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1.
Peng‐Fei Wang Hanshen Xin Tong‐Tong Zuo Dr. Qinghao Li Dr. Xinan Yang Dr. Ya‐Xia Yin Prof. Xike Gao Prof. Xiqian Yu Prof. Yu‐Guo Guo 《Angewandte Chemie (International ed. in English)》2018,57(27):8178-8183
Layered O3‐type sodium oxides (NaMO2, M=transition metal) commonly exhibit an O3–P3 phase transition, which occurs at a low redox voltage of about 3 V (vs. Na+/Na) during sodium extraction and insertion, with the result that almost 50 % of their total capacity lies at this low voltage region, and they possess insufficient energy density as cathode materials for sodium‐ion batteries (NIBs). Therefore, development of high‐voltage O3‐type cathodes remains challenging because it is difficult to raise the phase‐transition voltage by reasonable structure modulation. A new example of O3‐type sodium insertion materials is presented for use in NIBs. The designed O3‐type Na0.7Ni0.35Sn0.65O2 material displays a highest redox potential of 3.7 V (vs. Na+/Na) among the reported O3‐type materials based on the Ni2+/Ni3+ couple, by virtue of its increased Ni?O bond ionicity through reduced orbital overlap between transition metals and oxygen within the MO2 slabs. This study provides an orbital‐level understanding of the operating potentials of the nominal redox couples for O3‐NaMO2 cathodes. The strategy described could be used to tailor electrodes for improved performance. 相似文献
2.
Ting Jin Peng‐Fei Wang Qin‐Chao Wang Kunjie Zhu Tao Deng Jiaxun Zhang Wei Zhang Xiao‐Qing Yang Lifang Jiao Chunsheng Wang 《Angewandte Chemie (International ed. in English)》2020,59(34):14511-14516
P2‐type layered oxides suffer from an ordered Na+/vacancy arrangement and P2→O2/OP4 phase transitions, leading them to exhibit multiple voltage plateaus upon Na+ extraction/insertion. The deficient sodium in the P2‐type cathode easily induces the bad structural stability at deep desodiation states and limited reversible capacity during Na+ de/insertion. These drawbacks cause poor rate capability and fast capacity decay in most P2‐type layered oxides. To address these challenges, a novel high sodium content (0.85) and plateau‐free P2‐type cathode‐Na0.85Li0.12Ni0.22Mn0.66O2 (P2‐NLNMO) was developed. The complete solid‐solution reaction over a wide voltage range ensures both fast Na+ mobility (10?11 to 10?10 cm2 s?1) and small volume variation (1.7 %). The high sodium content P2‐NLNMO exhibits a higher reversible capacity of 123.4 mA h g?1, superior rate capability of 79.3 mA h g?1 at 20 C, and 85.4 % capacity retention after 500 cycles at 5 C. The sufficient Na and complete solid‐solution reaction are critical to realizing high‐performance P2‐type cathodes for sodium‐ion batteries. 相似文献
3.
Dr. Haijun Yu Dr. Yang Ren Dongdong Xiao Shaohua Guo Dr. Yanbei Zhu Dr. Yumin Qian Prof. Lin Gu Prof. Haoshen Zhou 《Angewandte Chemie (International ed. in English)》2014,53(34):8963-8969
Sodium‐ion batteries are important alternative energy storage devices that have recently come again into focus for the development of large‐scale energy storage devices because sodium is an abundant and low‐cost material. However, the development of electrode materials with long‐term stability has remained a great challenge. A novel negative‐electrode material, a P2‐type layered oxide with the chemical composition Na2/3Co1/3Ti2/3O2, exhibits outstanding cycle stability (ca. 84.84 % capacity retention for 3000 cycles, very small decrease in the volume (0.046 %) after 500 cycles), good rate capability (ca. 41 % capacity retention at a discharge/charge rate of 10 C), and a usable reversible capacity of about 90 mAh g?1 with a safe average storage voltage of approximately 0.7 V in the sodium half‐cell. This P2‐type layered oxide is a promising anode material for sodium‐ion batteries with a long cycle life and should greatly promote the development of room‐temperature sodium‐ion batteries. 相似文献
4.
Suppressing the P2–O2 Phase Transition of Na0.67Mn0.67Ni0.33O2 by Magnesium Substitution for Improved Sodium‐Ion Batteries
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Peng‐Fei Wang Ya You Dr. Ya‐Xia Yin Yue‐Sheng Wang Prof. Li‐Jun Wan Prof. Lin Gu Prof. Yu‐Guo Guo 《Angewandte Chemie (International ed. in English)》2016,55(26):7445-7449
Room‐temperature sodium‐ion batteries (SIBs) have shown great promise in grid‐scale energy storage, portable electronics, and electric vehicles because of the abundance of low‐cost sodium. Sodium‐based layered oxides with a P2‐type layered framework have been considered as one of the most promising cathode materials for SIBs. However, they suffer from the undesired P2–O2 phase transition, which leads to rapid capacity decay and limited reversible capacities. Herein, we show that this problem can be significantly mitigated by substituting some of the nickel ions with magnesium to obtain Na0.67Mn0.67Ni0.33?xMgxO2 (0≤x≤0.33). Both the reversible capacity and the capacity retention of the P2‐type cathode material were remarkably improved as the P2–O2 phase transition was thus suppressed during cycling. This strategy might also be applicable to the modulation of the physical and chemical properties of layered oxides and provides new insight into the rational design of high‐capacity and highly stable cathode materials for SIBs. 相似文献
5.
Electrochemical and Structural Study of Layered P2‐Type Na2/3Ni1/3Mn2/3O2 as Cathode Material for Sodium‐Ion Battery
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Yanfen Wen Dr. Bei Wang Guang Zeng Prof. Kazuhiro Nogita Delai Ye Prof. Lianzhou Wang 《化学:亚洲杂志》2015,10(3):661-666
P2‐type Na2/3Ni1/3Mn2/3O2 was synthesized by a controlled co‐precipitation method followed by a high‐temperature solid‐state reaction and was used as a cathode material for a sodium‐ion battery (SIB). The electrochemical behavior of this layered material was studied and an initial discharge capacity of 151.8 mA h g?1 was achieved in the voltage range of 1.5–3.75 V versus Na+/Na. The retained discharge capacity was found to be 123.5 mA h g?1 after charging/discharging 50 cycles, approximately 81.4 % of the initial discharge capacity. In situ X‐ray diffraction analysis was used to investigate the sodium insertion and extraction mechanism and clearly revealed the reversible structural changes of the P2‐Na2/3Ni1/3Mn2/3O2 and no emergence of the O2‐Ni1/3Mn2/3O2 phase during the cycling test, which is important for designing stable and high‐performance SIB cathode materials. 相似文献
6.
Zichao Yan Liang Tang Yangyang Huang Weibo Hua Yong Wang Rong Liu Qinfen Gu Sylvio Indris Shu‐Lei Chou Yunhui Huang Minghong Wu Shi‐Xue Dou 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2019,131(5):1426-1430
Low‐cost layered oxides free of Ni and Co are considered to be the most promising cathode materials for future sodium‐ion batteries. Biphasic Na0.78Cu0.27Zn0.06Mn0.67O2 obtained via superficial atomic‐scale P3 intergrowth with P2 phase induced by Zn doping, consisting of inexpensive transition metals, is a promising cathode for sodium‐ion batteries. The P3 phase as a covering layer in this composite shows not only in excellent electrochemical performance but also its tolerance to moisture. The results indicate that partial Zn substitutes can effectively control biphase formation for improving the structural/electrochemical stability as well as the ionic diffusion coefficient. Based on in situ synchrotron X‐ray diffraction coupled with electron‐energy‐loss spectroscopy, a possible Cu2+/3+ redox reaction mechanism has now been revealed. 相似文献
7.
Xiaoyan Li Kaikai Li Sicong Zhu Ke Fan Linlong Lyu Haimin Yao Yiyang Li Jinlian Hu Haitao Huang Yiu‐Wing Mai John B. Goodenough 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2019,131(19):6305-6309
The sodium‐ion battery is a promising battery technology owing to its low price and high abundance of sodium. However, the sluggish kinetics of sodium ion makes it hard to achieve high‐rate performance, therefore impairing the power density. In this work, a fiber‐in‐tube Co9S8‐carbon(C)/Co9S8 is designed with fast sodiation kinetics. The experimental and simulation analysis show that the dominating capacitance mechanism for the high Na‐ion storage performance is due to abundant grain boundaries, three exposed layer interfaces, and carbon wiring in the design. As a result, the fiber‐in‐tube hybrid anode shows a high specific capacity of 616 mAh g?1 after 150 cycles at 0.5 A g?1. At 1 A g?1, a capacity of ca. 451 mAh g?1 can be achieved after 500 cycles. More importantly, a high energy density of 779 Wh kg?1 and power density of 7793 W kg?1 can be obtained simultaneously. 相似文献
8.
Graphite‐Nanoplate‐Coated Bi2S3 Composite with High‐Volume Energy Density and Excellent Cycle Life for Room‐Temperature Sodium–Sulfide Batteries
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Wei‐Jie Li Chao Han Dr. Shu‐Lei Chou Prof. Jia‐Zhao Wang Prof. Zhen Li Yong‐Mook Kang Prof. Hua‐Kun Liu Prof. Shi‐Xue Dou 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(2):590-597
Graphite‐nanoplate‐coated Bi2S3 composite (Bi2S3@C) has been prepared by a simple, scalable, and energy‐efficient precipitation method combined with ball milling. The Bi2S3@C composite was used as the cathode material for sodium–sulfide batteries. It delivered an initial capacity of 550 mAh g?1 and high stable specific energy in the range of 275–300 Wh kg?1 at 0.1 C, with an enhanced capacity retention of 69 % over 100 cycles. The unique structure demonstrates superior cycling stability, with a capacity drop of 0.3 % per cycle over 100 cycles, compared with that of bare Bi2S3. The sodium storage mechanism of Bi2S3 was investigated based on ex situ X‐ray diffraction and scanning transmission electron microscopy. 相似文献
9.
Chenglong Zhao Feixiang Ding Yaxiang Lu Liquan Chen Yong‐Sheng Hu 《Angewandte Chemie (International ed. in English)》2020,59(1):264-269
Material innovation on high‐performance Na‐ion cathodes and the corresponding understanding of structural chemistry still remain a challenge. Herein, we report a new concept of high‐entropy strategy to design layered oxide cathodes for Na‐ion batteries. An example of layered O3‐type NaNi0.12Cu0.12Mg0.12Fe0.15Co0.15Mn0.1Ti0.1Sn0.1Sb0.04O2 has been demonstrated, which exhibits the longer cycling stability (ca. 83 % of capacity retention after 500 cycles) and the outstanding rate capability (ca. 80 % of capacity retention at the rate of 5.0 C). A highly reversible phase‐transition behavior between O3 and P3 structures occurs during the charge‐discharge process, and importantly, this behavior is delayed with more than 60 % of the total capacity being stored in O3‐type region. Possible mechanism can be attributed to the multiple transition‐metal components in this high‐entropy material which can accommodate the changes of local interactions during Na+ (de)intercalation. This strategy opens new insights into the development of advanced cathode materials. 相似文献
10.
An O3‐type Oxide with Low Sodium Content as the Phase‐Transition‐Free Anode for Sodium‐Ion Batteries
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Chenglong Zhao Dr. Maxim Avdeev Prof. Liquan Chen Prof. Yong‐Sheng Hu 《Angewandte Chemie (International ed. in English)》2018,57(24):7056-7060
Layered transition metal oxides NaxMO2 (M=transition metal) with P2 or O3 structure have attracted attention in sodium‐ion batteries (NIBs). A universal law is found to distinguish structural competition between P2 and O3 types based on the ratio of interlayer distances of the alkali metal layer d(O‐Na‐O) and transition‐metal layer d(O‐M‐O). The ratio of about 1.62 can be used as an indicator. O3‐type Na0.66Mg0.34Ti0.66O2 oxide is prepared as a stable anode for NIBs, in which the low Na‐content (ca. 0.66) usually undergoes a P2‐type structure with respect to NaxMO2. This material delivers an available capacity of about 98 mAh g?1 within a voltage range of 0.4–2.0 V and exhibits a better cycling stability (ca. 94.2 % of capacity retention after 128 cycles). In situ X‐ray diffraction reveals a single‐phase reaction in the discharge–charge process, which is different from the common phase transitions reported in O3‐type electrodes, ensuring long‐term cycling stability. 相似文献
11.
Shaohua Guo Dr. Pan Liu Dr. Yang Sun Kai Zhu Dr. Jin Yi Prof. Mingwei Chen Prof. Masayoshi Ishida Prof. Haoshen Zhou 《Angewandte Chemie (International ed. in English)》2015,54(40):11701-11705
Recently, there has been great interest in developing advanced sodium‐ion batteries for large‐scale application. Most efforts have concentrated on the search for high‐performance electrode materials only in sodium half‐cells. Research on sodium full cells for practical application has encountered many problems, such as insufficient cycles with rapid capacity decay, low safety, and low operating voltage. Herein, we present a layered P2‐Na0.66Ni0.17Co0.17Ti0.66O2, as both an anode (ca. 0.69 V versus Na+/Na) and as a high‐voltage cathode (ca. 3.74 V versus Na+/Na). The full cell based on this bipolar electrode exhibits well‐defined voltage plateaus near 3.10 V, which is the highest average voltage in the symmetric cells. It also shows the longest cycle life (75.9 % capacity retention after 1000 cycles) in all sodium full cells, a usable capacity of 92 mAh g?1, and superior rate capability (65 mAh g?1 at a high rate of 2C). 相似文献
12.
Dr. Jie Gao Michael A. Lowe Sean Conte Stephen E. Burkhardt Prof. Héctor D. Abruña 《Chemistry (Weinheim an der Bergstrasse, Germany)》2012,18(27):8521-8526
Organosulfur compounds with multiple thiol groups are promising for high gravimetric energy density electrochemical energy storage. We have synthesized a poly(2,5‐dimercapto‐1,3,4‐thiadiazole) (PDMcT)/poly(3,4‐ethylenedioxythiophene) (PEDOT) composite cathode for lithium‐ion batteries with a new method and investigated its electrochemical behavior by charge/discharge cycles and cyclic voltammetry (CV) in an ether‐based electrolyte. Based on a comparison of the electrochemical performance with a carbonate‐based electrolyte, we found a much higher discharge capacity, but also a very attractive cycling performance of PDMcT by using a tetra(ethylene glycol) dimethyl ether (TEGDME)‐based electrolyte. The first discharge capacity of the as‐synthesized PDMcT/PEDOT composite approached 210 mAh g?1 in the TEGDME‐based electrolyte. CV results clearly show that the redox reactions of PDMcT are highly reversible in this TEGDME‐based electrolyte. The reversible capacity remained around 120 mAh g?1 after 20 charge/discharge cycles. With improved cycling performance and very low cost, PDMcT could become a very promising cathode material when combined with a TEGDME‐based electrolyte. The poor capacity in the carbonate‐based electrolyte is a consequence of the irreversible reaction of the DMcT monomer and dimer with the solvent, emphasizing the importance of electrolyte chemistry when studying molecular‐based battery materials. 相似文献
13.
Xiangsi Liu Wenhua Zuo Bizhu Zheng Yuxuan Xiang Ke Zhou Zhumei Xiao Peizhao Shan Jingwen Shi Qi Li Guiming Zhong Riqiang Fu Yong Yang 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2019,131(50):18254-18263
Sodium layered P2‐stacking Na0.67MnO2 materials have shown great promise for sodium‐ion batteries. However, the undesired Jahn–Teller effect of the Mn4+/Mn3+ redox couple and multiple biphasic structural transitions during charge/discharge of the materials lead to anisotropic structure expansion and rapid capacity decay. Herein, by introducing abundant Al into the transition‐metal layers to decrease the number of Mn3+, we obtain the low cost pure P2‐type Na0.67AlxMn1?xO2 (x=0.05, 0.1 and 0.2) materials with high structural stability and promising performance. The Al‐doping effect on the long/short range structural evolutions and electrochemical performances is further investigated by combining in situ synchrotron XRD and solid‐state NMR techniques. Our results reveal that Al‐doping alleviates the phase transformations thus giving rise to better cycling life, and leads to a larger spacing of Na+ layer thus producing a remarkable rate capability of 96 mAh g‐1 at 1200 mA g‐1. 相似文献
14.
Xiangsi Liu Wenhua Zuo Bizhu Zheng Yuxuan Xiang Ke Zhou Zhumei Xiao Peizhao Shan Jingwen Shi Qi Li Guiming Zhong Riqiang Fu Yong Yang 《Angewandte Chemie (International ed. in English)》2019,58(50):18086-18095
Sodium layered P2‐stacking Na0.67MnO2 materials have shown great promise for sodium‐ion batteries. However, the undesired Jahn–Teller effect of the Mn4+/Mn3+ redox couple and multiple biphasic structural transitions during charge/discharge of the materials lead to anisotropic structure expansion and rapid capacity decay. Herein, by introducing abundant Al into the transition‐metal layers to decrease the number of Mn3+, we obtain the low cost pure P2‐type Na0.67AlxMn1?xO2 (x=0.05, 0.1 and 0.2) materials with high structural stability and promising performance. The Al‐doping effect on the long/short range structural evolutions and electrochemical performances is further investigated by combining in situ synchrotron XRD and solid‐state NMR techniques. Our results reveal that Al‐doping alleviates the phase transformations thus giving rise to better cycling life, and leads to a larger spacing of Na+ layer thus producing a remarkable rate capability of 96 mAh g‐1 at 1200 mA g‐1. 相似文献
15.
Dr. Shenglai Yao Dr. Yun Xiong Dr. Tibor Szilvási Prof. Dr. Hansjörg Grützmacher Prof. Dr. Matthias Driess 《Angewandte Chemie (International ed. in English)》2016,55(15):4781-4785
The first 4π‐electron resonance‐stabilized 1,3‐digerma‐2,4‐diphosphacyclobutadiene [LH2Ge2P2] 4 (LH=CH[CHNDipp]2 Dipp=2,6‐iPr2C6H3) with four‐coordinate germanium supported by a β‐diketiminate ligand and two‐coordinate phosphorus atoms has been synthesized from the unprecedented phosphaketenyl‐functionalized N‐heterocyclic germylene [LHGe‐P=C=O] 2 a prepared by salt‐metathesis reaction of sodium phosphaethynolate (P≡C?ONa) with the corresponding chlorogermylene [LHGeCl] 1 a . Under UV/Vis light irradiation at ambient temperature, release of CO from the P=C=O group of 2 a leads to the elusive germanium–phosphorus triply bonded species [LHGe≡P] 3 a , which dimerizes spontaneously to yield black crystals of 4 as isolable product in 67 % yield. Notably, release of CO from the bulkier substituted [LtBuGe‐P=C=O] 2 b (LtBu=CH[C(tBu)N‐Dipp]2) furnishes, under concomitant extrusion of the diimine [Dipp‐NC(tBu)]2, the bis‐N,P‐heterocyclic germylene [DippNC(tBu)C(H)PGe]2 5 . 相似文献
16.
Yu‐Ling Wang Qing‐Yan Liu Li Xu 《Acta Crystallographica. Section C, Structural Chemistry》2007,63(7):m304-m307
The crystal structure of the title compound, {[Tm(C8H3O7S)(H2O)5]·1.5C10H8N2·0.5H2O}n, is built up from two [Tm(SIP)(H2O)5] molecules (SIP3− is 5‐sulfonatobenzene‐1,3‐dicarboxylate), three 4,4′‐bipyridyl (bpy) molecules and one solvent water molecule. One of the bpy molecules and the solvent water molecule are located on an inversion centre and a twofold rotation axis, respectively. The TmIII ion coordination is composed of four carboxylate O atoms from two trianionic SIP3− ligands and five coordinated water molecules. The Tm3+ ions are linked by the SIP3− ligands to form a one‐dimensional zigzag chain propagating along the c axis. The chains are linked by interchain O—H...O hydrogen bonds to generate a two‐dimensional layered structure. The bpy molecules are not involved in coordination but are linked by O—H...N hydrogen bonds to form two‐dimensional layers. The two‐dimensional layers are further bridged by the bpy molecules as pillars and the solvent water molecules through hydrogen bonds, giving a three‐dimensional supramolecular structure. π–π stacking interactions between the parallel aromatic rings, arranged in an offset fashion with a face‐to‐face distance of 3.566 (1) Å, are observed in the crystal packing. 相似文献
17.
The synthesis of a metal–organic framework (MOF) named IITI‐1 is reported by employing an H2L linker with Cu(NO3)2?3 H2O in a mixed solvent system of N,N‐dimethyl formamide (DMF) and H2O. Further, in order to explore the energy storage application of IITI‐1 , a IITI‐1/CNT hybrid was prepared by a simple ultrasonication technique. Incorporation of a carbon nanotube (CNT) in the layered IITI‐1 MOF gave rise to enhanced electrolyte accessibility along with improved electrochemical storage capacity. The electrochemical investigations reveal a high specific capacitance (380 F g?1 at 1.6 A g?1) with a good rate performance for IITI‐1/CNT . The IITI‐1 MOF and the IITI‐1/CNT composite were characterized by PXRD, BET, SEM, and TEM techniques. Moreover, IITI‐1 MOF was also confirmed by single‐crystal XRD analysis. 相似文献
18.
Crosslinked P(VDF‐CTFE)/PS‐COOH nanocomposites for high‐energy‐density capacitor application
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Yingxin Chen Xin Tang Jie Shu Xiaoliang Wang Wenbing Hu Qun‐Dong Shen 《Journal of Polymer Science.Polymer Physics》2016,54(12):1160-1169
High‐capacity or high‐power‐density capacitors are being actively investigated for portable electronics, electric vehicles, and electric power systems. The dielectric nanocomposite with a small loading of carboxylic polystyrene (PS‐COOH) nanoparticles in poly(vinylidene fluoride‐chlorotrifluoroethylene) [P(VDF‐CTFE)] matrix, followed by chemical crosslinking has been described. Combination of these two methods significantly improved the capacity of electric energy storage at low electric field. Specially, the nanocomposite with 2 wt % nanoparticles and 15 wt % crosslinking agent achieved a dielectric constant of 17.2 and a discharged energy density of 17.5 J/cm3 (4.9 Wh/L) at an electric field as high as 324 MV/m, while corresponding values for pristine P(VDF‐CTFE) are 9.6 and 13.3 J/cm3 (3.7 Wh/L), respectively. Fundamental physics underlying the enhancement in the performance of the nanocomposites with respect to P(VDF‐CTFE) is illustrated by solid‐state 19F nuclear magnetic resonance of direct excitation or 19F{1H} cross polarization. It revealed different dynamics behavior between crystalline/amorphous regions, and PS‐COOH nanoparticles favored the formation of polar γ‐form crystals. Small‐angle X‐ray scattering studies revealed the contribution of the interface to the extraordinary storage of electric energies in the nanocomposites. This approach provided a facile and straightforward way to design or understand PVDF‐based polymers for their practical applications in high‐energy‐density capacitors. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2016 , 54, 1160–1169 相似文献
19.
Peilei Yang Chaoyang Zhang Malin Li Xu Yang Prof. Dr. Chunzhong Wang Dr. Xiaofei Bie Prof. Dr. Yingjin Wei Prof. Dr. Gang Chen Prof. Dr. Fei Du 《Chemphyschem》2015,16(16):3408-3412
As a promising positive electrode material for sodium‐ion batteries (SIBs), layered sodium oxides have attracted considerable attention in recent years. In this work, stoichiometric P2‐phase NaCo0.5Mn0.5O2 was prepared through the conventional solid‐state reaction, and its structural and physical properties were studied in terms of XRD, XPS, and magnetic susceptibility. Furthermore, the P2‐NaCo0.5Mn0.5O2 electrode delivered a discharge capacity of 124.3 mA h g?1 and almost 100 % initial coulombic efficiency over the potential window of 1.5–4.15 V. It also showed good cycle stability, with a reversible capacity and capacity retention reaching approximately 85 mA h g?1 and 99 %, respectively, at the 5 C rate after 100 cycles. Additionally, cyclic voltammetry and ex situ XRD were employed to explain the electrochemical behavior at the different electrochemical stages. Owing to the applicable performances, P2‐NaCo0.5Mn0.5O2 can be considered as a potential positive electrode material for SIBs. 相似文献
20.
Graham Smith Urs D. Wermuth 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(5):534-537
The structures of two ammonium salts of 3‐carboxy‐4‐hydroxybenzenesulfonic acid (5‐sulfosalicylic acid, 5‐SSA) have been determined at 200 K. In the 1:1 hydrated salt, ammonium 3‐carboxy‐4‐hydroxybenzenesulfonate monohydrate, NH4+·C7H5O6S−·H2O, (I), the 5‐SSA− monoanions give two types of head‐to‐tail laterally linked cyclic hydrogen‐bonding associations, both with graph‐set R44(20). The first involves both carboxylic acid O—H...Owater and water O—H...Osulfonate hydrogen bonds at one end, and ammonium N—H...Osulfonate and N—H...Ocarboxy hydrogen bonds at the other. The second association is centrosymmetric, with end linkages through water O—H...Osulfonate hydrogen bonds. These conjoined units form stacks down c and are extended into a three‐dimensional framework structure through N—H...O and water O—H...O hydrogen bonds to sulfonate O‐atom acceptors. Anhydrous triammonium 3‐carboxy‐4‐hydroxybenzenesulfonate 3‐carboxylato‐4‐hydroxybenzenesulfonate, 3NH4+·C7H4O6S2−·C7H5O6S−, (II), is unusual, having both dianionic 5‐SSA2− and monoanionic 5‐SSA− species. These are linked by a carboxylic acid O—H...O hydrogen bond and, together with the three ammonium cations (two on general sites and the third comprising two independent half‐cations lying on crystallographic twofold rotation axes), give a pseudo‐centrosymmetric asymmetric unit. Cation–anion hydrogen bonding within this layered unit involves a cyclic R33(8) association which, together with extensive peripheral N—H...O hydrogen bonding involving both sulfonate and carboxy/carboxylate acceptors, gives a three‐dimensional framework structure. This work further demonstrates the utility of the 5‐SSA− monoanion for the generation of stable hydrogen‐bonded crystalline materials, and provides the structure of a dianionic 5‐SSA2− species of which there are only a few examples in the crystallographic literature. 相似文献