3 O 2 (NCM523) has become commonly commercial materials because of its high energy density, low cost, etc [ 1 – 4 ]. However, the NCM523 cathode material also faces several challenges. Firstly, it suffers from severe cationic mixing, because the radius of Ni 2+ (0.069 nm) and Li + (0.076 nm) is close, that Ni 2+ could easily occupy the position of Li + during charge and discharge processes [ 5 ]. Secondly, the lithium-ion transfer rate remains relatively low. The rate of lithium-ion transport is associated with the particle diameter. The larger the particle diameter, the fewer surfaces exposed that are favorable for Li + transport. Thirdly, its cycle performance is subpar. Especially, during the high-voltage charging process, NCM523 may undergo an irreversible phase transformation from a layered structure (R-3m) to a spinel-like (Fd-3m) or a rock-salt phase (Fm-3m) structure. This phase transition is typically accompanied by an abrupt change in lattice volume, leading to structural degradation and the formation of crack [ 6 , 7 ]. Currently, in order to solve the aforementioned issues, there are various methods such as ion doping [ 8 , 9 ], surface coating [ 10 – 12 ], special structural design [ 13 , 14 ] and material preparation techniques. These approaches have yielded favorable outcomes. However, to further enhance the electrochemical performance, employing specialized approaches is necessary. The utilization of a high magnetic field to obtain superior capabilities of lithium batteries has emerged as a novel method over the past two decades [ 15 ]. For instance, Zhou [ 16 ] and Kim [ 17 ] et al. obtained B-axis oriented lithium iron phosphate cathode materials by applying a magnetic field during the preparation of cathode slurry. Compared to non-magnetically oriented LiFePO 4 counterparts, incorporating a magnetic field increased lithium-ion diffusion rate and reduced electrode polarization. After mixing NCM precursor with conductor and adhesive materials, Kim [ 18 ] et al. used an external magnetic field to control the crystal alignment of LiNi 0.5 Co 0.2 Mn 0.3 O 2 so that Li + mainly moves along (00l) plane during the transmission process. This greatly improves the transmission rate of Li + ions, which can enhance the specific capacity and rate performance of NCM523 cathode material. These above examples demonstrate the effectiveness of applying a high magnetic field in the preparation of electrode slurries. Therefore, further investigation into the impact of high magnetic fields on the synthesis of electrode materials is necessary. In this study, the precursor of LiNi 0.5 Co 0.2 Mn 0.3 O 2 was synthesized by hydrothermal method under pulsed high magnetic field. In order to research the properties enhancement of NCM523 material which is prepared under high magnetic field, electrochemical tests (CV, EIS, etc.) and physicochemical characterization (XRD, SEM, EDS, XPS) were carried out. 2. Experimental 2.1 Material preparation The precursor Ni 0.5 Co 0.2 Mn 0.3 CO 3 was synthesized by a hydrothermal reaction under pulsed high magnetic field. Firstly, Ni(CH 3 COO) 2 ·4H 2 O、Co(CH 3 COO) 2 ·4H 2 O、Mn(CH 3 COO) 2 ·4H 2 O were dissolved in deionized water with a molar ratio of 5:2:3, and added CTAB and vitamin C. The solution was stirred for 20 minutes, which is called solution A. The solution A was putted into an ice-water bath and added Na 2 CO 3 solution drop by drop at intervals of 5 s to obtain the solution B with the magneton speed of 600 r/min. The solution B was ultrasonicated for 30 min and then stirred at 700 r/min for 1 h. Subsequently, it was placed in the autoclave lined by PTFE with 80% filling volume. The autoclave was placed into the pulsed high magnetic field. The hydrothermal temperature was set to 180 ℃ and magnetic field intensity was 3 T with the 20 s interval of pulsed magnetization. After reaction for 12h, the reactant was removed. Then the reactant was ultrasonicated and stirred for a while. After pumping, filtering and washing the precipitation for several times, the precipitate was obtained. Finally, the precipitate was dried under 80 ℃ for 24 h to produce Ni 0.5 Co 0.2 Mn 0.3 CO 3 precursor. Comparison sample was prepared non-magnetic field. The precursors obtained with and without pulsed magnetic field were labeled as T-Precursor and P-Precursor. LiNi 0.5 Co 0.2 Mn 0.3 O 2 cathode material was synthesized by high-temperature solid-state reaction. The Precursors were mixed with a certain amount of Li 2 CO 3 (Li excess 5%). After mechanically grounding evenly, the mixtures were transferred to a tubular furnace, heated in an oxygen atmosphere with a temperature rise rate of 3 ℃/min and maintained at 300 ℃ for 1h, 500 ℃ for 6h, 870 ℃ for 12h. Upon cooling of the tubular furnace to room temperature, the final products were fully ground using the mortar. The LiNi 0.5 Co 0.2 Mn 0.3 O 2 prepared from T-Precursor and P-Precursor was labeled as T-NCM523 and P-NCM523, respectively. 2.2 Material characterization The crystal structure of the samples was analyzed using X-ray diffraction (XRD, Rigaku smartlab 9) with scattering angle 2θ in the range of 10–80° and scanning rate of 2°/min. Field emission scanning electron microscopy (FE-SEM, Sigma 300) coupled with energy dispersive spectroscopy (EDS, Oxford Xplore 30) was used to examine the micro-morphology and elemental distribution of the prepared samples. X-ray photoelectron spectroscopy (XPS, Thermo Scientific K-Alpha) was employed to detect the surface chemical composition of the samples. 2.3 Electrochemical measurements The CR2016 coin cells were self-assembled in an argon-filled glove box and tested for their electrochemical performance. The cathode slurry consisted of 80% active material, 10% carbon black and 10% polyvinylidene fluoride (PVDF) uniformly dispersed in N-methyl-2-pyrrolidone (NMP), and then the mixture was coated on aluminum foil and dried in a vacuum oven at 80℃ for 12 h. The electrolyte was 1 mol·L − 1 LiPF 6 solution in a mixture of ethylene carbonate (EC), dimethyl carbonate (DMC), and ethylene methyl carbonate (EMC) (1:1:1, v/v/v). Celgard 2500 microporous polypropylene membrane served as the separator, and lithium metal served as the anode. The cathode, electrolyte, separator and anode were assembled into a cell in a glove box under H 2 O and O 2 atmosphere both less than 0.01 ppm. The cells were charged and discharged on a Land CT2001A device (China) at a balanced current in the voltage range of 3-4.5 V. In the electrochemical workstation (CHI 660E, CH Instruments), a cyclic voltammetry (CV) test was conducted at a voltage sweep rate of 0.1 mV/s, and an electrochemical impedance spectroscopy (EIS) test was performed in 0.01–105 Hz. 3. Results and discussion 3.1 Structure and morphology The XRD patterns of NCM523 cathode materials prepared with and without magnetic field have been shown in Fig. 1 . The diffraction peaks of T-NCM523 and P-NCM523 are shar, which indicates that the two samples have high crystallinity. And the XRD patterns of the two samples are matched with the standard card PDF#74–0919 [ 19 ], with the hexagonal α-NaFeO 2 layered structure of R-3m space group, which suggests that applying external magnetic field does not change the crystal structure. Additionally, no peaks corresponding to extraneous impurities were detected in either sample, which also means that they do not contain other impurity phases [ 20 ]. Furthermore, the clear split peaks between (006)/(012) and (108)/(110) also confirm the layer structure of the both samples [ 4 , 21 , 22 ]. The lattice parameters of T-NCM523 and P-NCM523 calculated from the XRD patterns were listed in Table 1 . The values of the lattice parameter c/a for both samples are above 4.9, which proves the presence of a well-defined layer structure. And the c/a ratio of T-NCM523 is slightly higher than that of the P-NCM523, which indicates that the sample prepared under the magnetic field has a better layer structure. Furthermore, it is well known that the intensity ratio between (104) and (003) is a reliable parameter for evaluating the cation mixing, i.e., the I 003 /I 104 ratio higher than 1.2 often indicates that the material has a low Li + /Ni 2+ cation mixing. A higher c/a ratio indicates lower cation mixing [ 23 ]. The I 003 /I 104 intensity ratios of T-NCM523 and P-NCM523 are 1.5596 and 1.2129, respectively, which are both above 1.2. And the ratio of T-NCM523 is higher than that of P-NCM523, which means that the NCM523 prepared under the high magnetic field has a lower cation mixing. Table 1 XRD Rietveld refinement results of T-NCM523 and P-NCM523 Sample a (Å) c (Å) c/a I (003) /I (104) T-NCM523 2.8680 14.2238 4.9595 1.5596 P-NCM523 2.8677 14.2158 4.9572 1.2129 In order to further observe the influence of magnetic field on the microscopic morphology of the NCM523 cathode material, SEM was employed to examine the precursors and final products, as shown in Fig. 2 . Figure 2 (a) and 2 (b) are the micro-morphology of T-Precursor and P-Precursor, and it could be seen that both samples are composed of many secondary particles, which are aggregated from fine spherical particles with diameters in the range of tens of nanometer. Comparing the two samples, the T-Precursor sample has smaller primary particle and more uniform. This is the result that during the hydrothermal reaction process, the high magnetic field provides energy for the nucleation and growth of precursors [ 24 ], which facilitates the formation of fine and homogeneous crystal nucleus and inhibits the rapid growth of them by affecting the charged particles in the solution. Figure 2 (c) and 2 (d) show the morphology of T-NCM523 and P-NCM523. Both samples have irregular polyhedral shapes and smooth surface. As well, the particle size of P-NCM523 is approximately double of T-NCM523. The small and uniform primary size of the T-NCM523 is also maintained after lithiation and sintering, which suggests that applying a high magnetic field facilitates the reduction of materials size in the process of the cathode material preparation [ 25 ]. Figure 3 shows the EDS maping/line scan results of T-NCM523 and P-NCM523 samples. From these results, the uniform distribution of Ni, Co and Mn on the surface of the two samples was observed. From the comparison of the line scan results of the two samples, it is concluded that the elements distribution on the surface of the T-NCM523 is more homogeneous than that of the P-NCM523. Under the high magnetic field, the magnetic stirring makes the charged particles of Ni, Co and Mn magnetic elements more uniformly distributed during the precursor formation, which is also conducive to the stability of the LiNi 0.5 Co 0.2 Mn 0.3 O 2 cathode material. X-ray photoelectron spectroscopy (XPS) was employed to investigate the effect of pulsed magnetic field on the valences of transition metal elements in LiNi 0.5 Co 0.2 Mn 0.3 O 2 . The XPS test results of T-NCM523 and P-NCM523 samples are presented in Fig. 4 . According to the C1s peak (284.80 eV), the electron binding energy of each detected element was calibrated, and the fine spectrum of detected elements was fitted and analyzed using Avantage software. It can be seen from the full spectrum of the two samples in Fig. 4 (a), T-NCM523 and P-NCM523 have similar XPS spectra. And the characteristic peaks of Ni, Co and Mn are obvious. Figure 4 (b) presents the fitted Ni 2p orbital spectra for both samples. The peaks of 879.40, 873.24, 860.83, 856.56, 855.20 eV electron binding energy correspond to the Ni 2p1/2 satellite peak orbit, Ni 2p1/2 orbit, Ni 2p3/2 satellite peak orbit, Ni 3+ 2p3/2 and Ni 2+ 2p3/2 orbits, respectively [ 26 , 27 ]. The Ni element exists in both samples in + 2 and + 3 valence forms, but the relative content of Ni 2+ in the T-NCM523 sample is reduced by 3.48%, which indicates that the application of the pulsed high magnetic field reduces the Li + /Ni 2+ cation mixing behavior, in accordance with the test results of XRD. From Fig. 4 (c), according to the fitting results of Co 2p orbitals, the electronic binding energies of Co 2p1/2 and Co 2p3/2 orbitals are 796.12 and 780.79 eV, respectively, indicating that Co exists in the form of + 3 valence [ 28 ].Moreover, Fig. 4 (d) illustrates the fitting results for the fine spectra of Mn 2p orbitals. The peaks of 654.21, 643.15, 641.98, 637.73eV electron binding energy correspond to the Mn 2p1/2, Mn 4+ 2p3/2, Mn 3+ 2p3/2, and Mn 2p3/2, and the elemental Mn was determined to be + 3 and + 4 valences. The relative content of Mn 4+ in T-NCM523 samples increased by 11.11%, which was conducive to inhibiting J-T distortion and stabilizing the crystal structure of LiNi 0.5 Co 0.2 Mn 0.3 O 2 material [ 29 , 30 ]. 3.2 Electrochemical properties Figure 5 shows the initial charge-discharge curves, rate capacity, and cycle performance of T-NCM523 and P-NCM523 at 1C (1C = 180 mA/g), 3-4.5V high cut-off voltage, respectively. The data presented in Fig. 5 are provided in Table 2 . The first cycle charge/discharge specific capacities of T-NCM523 are 228.3 mAh/g and 187.5 mAh/g, respectively. And the Coulombic efficiency is 82.1%. The first cycle charge/discharge specific capacities of the P-NCM523 sample are 221.6 mAh/g and 178.3 mAh/g, respectively, within an initial Coulombic efficiency is 80.5%. Compared to the sample prepared without the magnetic field, T-NCM523 exhibits an improvement in initial discharge capacity by 9.2 mAh/g and an increase in Coulombic efficiency by 1.6%. These findings implies that NCM523 prepared under the high magnetic field has higher discharge specific capacity and coulombic efficiency. Table 2 Initial charge-discharge specific capacities and columbic efficiency of the T-NCM523 and P-NCM523 at 1C. Samples Charge capacity (mAh/g) Discharge capacity (mAh/g) Irreversible capacity loss (mAh/g) Coulombic efficiency (%) T-NCM523 228.3 187.5 40.8 82.1 P-NCM523 221.6 178.3 43.3 80.5 Figure 6 (a) is the rate performance of the two samples (0.1 C = 18 mA/g, 0.2 C = 36 mA/g, 0.5 C = 90 mA/g, 1 C = 180 mA/g, and 5 C = 900 mA/g). With increasing current density, the discharge-specific capacity of both samples exhibits a declining trend, and P-NCM523 has an even more significant decrease. At 0.1 C rate, the discharge specific capacities of T-NCM523 and P-NCM523 reached 220.7 mAh/g and 199.5 mAh/g, respectively. As the current density was increased, the discharge-specific capacity of T-NCM523 decreased less than that of P-NCM523 by 24.3 mAh/g at 1 C. The T-NCM523 is 43.0 mAh/g above the P-NCM523 at the current density of 5 C. Because, under the high current density, obstructed by the influence of the electrode/electrolyte interface and the viscosity of the electrolyte, etc. Li + is difficult to migrate quickly to the electrode surface and participate in the reaction, which makes the battery capacity decrease [ 31 – 33 ]. And owing to the better layer structure and smaller particle size of the NCM523 prepared under magnetic field, the exposed surface favorable for Li + transport is increased and the transport distance is shortened, which provides a fast Li + transport channel. Thus it can be compensating for some of the rate difference, which causes the decrease is slighter than that of the original sample [ 34 ]. Upon the current density reaching 0.1 C again after 31 cycles, the discharge specific capacity of both samples closely matches their initial values, indicating good reversibility for both materials. Figure 6 (b) illustrates the cycle performance of the two samples, which is evaluated at a high cut-off voltage range of 3.0–4.5 V and 1 C. The corresponding data for Fig. 6 (b) is listed in Table 3 . The initial discharge-specific capacities of the T-NCM523 and P-NCM523 were 190.4 mAh/g and 178.3 mAh/g, respectively. After 200 cycles, the discharge capacity of P-NCM523 declined to 122.9 mAh/g, and a capacity retention rate is 68.9%. In contrast, T-NCM523 exhibited a discharge capacity of 147.3 mAh/g and a capacity retention rate of 77.4%, which is 8.5% higher than that of P-NCM523.The initial discharge-specific capacity and cycle stability of T-NCM523 are both higher than that of P-NCM523. Table 3 Cycle performance of the T-NCM523 and P-NCM523 at 3.0-4.5 V under 1 C. Samples Initial discharge capacity (mAh/g) Discharge capacity after 200 cycles (mAh/g) Irreversible capacity loss (mAh/g) Capacity retention after 200 cycles(%) T-NCM523 190.4 147.3 43.1 77.4 P-NCM523 178.3 122.9 55.4 68.9 For further evaluating the electrochemical reaction reversibility and Li + transport ability, Cyclic Voltammetry (CV) and Electrochemical Impedance Spectroscopy (EIS) were performed. Figure 7 (a) and 7 (b) show the CV curves of T-NCM523 and P-NCM523. Both curves present a pair of redox peaks corresponding to Ni 2+ /Ni 4+ interconversion, and the absence of other peaks suggests that within the tested voltage range, the current is derived from the valence change of nickel ions, and the electrochemical reaction is reversible [ 35 ]. It also suggests that the crystal structure is relatively stable. During the first charging and discharging cycles of the battery, the electrolyte and electrode react at the solid/liquid two-phase interface to form a passivating surface layer covering the electrode material (solid electrolyte SEI layer). The formation and growth of SEI film, decomposition of electrolyte and other side reactions lead to electrode polarization, which makes a potential difference (expressed as △E) exists between the Ni 2+ /Ni 4+ peaks. Therefore, the △E value is reflected the degree of electrode polarization. The smaller the △E value, the lower the electrode polarization and the better the reversibility [ 7 ]. As it can be seen from the Fig. 6 , the ΔE 3 (△E 3 represents the third cycle of △E)value of T-NCM523 was 0.191, while that of P-NCM523 was 0.264. This indicates that the NCM523 prepared under the pulsed high magnetic field has lower electrode polarization and the better reversibility, which also leads to better cycling stability as well as rate performance. After 150 cycles within 3.0-4.5 V at 1C, the impedance of two samples was tested, as depicted in Fig. 8 (a) and 8 (b). The Nyquist plot was fitted using Zview software. And the corresponding equivalent circuit model is also shown in Fig. 8 (a). The plot in Fig. 8 (a) consists of two semi-circles and a sloped line. The semicircle in the high/middle-frequency region represents the SEI film resistance and charge transfer resistance (R f and R ct ) on the cathode material surface, respectively. While the intersection point of the semicircle with the horizontal axis represents the electrolyte resistance R s , and the sloped line (the Warburg curve) is associated with the Li + transport rate [ 36 ]. After 150 cycles, due to the side reaction between the electrolyte and the cathode material under high voltage, the R f and R ct values of both samples are high, in which the surface film impedance (R f ) of the P-NCM523 is 311.5 Ω, which is much higher than that of 191.3 Ω of the T-NCM523(See Table 4 for details). In addition, the charge transfer resistance (R ct ) of the T-NCM523 is reduced by 63.5% compared to the P-NCM523, which implies less internal energy consumption, the superior cycle and rate performance. The Li + diffusion coefficient (D) is calculated by the equations ( 1 ) and ( 2 ), as follows [ 37 ]: $$\:D=\frac{{R}^{2}{T}^{2}}{2{A}^{2}{n}^{4}{F}^{4}{C}^{2}{\sigma\:}^{2}}$$ 1 $$\:{Z}^{{\prime\:}}={R}_{s}+{R}_{ct}+\sigma\:{\omega\:}^{-1/2}$$ 2 Where R is the constant (8.314 J/mol K), T represents the absolute temperature (298 K), A represents the surface area of the positive electrode plate (1.767 cm 2 ), n is the number of electrons involved in the redox reaction (n = 1), and C represents the concentration of lithium ions per unit volume (7.818×10 − 4 mol/cm 3 ). F is the Faraday constant (96485.3 C/mol) and σ refers to the Warburg factor, which can be derived by linear fitting the slope from Z'-ω −1⁄2 in Fig. 7 (b) according to the formula (1–2) [38] . Table 4 EIS parameters of P-NCM523 and T-NCM523 after 150 cycles Samples R s (Ω) R f (Ω) R ct (Ω) D *10 10 (cm 2 /s) P-NCM523 8.06 311.5 168.40 1.51 T-NCM523 11.28 191.3 61.41 6.25 The calculations from the above equations are only used for qualitative analysis due to the difficulty in calculating the lithium-ion concentration C. The lithium-ion diffusion coefficients D of T-NCM523 and P-NCM523 are 6.25 × 10 − 10 cm 2 /s and 1.51 × 10 − 10 cm 2 /s, respectively. T-NCM523 cathode material has a bigger lithium-ion diffusion coefficient. Because of the application of pulsed high magnetic field, the nucleation rate of the cathode material increases during the hydrothermal reaction, and the primary particle size decreases. The obtained cathode material has a relatively larger specific surface area, which exposes more crystal faces conducive to lithium-ion transport. Meanwhile, the low cation mixing facilitates the reversible de-embedding/embedding of Li + , and the better layer structure provides an efficient diffusion pathway for Li + in the interior of the material. As a result, the cathode material exhibits lower electrochemical impedance and higher Li-ion diffusion coefficient, that is consistent with the superior electrochemical performance of the previous T-NCM523. 4. Conclusions The LiNi 0.5 Co 0.2 Mn 0.3 O 2 cathode material synthesized by hydrothermal method under the pulsed high magnetic field has higher Li + diffusion coefficient, better cycle and rate performance comparing to the NCM523 prepared without the high magnetic field. This is attributed to its smaller particle size, the better layer structure and the lower Li + /Ni 2+ cation mixing. The smaller particle size has more exposed surface that favors Li + transport and shortens the Li + transport distance, and the better layer structure provides the lower degree of tortuosity for Li + transport and reduces the electrode polarization. All these increase the Li + diffusion coefficient. The lower Li + /Ni 2+ cation mixing favors the reversible de-embedding/embedding of Li + , which improves the specific charge/discharge capacity, the cycle and rate performances. Declarations Declaration of competing interest The authors have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. Declaration of Funding No funding was received for conducting this study. Author contribution All authors were involved in the conception and design of the study. Conceptualization, Methodology, Data curation, Writing, Visualization, Investigation, Reviewing and Editing: WR Sun. Reviewing, Editing: GW Lin. 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Surface modification of LiNi 0.5 Co 0.2 Mn 0.3 O 2 cathode materials with Li 2 O-B 2 O 3 -LiBr for lithium-ion batteries [J]. International Journal of Energy Research, 2019, 43(9): 4644–51. http://dx.doi.org/https://doi.org/10.1002/er.4601 Zuo C, Hu Z, Qi R, et al. Double the Capacity of Manganese Spinel for Lithium-Ion Storage by Suppression of Cooperative Jahn–Teller Distortion [J]. Advanced Energy Materials, 2020, 10(34): 2000363. http://dx.doi.org/https://doi.org/10.1002/aenm.202000363 Capsoni D, Bini M, Chiodelli G, et al. Inhibition of Jahn – Teller Cooperative Distortion in LiMn 2 O 4 Spinel by Ga 3+ Doping [J]. The Journal of Physical Chemistry B, 2002, 106(30): 7432–8. http://dx.doi.org/10.1021/jp020220u Liu S, Wu H, Huang L, et al. Synthesis of Li 2 Si 2 O 5 -coated LiNi 0.6 Co 0.2 Mn 0.2 O 2 cathode materials with enhanced high-voltage electrochemical properties for lithium-ion batteries [J]. Journal of Alloys and Compounds, 2016, 674: 447 – 54. http://dx.doi.org/https://doi.org/10.1016/j.jallcom.2016.03.060 Chen Z, Kim G-T, Guang Y, et al. Manganese phosphate coated Li[Ni 0.6 Co 0.2 Mn 0.2 ]O 2 cathode material: Towards superior cycling stability at elevated temperature and high voltage [J]. Journal of Power Sources, 2018, 402: 263 – 71. http://dx.doi.org/https://doi.org/10.1016/j.jpowsour.2018.09.049 Chen S, He T, Su Y, et al. Ni-Rich LiNi 0.8 Co 0.1 Mn 0.1 O 2 Oxide Coated by Dual-Conductive Layers as High Performance Cathode Material for Lithium-Ion Batteries [J]. ACS Applied Materials & Interfaces, 2017, 9(35): 29732–43. http://dx.doi.org/10.1021/acsami.7b08006 Bund A, Koehler S, Kuehnlein H H, et al. Magnetic field effects in electrochemical reactions [J]. Electrochimica Acta, 2003, 49(1): 147 – 52.http://dx.doi.org/https://doi.org/ 10.1016/j.electacta.2003.04.009 Liu W, Oh P, Liu X, et al. Nickel-Rich Layered Lithium Transition-Metal Oxide for High-Energy Lithium-Ion Batteries [J]. Angewandte Chemie International Edition, 2015, 54(15): 4440–57. http://dx.doi.org/https://doi.org/10.1002/anie.201409262 Li L, Zhang Z, Fu S, et al. Co-modification by LiAlO 2 -coating and Al-doping for LiNi 0.5 Co 0.2 Mn 0.3 O 2 as a high-performance cathode material for lithium-ion batteries with a high cutoff voltage [J]. Journal of Alloys and Compounds, 2018, 768: 582 – 90. http://dx.doi.org/https://doi.org/10.1016/j.jallcom.2018.07.223 Zhou Y, Niu P-H, Li Z-H, et al. Metallurgy of aluminum-inspired formation of aluminosilicate-coated nanosilicon for lithium-ion battery anode [J]. Rare Metals, 2022, 41. http://dx.doi.org/10.1007/s12598-022-01961-y Trevisanello E, Ruess R, Conforto G, et al. Polycrystalline and Single Crystalline NCM Cathode Materials—Quantifying Particle Cracking, Active Surface Area, and Lithium Diffusion [J]. Advanced Energy Materials, 2021, 11(18): 2003400. http://dx.doi.org/https://doi.org/10.1002/aenm.202003400 Additional Declarations No competing interests reported. Cite Share Download PDF Status: Posted Version 1 posted 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. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. 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-5443801","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":383582362,"identity":"834bec12-5a2d-4a58-bee0-cde0717d2c54","order_by":0,"name":"Wenrui Sun","email":"","orcid":"","institution":"Shanghai University","correspondingAuthor":false,"prefix":"","firstName":"Wenrui","middleName":"","lastName":"Sun","suffix":""},{"id":383582363,"identity":"7e04c937-29dc-49ae-944b-b3073fcc7b77","order_by":1,"name":"Genwen Lin","email":"","orcid":"","institution":"Shanghai University","correspondingAuthor":false,"prefix":"","firstName":"Genwen","middleName":"","lastName":"Lin","suffix":""},{"id":383582364,"identity":"b6442196-424e-4b65-9c77-12202e1579c5","order_by":2,"name":"Xueqian Zhang","email":"","orcid":"","institution":"Shanghai University","correspondingAuthor":false,"prefix":"","firstName":"Xueqian","middleName":"","lastName":"Zhang","suffix":""},{"id":383582365,"identity":"9ea91730-3aa0-48f8-9230-a80247703c01","order_by":3,"name":"Hongming Jin","email":"","orcid":"","institution":"Shanghai University","correspondingAuthor":false,"prefix":"","firstName":"Hongming","middleName":"","lastName":"Jin","suffix":""},{"id":383582366,"identity":"5ade85c2-0c46-4e0b-9e97-cf9116771a58","order_by":4,"name":"Mingyuan Zhu","email":"","orcid":"","institution":"Shanghai University","correspondingAuthor":false,"prefix":"","firstName":"Mingyuan","middleName":"","lastName":"Zhu","suffix":""},{"id":383582367,"identity":"d080a0e9-f98c-4383-8019-3a0754941fea","order_by":5,"name":"Ying Li","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA2klEQVRIiWNgGAWjYBACPmYGhgMMDDZy/Aw8ID4zYS1sEC1pxpINRGuBUIcSNxwgWgs7j+Hhgl8HGDefP3tMgqHCOrGB/ewBAg7jMTg8s+8Os9mNvDQJhjPpiQ08eQmEtfD2PGMzu8FjJsHYdjixQYLHgBgth3mM+88AtfwjVgvPj8MSBgw5QC0NRGlhKzjM25BmIHEjx9gi4Vi6cRtPDn4t/PyHN3/m+WNT399/xvDGhxpr2X72M/i1MDBwGDAwtkHZCQzwmMIH2B8wMPwhrGwUjIJRMApGMAAALYJANT60/HQAAAAASUVORK5CYII=","orcid":"","institution":"Shanghai University","correspondingAuthor":true,"prefix":"","firstName":"Ying","middleName":"","lastName":"Li","suffix":""}],"badges":[],"createdAt":"2024-11-13 05:08:37","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-5443801/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-5443801/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":70379492,"identity":"c9f1f6b0-7962-4f69-a7a7-b14b505f87c1","added_by":"auto","created_at":"2024-12-02 15:49:10","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":50462,"visible":true,"origin":"","legend":"\u003cp\u003eXRD patterns of T-NCM523 and P-NCM523\u003c/p\u003e","description":"","filename":"image1.png","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/319b86b10cc76da05dc679b9.png"},{"id":70381205,"identity":"6b5b0e37-7fc3-4486-9f38-0191ebf3a4fe","added_by":"auto","created_at":"2024-12-02 16:05:12","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":1041815,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of NCM523 cathode materials prepared with and without magnetic field. Before sintering:(a) T-Precursor, (b) P-Precursor; Final sample:(c) T-NCM523, (d) P-NCM523\u003c/p\u003e","description":"","filename":"image2.png","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/b63c1c57feea5c6303bcc45c.png"},{"id":70382666,"identity":"8ff162b6-7c2b-439a-abc2-2c694a7d4977","added_by":"auto","created_at":"2024-12-02 16:28:49","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":487012,"visible":true,"origin":"","legend":"\u003cp\u003eEDS elemental mapping and line-scan images of (a) T-NCM and (b) P-NCM samples\u003c/p\u003e","description":"","filename":"image3.png","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/07789af147bc4c9d2e63646b.png"},{"id":70382474,"identity":"96b1efc6-036b-441b-989d-05b2a484ceb6","added_by":"auto","created_at":"2024-12-02 16:26:54","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":137664,"visible":true,"origin":"","legend":"\u003cp\u003eXPS spectra of (a) survey scan, (b) Ni 2p, (c) Co 2p, (d) Mn 2p\u003c/p\u003e","description":"","filename":"image4.png","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/bfc695f2b8db569c0a14f645.png"},{"id":70379498,"identity":"9b7a6c87-0ab6-49ed-a8f5-f16ae163fb03","added_by":"auto","created_at":"2024-12-02 15:49:10","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":140597,"visible":true,"origin":"","legend":"\u003cp\u003eThe initial charge-discharge curves of (a) T-NCM523 and(b) P-NCM523, (c) Comparison of the two samples\u003c/p\u003e","description":"","filename":"image5.png","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/336f3dc4ed4066e2dfec6e1c.png"},{"id":70380863,"identity":"c51378aa-1d1c-407a-bc91-68fa3470d57c","added_by":"auto","created_at":"2024-12-02 15:57:10","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":131948,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Rate performance and (b) Cycle performance of T-NCM523 and P-NCM523.\u003c/p\u003e","description":"","filename":"image6.png","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/34f954ce14960fedd32f630c.png"},{"id":70380865,"identity":"7ec1bc8c-c512-4aae-8c20-832fb1889715","added_by":"auto","created_at":"2024-12-02 15:57:10","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":134142,"visible":true,"origin":"","legend":"\u003cp\u003eInitial three CV profiles of (a)T-NCM523 and (b) P-NCM523 after 10 cycles.\u003c/p\u003e","description":"","filename":"image7.png","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/663196a49fa8cda3e3627474.png"},{"id":70379497,"identity":"cfe98668-b45b-47e9-9b41-f81298edf9ec","added_by":"auto","created_at":"2024-12-02 15:49:10","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":118875,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Nyquist plots of T-NCM523 and P-NCM523 after 150 cycles, (b) The relationship between ω \u003csup\u003e-1/2 \u003c/sup\u003eand Z'.\u003c/p\u003e","description":"","filename":"image8.png","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/fd17ee88e195c9ba25e69294.png"},{"id":72108861,"identity":"0d36b913-5f6c-4db7-a56f-45a4e6f6f0e1","added_by":"auto","created_at":"2024-12-22 16:16:27","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2971270,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-5443801/v1/b818c51f-8a96-4fea-b4fb-ff2c6ddd023b.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"The modification of NCM cathode material prepared by hydrothermal method under pulsed high magnetic field","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eAs a typical cathode material, LiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e (NCM523) has become commonly commercial materials because of its high energy density, low cost, etc [\u003cspan additionalcitationids=\"CR2 CR3\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. However, the NCM523 cathode material also faces several challenges. Firstly, it suffers from severe cationic mixing, because the radius of Ni\u003csup\u003e2+\u003c/sup\u003e (0.069 nm) and Li\u003csup\u003e+\u003c/sup\u003e (0.076 nm) is close, that Ni\u003csup\u003e2+\u003c/sup\u003e could easily occupy the position of Li\u003csup\u003e+\u003c/sup\u003e during charge and discharge processes [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. Secondly, the lithium-ion transfer rate remains relatively low. The rate of lithium-ion transport is associated with the particle diameter. The larger the particle diameter, the fewer surfaces exposed that are favorable for Li\u003csup\u003e+\u003c/sup\u003e transport. Thirdly, its cycle performance is subpar. Especially, during the high-voltage charging process, NCM523 may undergo an irreversible phase transformation from a layered structure (R-3m) to a spinel-like (Fd-3m) or a rock-salt phase (Fm-3m) structure. This phase transition is typically accompanied by an abrupt change in lattice volume, leading to structural degradation and the formation of crack [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e, \u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eCurrently, in order to solve the aforementioned issues, there are various methods such as ion doping [\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e, \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e], surface coating [\u003cspan additionalcitationids=\"CR11\" citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e], special structural design [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e, \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e] and material preparation techniques. These approaches have yielded favorable outcomes. However, to further enhance the electrochemical performance, employing specialized approaches is necessary. The utilization of a high magnetic field to obtain superior capabilities of lithium batteries has emerged as a novel method over the past two decades [\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. For instance, Zhou [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e] and Kim [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e] et al. obtained B-axis oriented lithium iron phosphate cathode materials by applying a magnetic field during the preparation of cathode slurry. Compared to non-magnetically oriented LiFePO\u003csub\u003e4\u003c/sub\u003e counterparts, incorporating a magnetic field increased lithium-ion diffusion rate and reduced electrode polarization. After mixing NCM precursor with conductor and adhesive materials, Kim [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e] et al. used an external magnetic field to control the crystal alignment of LiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e so that Li\u003csup\u003e+\u003c/sup\u003e mainly moves along (00l) plane during the transmission process. This greatly improves the transmission rate of Li\u003csup\u003e+\u003c/sup\u003e ions, which can enhance the specific capacity and rate performance of NCM523 cathode material. These above examples demonstrate the effectiveness of applying a high magnetic field in the preparation of electrode slurries. Therefore, further investigation into the impact of high magnetic fields on the synthesis of electrode materials is necessary.\u003c/p\u003e \u003cp\u003eIn this study, the precursor of LiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e was synthesized by hydrothermal method under pulsed high magnetic field. In order to research the properties enhancement of NCM523 material which is prepared under high magnetic field, electrochemical tests (CV, EIS, etc.) and physicochemical characterization (XRD, SEM, EDS, XPS) were carried out.\u003c/p\u003e"},{"header":"2. Experimental","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Material preparation\u003c/h2\u003e \u003cp\u003eThe precursor Ni\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e was synthesized by a hydrothermal reaction under pulsed high magnetic field. Firstly, Ni(CH\u003csub\u003e3\u003c/sub\u003eCOO)\u003csub\u003e2\u003c/sub\u003e\u0026middot;4H\u003csub\u003e2\u003c/sub\u003eO、Co(CH\u003csub\u003e3\u003c/sub\u003eCOO)\u003csub\u003e2\u003c/sub\u003e\u0026middot;4H\u003csub\u003e2\u003c/sub\u003eO、Mn(CH\u003csub\u003e3\u003c/sub\u003eCOO)\u003csub\u003e2\u003c/sub\u003e\u0026middot;4H\u003csub\u003e2\u003c/sub\u003eO were dissolved in deionized water with a molar ratio of 5:2:3, and added CTAB and vitamin C. The solution was stirred for 20 minutes, which is called solution A. The solution A was putted into an ice-water bath and added Na\u003csub\u003e2\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e solution drop by drop at intervals of 5 s to obtain the solution B with the magneton speed of 600 r/min. The solution B was ultrasonicated for 30 min and then stirred at 700 r/min for 1 h. Subsequently, it was placed in the autoclave lined by PTFE with 80% filling volume. The autoclave was placed into the pulsed high magnetic field. The hydrothermal temperature was set to 180 ℃ and magnetic field intensity was 3 T with the 20 s interval of pulsed magnetization. After reaction for 12h, the reactant was removed. Then the reactant was ultrasonicated and stirred for a while. After pumping, filtering and washing the precipitation for several times, the precipitate was obtained. Finally, the precipitate was dried under 80 ℃ for 24 h to produce Ni\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e precursor. Comparison sample was prepared non-magnetic field. The precursors obtained with and without pulsed magnetic field were labeled as T-Precursor and P-Precursor.\u003c/p\u003e \u003cp\u003eLiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e cathode material was synthesized by high-temperature solid-state reaction. The Precursors were mixed with a certain amount of Li\u003csub\u003e2\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e (Li excess 5%). After mechanically grounding evenly, the mixtures were transferred to a tubular furnace, heated in an oxygen atmosphere with a temperature rise rate of 3 ℃/min and maintained at 300 ℃ for 1h, 500 ℃ for 6h, 870 ℃ for 12h. Upon cooling of the tubular furnace to room temperature, the final products were fully ground using the mortar. The LiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e prepared from T-Precursor and P-Precursor was labeled as T-NCM523 and P-NCM523, respectively.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Material characterization\u003c/h2\u003e \u003cp\u003eThe crystal structure of the samples was analyzed using X-ray diffraction (XRD, Rigaku smartlab 9) with scattering angle 2θ in the range of 10\u0026ndash;80\u0026deg; and scanning rate of 2\u0026deg;/min. Field emission scanning electron microscopy (FE-SEM, Sigma 300) coupled with energy dispersive spectroscopy (EDS, Oxford Xplore 30) was used to examine the micro-morphology and elemental distribution of the prepared samples. X-ray photoelectron spectroscopy (XPS, Thermo Scientific K-Alpha) was employed to detect the surface chemical composition of the samples.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Electrochemical measurements\u003c/h2\u003e \u003cp\u003eThe CR2016 coin cells were self-assembled in an argon-filled glove box and tested for their electrochemical performance. The cathode slurry consisted of 80% active material, 10% carbon black and 10% polyvinylidene fluoride (PVDF) uniformly dispersed in N-methyl-2-pyrrolidone (NMP), and then the mixture was coated on aluminum foil and dried in a vacuum oven at 80℃ for 12 h. The electrolyte was 1 mol\u0026middot;L\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e LiPF\u003csub\u003e6\u003c/sub\u003e solution in a mixture of ethylene carbonate (EC), dimethyl carbonate (DMC), and ethylene methyl carbonate (EMC) (1:1:1, v/v/v). Celgard 2500 microporous polypropylene membrane served as the separator, and lithium metal served as the anode. The cathode, electrolyte, separator and anode were assembled into a cell in a glove box under H\u003csub\u003e2\u003c/sub\u003eO and O\u003csub\u003e2\u003c/sub\u003e atmosphere both less than 0.01 ppm. The cells were charged and discharged on a Land CT2001A device (China) at a balanced current in the voltage range of 3-4.5 V. In the electrochemical workstation (CHI 660E, CH Instruments), a cyclic voltammetry (CV) test was conducted at a voltage sweep rate of 0.1 mV/s, and an electrochemical impedance spectroscopy (EIS) test was performed in 0.01\u0026ndash;105 Hz.\u003c/p\u003e \u003c/div\u003e"},{"header":"3. Results and discussion","content":"\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003e3.1 Structure and morphology\u003c/h2\u003e \u003cp\u003eThe XRD patterns of NCM523 cathode materials prepared with and without magnetic field have been shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. The diffraction peaks of T-NCM523 and P-NCM523 are shar, which indicates that the two samples have high crystallinity. And the XRD patterns of the two samples are matched with the standard card PDF#74\u0026ndash;0919 [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e], with the hexagonal α-NaFeO\u003csub\u003e2\u003c/sub\u003e layered structure of R-3m space group, which suggests that applying external magnetic field does not change the crystal structure. Additionally, no peaks corresponding to extraneous impurities were detected in either sample, which also means that they do not contain other impurity phases [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]. Furthermore, the clear split peaks between (006)/(012) and (108)/(110) also confirm the layer structure of the both samples [\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e, \u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e, \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe lattice parameters of T-NCM523 and P-NCM523 calculated from the XRD patterns were listed in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. The values of the lattice parameter c/a for both samples are above 4.9, which proves the presence of a well-defined layer structure. And the c/a ratio of T-NCM523 is slightly higher than that of the P-NCM523, which indicates that the sample prepared under the magnetic field has a better layer structure. Furthermore, it is well known that the intensity ratio between (104) and (003) is a reliable parameter for evaluating the cation mixing, i.e., the I\u003csub\u003e003\u003c/sub\u003e/I\u003csub\u003e104\u003c/sub\u003e ratio higher than 1.2 often indicates that the material has a low Li\u003csup\u003e+\u003c/sup\u003e/Ni\u003csup\u003e2+\u003c/sup\u003e cation mixing. A higher c/a ratio indicates lower cation mixing [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e]. The I\u003csub\u003e003\u003c/sub\u003e/I\u003csub\u003e104\u003c/sub\u003e intensity ratios of T-NCM523 and P-NCM523 are 1.5596 and 1.2129, respectively, which are both above 1.2. And the ratio of T-NCM523 is higher than that of P-NCM523, which means that the NCM523 prepared under the high magnetic field has a lower cation mixing.\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\u003eXRD Rietveld refinement results of T-NCM523 and P-NCM523\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\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\u003ea (\u0026Aring;)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003ec (\u0026Aring;)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003ec/a\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eI\u003csub\u003e(003)\u003c/sub\u003e/I\u003csub\u003e(104)\u003c/sub\u003e\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eT-NCM523\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e2.8680\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e14.2238\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e4.9595\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e1.5596\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP-NCM523\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e2.8677\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e14.2158\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e4.9572\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e1.2129\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 further observe the influence of magnetic field on the microscopic morphology of the NCM523 cathode material, SEM was employed to examine the precursors and final products, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (a) and 2 (b) are the micro-morphology of T-Precursor and P-Precursor, and it could be seen that both samples are composed of many secondary particles, which are aggregated from fine spherical particles with diameters in the range of tens of nanometer. Comparing the two samples, the T-Precursor sample has smaller primary particle and more uniform. This is the result that during the hydrothermal reaction process, the high magnetic field provides energy for the nucleation and growth of precursors [\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e], which facilitates the formation of fine and homogeneous crystal nucleus and inhibits the rapid growth of them by affecting the charged particles in the solution. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (c) and 2 (d) show the morphology of T-NCM523 and P-NCM523. Both samples have irregular polyhedral shapes and smooth surface. As well, the particle size of P-NCM523 is approximately double of T-NCM523. The small and uniform primary size of the T-NCM523 is also maintained after lithiation and sintering, which suggests that applying a high magnetic field facilitates the reduction of materials size in the process of the cathode material preparation [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e shows the EDS maping/line scan results of T-NCM523 and P-NCM523 samples. From these results, the uniform distribution of Ni, Co and Mn on the surface of the two samples was observed. From the comparison of the line scan results of the two samples, it is concluded that the elements distribution on the surface of the T-NCM523 is more homogeneous than that of the P-NCM523. Under the high magnetic field, the magnetic stirring makes the charged particles of Ni, Co and Mn magnetic elements more uniformly distributed during the precursor formation, which is also conducive to the stability of the LiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e cathode material.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eX-ray photoelectron spectroscopy (XPS) was employed to investigate the effect of pulsed magnetic field on the valences of transition metal elements in LiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e. The XPS test results of T-NCM523 and P-NCM523 samples are presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e. According to the C1s peak (284.80 eV), the electron binding energy of each detected element was calibrated, and the fine spectrum of detected elements was fitted and analyzed using Avantage software. It can be seen from the full spectrum of the two samples in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e (a), T-NCM523 and P-NCM523 have similar XPS spectra. And the characteristic peaks of Ni, Co and Mn are obvious. Figure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e (b) presents the fitted Ni 2p orbital spectra for both samples. The peaks of 879.40, 873.24, 860.83, 856.56, 855.20 eV electron binding energy correspond to the Ni 2p1/2 satellite peak orbit, Ni 2p1/2 orbit, Ni 2p3/2 satellite peak orbit, Ni\u003csup\u003e3+\u003c/sup\u003e 2p3/2 and Ni\u003csup\u003e2+\u003c/sup\u003e 2p3/2 orbits, respectively [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. The Ni element exists in both samples in +\u0026thinsp;2 and +\u0026thinsp;3 valence forms, but the relative content of Ni\u003csup\u003e2+\u003c/sup\u003e in the T-NCM523 sample is reduced by 3.48%, which indicates that the application of the pulsed high magnetic field reduces the Li\u003csup\u003e+\u003c/sup\u003e/Ni\u003csup\u003e2+\u003c/sup\u003e cation mixing behavior, in accordance with the test results of XRD. From Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e (c), according to the fitting results of Co 2p orbitals, the electronic binding energies of Co 2p1/2 and Co 2p3/2 orbitals are 796.12 and 780.79 eV, respectively, indicating that Co exists in the form of +\u0026thinsp;3 valence [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e].Moreover, Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e (d) illustrates the fitting results for the fine spectra of Mn 2p orbitals. The peaks of 654.21, 643.15, 641.98, 637.73eV electron binding energy correspond to the Mn 2p1/2, Mn\u003csup\u003e4+\u003c/sup\u003e 2p3/2, Mn\u003csup\u003e3+\u003c/sup\u003e 2p3/2, and Mn 2p3/2, and the elemental Mn was determined to be +\u0026thinsp;3 and +\u0026thinsp;4 valences. The relative content of Mn\u003csup\u003e4+\u003c/sup\u003e in T-NCM523 samples increased by 11.11%, which was conducive to inhibiting J-T distortion and stabilizing the crystal structure of LiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e material [\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e, \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003e3.2 Electrochemical properties\u003c/h2\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e shows the initial charge-discharge curves, rate capacity, and cycle performance of T-NCM523 and P-NCM523 at 1C (1C\u0026thinsp;=\u0026thinsp;180 mA/g), 3-4.5V high cut-off voltage, respectively.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe data presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e are provided in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e. The first cycle charge/discharge specific capacities of T-NCM523 are 228.3 mAh/g and 187.5 mAh/g, respectively. And the Coulombic efficiency is 82.1%. The first cycle charge/discharge specific capacities of the P-NCM523 sample are 221.6 mAh/g and 178.3 mAh/g, respectively, within an initial Coulombic efficiency is 80.5%. Compared to the sample prepared without the magnetic field, T-NCM523 exhibits an improvement in initial discharge capacity by 9.2 mAh/g and an increase in Coulombic efficiency by 1.6%. These findings implies that NCM523 prepared under the high magnetic field has higher discharge specific capacity and coulombic efficiency.\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\u003eInitial charge-discharge specific capacities and columbic efficiency of the T-NCM523 and P-NCM523 at 1C.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSamples\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCharge capacity (mAh/g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eDischarge capacity (mAh/g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eIrreversible capacity loss (mAh/g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eCoulombic efficiency (%)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eT-NCM523\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e228.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e187.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e40.8\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e82.1\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP-NCM523\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e221.6\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e178.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e43.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e80.5\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\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e (a) is the rate performance of the two samples (0.1 C\u0026thinsp;=\u0026thinsp;18 mA/g, 0.2 C\u0026thinsp;=\u0026thinsp;36 mA/g, 0.5 C\u0026thinsp;=\u0026thinsp;90 mA/g, 1 C\u0026thinsp;=\u0026thinsp;180 mA/g, and 5 C\u0026thinsp;=\u0026thinsp;900 mA/g). With increasing current density, the discharge-specific capacity of both samples exhibits a declining trend, and P-NCM523 has an even more significant decrease. At 0.1 C rate, the discharge specific capacities of T-NCM523 and P-NCM523 reached 220.7 mAh/g and 199.5 mAh/g, respectively. As the current density was increased, the discharge-specific capacity of T-NCM523 decreased less than that of P-NCM523 by 24.3 mAh/g at 1 C. The T-NCM523 is 43.0 mAh/g above the P-NCM523 at the current density of 5 C. Because, under the high current density, obstructed by the influence of the electrode/electrolyte interface and the viscosity of the electrolyte, etc. Li\u003csup\u003e+\u003c/sup\u003e is difficult to migrate quickly to the electrode surface and participate in the reaction, which makes the battery capacity decrease [\u003cspan additionalcitationids=\"CR32\" citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e]. And owing to the better layer structure and smaller particle size of the NCM523 prepared under magnetic field, the exposed surface favorable for Li\u003csup\u003e+\u003c/sup\u003e transport is increased and the transport distance is shortened, which provides a fast Li\u003csup\u003e+\u003c/sup\u003e transport channel. Thus it can be compensating for some of the rate difference, which causes the decrease is slighter than that of the original sample [\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e]. Upon the current density reaching 0.1 C again after 31 cycles, the discharge specific capacity of both samples closely matches their initial values, indicating good reversibility for both materials.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure \u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e (b) illustrates the cycle performance of the two samples, which is evaluated at a high cut-off voltage range of 3.0\u0026ndash;4.5 V and 1 C. The corresponding data for Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e (b) is listed in Table\u0026nbsp;\u003cspan refid=\"Tab3\" class=\"InternalRef\"\u003e3\u003c/span\u003e. The initial discharge-specific capacities of the T-NCM523 and P-NCM523 were 190.4 mAh/g and 178.3 mAh/g, respectively. After 200 cycles, the discharge capacity of P-NCM523 declined to 122.9 mAh/g, and a capacity retention rate is 68.9%. In contrast, T-NCM523 exhibited a discharge capacity of 147.3 mAh/g and a capacity retention rate of 77.4%, which is 8.5% higher than that of P-NCM523.The initial discharge-specific capacity and cycle stability of T-NCM523 are both higher than that of P-NCM523.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab3\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 3\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eCycle performance of the T-NCM523 and P-NCM523 at 3.0-4.5 V under 1 C.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSamples\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eInitial discharge capacity (mAh/g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eDischarge capacity after 200 cycles (mAh/g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eIrreversible capacity loss (mAh/g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eCapacity retention after 200 cycles(%)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eT-NCM523\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e190.4\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e147.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e43.1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e77.4\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP-NCM523\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e178.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e122.9\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e55.4\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e68.9\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\u003eFor further evaluating the electrochemical reaction reversibility and Li\u003csup\u003e+\u003c/sup\u003e transport ability, Cyclic Voltammetry (CV) and Electrochemical Impedance Spectroscopy (EIS) were performed. Figure\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e (a) and 7 (b) show the CV curves of T-NCM523 and P-NCM523. Both curves present a pair of redox peaks corresponding to Ni\u003csup\u003e2+\u003c/sup\u003e/Ni\u003csup\u003e4+\u003c/sup\u003e interconversion, and the absence of other peaks suggests that within the tested voltage range, the current is derived from the valence change of nickel ions, and the electrochemical reaction is reversible [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e]. It also suggests that the crystal structure is relatively stable. During the first charging and discharging cycles of the battery, the electrolyte and electrode react at the solid/liquid two-phase interface to form a passivating surface layer covering the electrode material (solid electrolyte SEI layer). The formation and growth of SEI film, decomposition of electrolyte and other side reactions lead to electrode polarization, which makes a potential difference (expressed as △E) exists between the Ni\u003csup\u003e2+\u003c/sup\u003e /Ni\u003csup\u003e4+\u003c/sup\u003e peaks. Therefore, the △E value is reflected the degree of electrode polarization. The smaller the △E value, the lower the electrode polarization and the better the reversibility [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. As it can be seen from the Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e, the ΔE\u003csub\u003e3\u003c/sub\u003e (△E\u003csub\u003e3\u003c/sub\u003e represents the third cycle of △E)value of T-NCM523 was 0.191, while that of P-NCM523 was 0.264. This indicates that the NCM523 prepared under the pulsed high magnetic field has lower electrode polarization and the better reversibility, which also leads to better cycling stability as well as rate performance.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eAfter 150 cycles within 3.0-4.5 V at 1C, the impedance of two samples was tested, as depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e (a) and 8 (b). The Nyquist plot was fitted using Zview software. And the corresponding equivalent circuit model is also shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e(a). The plot in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e (a) consists of two semi-circles and a sloped line. The semicircle in the high/middle-frequency region represents the SEI film resistance and charge transfer resistance (R\u003csub\u003ef\u003c/sub\u003e and R\u003csub\u003ect\u003c/sub\u003e) on the cathode material surface, respectively. While the intersection point of the semicircle with the horizontal axis represents the electrolyte resistance R\u003csub\u003es\u003c/sub\u003e, and the sloped line (the Warburg curve) is associated with the Li\u003csup\u003e+\u003c/sup\u003e transport rate [\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. After 150 cycles, due to the side reaction between the electrolyte and the cathode material under high voltage, the R\u003csub\u003ef\u003c/sub\u003e and R\u003csub\u003ect\u003c/sub\u003e values of both samples are high, in which the surface film impedance (R\u003csub\u003ef\u003c/sub\u003e) of the P-NCM523 is 311.5 Ω, which is much higher than that of 191.3 Ω of the T-NCM523(See Table \u003cspan refid=\"Tab4\" class=\"InternalRef\"\u003e4\u003c/span\u003e for details). In addition, the charge transfer resistance (R\u003csub\u003ect\u003c/sub\u003e) of the T-NCM523 is reduced by 63.5% compared to the P-NCM523, which implies less internal energy consumption, the superior cycle and rate performance. The Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficient (D) is calculated by the equations (\u003cspan refid=\"Equ1\" class=\"InternalRef\"\u003e1\u003c/span\u003e) and (\u003cspan refid=\"Equ2\" class=\"InternalRef\"\u003e2\u003c/span\u003e), as follows [\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e]:\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ1\" name=\"EquationSource\"\u003e\n$$\\:D=\\frac{{R}^{2}{T}^{2}}{2{A}^{2}{n}^{4}{F}^{4}{C}^{2}{\\sigma\\:}^{2}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\u003c/div\u003e\u003cdiv id=\"Equ2\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ2\" name=\"EquationSource\"\u003e\n$$\\:{Z}^{{\\prime\\:}}={R}_{s}+{R}_{ct}+\\sigma\\:{\\omega\\:}^{-1/2}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e2\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eWhere R is the constant (8.314 J/mol K), T represents the absolute temperature (298 K), A represents the surface area of the positive electrode plate (1.767 cm\u003csup\u003e2\u003c/sup\u003e), n is the number of electrons involved in the redox reaction (n\u0026thinsp;=\u0026thinsp;1), and C represents the concentration of lithium ions per unit volume (7.818\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;4\u003c/sup\u003e mol/cm\u003csup\u003e3\u003c/sup\u003e). F is the Faraday constant (96485.3 C/mol) and σ refers to the Warburg factor, which can be derived by linear fitting the slope from Z'-ω\u003csup\u003e\u0026minus;1\u0026frasl;2\u003c/sup\u003e in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e (b) according to the formula (1\u0026ndash;2) \u003cb\u003e[38]\u003c/b\u003e.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab4\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 4\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eEIS parameters of P-NCM523 and T-NCM523 after 150 cycles\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSamples\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eR\u003csub\u003es\u003c/sub\u003e (Ω)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eR\u003csub\u003ef\u003c/sub\u003e (Ω)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eR\u003csub\u003ect\u003c/sub\u003e (Ω)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eD *10\u003csup\u003e10\u003c/sup\u003e(cm\u003csup\u003e2\u003c/sup\u003e/s)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP-NCM523\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e8.06\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e311.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e168.40\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e1.51\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eT-NCM523\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e11.28\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e191.3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e61.41\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e6.25\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 calculations from the above equations are only used for qualitative analysis due to the difficulty in calculating the lithium-ion concentration C. The lithium-ion diffusion coefficients D of T-NCM523 and P-NCM523 are 6.25 \u0026times; 10\u003csup\u003e\u0026minus;\u0026thinsp;10\u003c/sup\u003e cm\u003csup\u003e2\u003c/sup\u003e/s and 1.51 \u0026times; 10\u003csup\u003e\u0026minus;\u0026thinsp;10\u003c/sup\u003e cm\u003csup\u003e2\u003c/sup\u003e/s, respectively. T-NCM523 cathode material has a bigger lithium-ion diffusion coefficient. Because of the application of pulsed high magnetic field, the nucleation rate of the cathode material increases during the hydrothermal reaction, and the primary particle size decreases. The obtained cathode material has a relatively larger specific surface area, which exposes more crystal faces conducive to lithium-ion transport. Meanwhile, the low cation mixing facilitates the reversible de-embedding/embedding of Li\u003csup\u003e+\u003c/sup\u003e, and the better layer structure provides an efficient diffusion pathway for Li\u003csup\u003e+\u003c/sup\u003e in the interior of the material. As a result, the cathode material exhibits lower electrochemical impedance and higher Li-ion diffusion coefficient, that is consistent with the superior electrochemical performance of the previous T-NCM523.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eThe LiNi\u003csub\u003e0.5\u003c/sub\u003eCo\u003csub\u003e0.2\u003c/sub\u003eMn\u003csub\u003e0.3\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e cathode material synthesized by hydrothermal method under the pulsed high magnetic field has higher Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficient, better cycle and rate performance comparing to the NCM523 prepared without the high magnetic field. This is attributed to its smaller particle size, the better layer structure and the lower Li\u003csup\u003e+\u003c/sup\u003e/Ni\u003csup\u003e2+\u003c/sup\u003e cation mixing. The smaller particle size has more exposed surface that favors Li\u003csup\u003e+\u003c/sup\u003e transport and shortens the Li\u003csup\u003e+\u003c/sup\u003e transport distance, and the better layer structure provides the lower degree of tortuosity for Li\u003csup\u003e+\u003c/sup\u003e transport and reduces the electrode polarization. All these increase the Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficient. The lower Li\u003csup\u003e+\u003c/sup\u003e/Ni\u003csup\u003e2+\u003c/sup\u003e cation mixing favors the reversible de-embedding/embedding of Li\u003csup\u003e+\u003c/sup\u003e, which improves the specific charge/discharge capacity, the cycle and rate performances.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eDeclaration of competing interest\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eDeclaration of Funding\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNo funding was received for conducting this study.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor contribution\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eAll authors were involved in the conception and design of the study. Conceptualization, Methodology, Data curation, Writing, Visualization, Investigation, Reviewing and Editing: WR Sun. Reviewing, Editing: GW Lin. Data curation, Document organization, Supporting experiments: XQ Zhang. XRD Testing: HM Jin. Writing Supervision: MY Zhu. Consultant, Supervision, Guidance, Software, Validation: Y Li. All authors read and approved the final draft.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAcknowledgements\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors thank the Analysis and Research Center of Shanghai University for their technical support.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eWinter M, Barnett B, Xu K. Before Li Ion Batteries [J]. 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Polycrystalline and Single Crystalline NCM Cathode Materials\u0026mdash;Quantifying Particle Cracking, Active Surface Area, and Lithium Diffusion [J]. Advanced Energy Materials, 2021, 11(18): 2003400.\u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttp://dx.doi.org/https://doi.org/10.1002/aenm.202003400\u003c/span\u003e\u003cspan address=\"10.1002/aenm.202003400\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"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":"Pulsed high magnetic field, hydrothermal method, NCM523, High voltage","lastPublishedDoi":"10.21203/rs.3.rs-5443801/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-5443801/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eHigh magnetic field serves as a unique technique for the materials preparation which is more applied in the magnetic materials, but seldom in the electrode materials. In this study, the pulsed high magnetic field was employed during the hydrothermal synthesis of the NCM523 precursor. And the electrochemical performances of NCM523 are researched: at a high cut-off voltage range from 3V to 4.5V and current density set at 1C = 180 mA/g, an initial specific discharge capacity is 190.4 mAh/g which is 12.1 mAh/g increased, and after 200 cycles both specific discharge capacity and capacity retention rate increased by 24.4 mAh/g and 8.5%, respectively, comparing to the sample prepared without magnetic field. The mechanism should be that the high magnetic field applied in the formation and growth of NCM crystal could improve its micro-structure such as layer structural, result in the mitigate Li\u003csup\u003e+\u003c/sup\u003e/Ni\u003csup\u003e2+\u003c/sup\u003e mixed-arrangement phenomenon and increase the Li\u003csup\u003e+\u003c/sup\u003e diffusion rate.\u003c/p\u003e","manuscriptTitle":"The modification of NCM cathode material prepared by hydrothermal method under pulsed high magnetic field","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-12-02 15:49:05","doi":"10.21203/rs.3.rs-5443801/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":"272cba98-8ed0-489c-a83e-2aa75a08fcd4","owner":[],"postedDate":"December 2nd, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2024-12-22T16:08:10+00:00","versionOfRecord":[],"versionCreatedAt":"2024-12-02 15:49:05","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-5443801","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-5443801","identity":"rs-5443801","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}