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Polyetherketoneketone/carbon fiber composites with an amorphous interface prepared by solution impregnation 通过溶液浸渍法制备具有无定形界面的聚醚酮酮/碳纤维复合材料
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-08-01 DOI: 10.1016/S1872-5805(22)60646-2

Interfacial adhesion between carbon fibers (CF) and polyetherketoneketone (PEKK) is a key factor that affects the mechanical performances of their composites. It is therefore of great importance to impregnate the CF bundles with PEKK as efficiently as possible. We report that PEKK with a good dispersion in a mixed solution of 4-chlorophenol and 1,2-dichloroethane can be introduced onto CF surfaces by solution impregnation and curing at 280, 320, 340 and 360 °C. The excellent wettability or infiltration of the PEKK solution guarantees a full covering and its tight binding to CFs, making it possible to evaluate the interfacial shear strength (IFSS) with the microdroplet method. The interior of the CF bundles is completely and uniformly filled with PEKK by solution impregnation, leading to a high interlaminar shear strength (ILSS). The maximum IFSS and ILSS reached 107.8 and 99.3 MPa, respectively. Such superior shear properties are ascribed to the formation of amorphous PEKK in the small spaces between CFs.

碳纤维(CF)与聚醚酮酮(PEKK)之间的界面粘附力是影响其复合材料机械性能的关键因素。因此,尽可能有效地将碳纤维束浸渍到 PEKK 中非常重要。我们报告了在 4-氯苯酚和 1,2-二氯乙烷的混合溶液中具有良好分散性的 PEKK 可通过溶液浸渍和在 280、320、340 和 360 °C 下固化的方法引入 CF 表面。PEKK 溶液极佳的润湿性或浸润性保证了它的全面覆盖和与 CF 的紧密结合,这使得用微滴法评估界面剪切强度(IFSS)成为可能。通过溶液浸渍,CF 束的内部完全均匀地充满了 PEKK,从而获得了很高的层间剪切强度(ILSS)。最大层间剪切强度(IFSS)和层间剪切强度(ILSS)分别达到 107.8 和 99.3 兆帕。这种优异的剪切性能归因于在 CF 之间的小空隙中形成了无定形 PEKK。
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引用次数: 0
Preparation of a high-performance synthetic pitch from aromatic hydrocarbons containing N/Cl 用含 N/Cl 的芳香烃制备高性能合成沥青
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-08-01 DOI: 10.1016/S1872-5805(24)60864-4

The preparation of a synthetic pitch from aromatic monomers could easily regulate structure orientation at the molecular level, which would be useful in fabrication. An isotropic synthetic pitch was prepared by a chlorine- and/or nitrogen-induced substitution polymerization reaction method using aromatic hydrocarbon precursors containing Cl and N, which for this study were chloromethyl naphthalene and quinoline. This method was verified by investigating the structural changes under different synthesis conditions, and the synthesis mechanism induced by aromatics containing Cl was also probed. The result shows that the pyridinic N in quinoline contains a lone pair of electrons, and is an effective active site to induce the polymerization reaction by coupling with aromatic hydrocarbons containing Cl. The reaction between such free radicals causes strong homopolymerization and oligomerization. A higher reaction temperature and longer reaction time significantly increased the degree of polymerization and thus increased the softening point of the pitch. A linear molecular structure was formed by the Cl substitution reaction, which produced a highly spinnable pitch with a softening point of 258.6 °C, and carbon fibers with a tensile strength of 1 163.82 MPa were obtained. This study provides a relatively simple and safe method for the preparation of high-quality spinnable pitch.

用芳香族单体制备合成沥青可以在分子水平上轻松调节结构取向,这在制造过程中非常有用。本研究采用氯和/或氮诱导的取代聚合反应方法,使用含 Cl 和 N 的芳香烃前体(本研究使用的是氯甲基萘和喹啉)制备了各向同性合成沥青。通过研究不同合成条件下的结构变化,验证了该方法的有效性,并探究了含 Cl 芳烃诱导的合成机理。结果表明,喹啉中的吡啶 N 含有一对孤对电子,是与含 Cl 的芳香烃偶联诱导聚合反应的有效活性位点。这种自由基之间的反应会引起强烈的均聚和低聚作用。较高的反应温度和较长的反应时间可显著提高聚合度,从而提高沥青的软化点。通过 Cl 取代反应形成了线性分子结构,产生了软化点为 258.6 °C 的高可纺性沥青,并获得了拉伸强度为 1 163.82 MPa 的碳纤维。这项研究为制备高质量可纺沥青提供了一种相对简单和安全的方法。
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引用次数: 0
A review of the catalytic preparation of mesophase pitch 介相沥青催化制备综述
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-08-01 DOI: 10.1016/S1872-5805(24)60862-0

Because of its high purity and excellent orientation, mesophase pitch is a superior precursor for high-performance carbon materials. However, the preparation of top-notch mesophase pitch faces challenges. Catalytic polycondensation at low temperatures is more favorable for synthesizing mesophase pitch, because it circumvents the high-temperature free radical reaction of other thermal polycondensation approaches. The reaction is gentle and can be easily controlled. It has the potential to significantly improve the yield of mesophase pitch and easily introduce naphthenic characteristics into the molecules, catalytic polycondensation is therefore a preferred method of synthesizing highly spinnable mesophase pitch. This review provides a synopsis of the selective pretreatment of the raw materials to prepare different mesophase pitches, and explains the reaction mechanism and associated research advances for different catalytic systems in recent years. Finally, how to manufacture high-quality mesophase pitch by using a catalyst-promoter system is summarized and proposed, which may provide a theoretical basis for the future design of high-quality pitch molecules.

介相沥青纯度高、取向性好,是高性能碳材料的优质前驱体。然而,顶级介相沥青的制备面临着挑战。低温催化缩聚更有利于合成介相沥青,因为它避免了其他热缩聚方法的高温自由基反应。反应温和,易于控制。因此,催化缩聚是合成高可纺性介相沥青的首选方法。本综述概述了制备不同介相沥青的原材料选择性预处理方法,并解释了近年来不同催化体系的反应机理和相关研究进展。最后,总结并提出了如何利用催化剂-促进剂体系制造高品质介相沥青,为今后设计高品质沥青分子提供理论依据。
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引用次数: 0
Increasing the toughness while reducing the viscosity of carbon nano-tube/polyether imide/polyether ether ketone nanocomposites 在降低碳纳米管/聚醚酰亚胺/聚醚醚酮纳米复合材料粘度的同时提高其韧性
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-08-01 DOI: 10.1016/S1872-5805(22)60643-7

Polyether ether ketone (PEEK) has good mechanical properties. However, its high viscosity when molten limits its use because it is hard to process. PEEK nanocomposites containing both carbon nanotubes (CNTs) and polyether imide (PEI) were prepared by a direct wet powder blending method using a vertical injection molding machine. The addition of an optimum amount of PEI lowered the viscosity of the molten PEEK by approximately 50% while producing an increase in the toughness of the nanocomposites, whose strain to failure increased by 129%, and fracture energy increased by 97%. The uniformly dispersed CNT/PEI powder reduced the processing difficulty of PEEK nanocomposites without affecting the thermal resistance. This improvement of the strength and viscosity of PEEK facilitate its use in the preparation of thermoplastic composites.

聚醚醚酮(PEEK)具有良好的机械性能。然而,其熔融时的高粘度限制了它的使用,因为它很难加工。使用立式注塑机,通过直接湿粉混合法制备了含有碳纳米管(CNT)和聚醚酰亚胺(PEI)的 PEEK 纳米复合材料。添加最佳量的 PEI 可将熔融 PEEK 的粘度降低约 50%,同时提高纳米复合材料的韧性,其破坏应变提高了 129%,断裂能提高了 97%。均匀分散的 CNT/PEI 粉末降低了 PEEK 纳米复合材料的加工难度,同时不会影响其热阻。PEEK 强度和粘度的提高有助于其在热塑性复合材料制备中的应用。
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引用次数: 0
Semi-quantitative analysis of the structural evolution of mesophase pitch-based carbon foams by Raman and FTIR spectroscopy 利用拉曼光谱和傅立叶变换红外光谱对介相沥青基碳泡沫的结构演变进行半定量分析
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-08-01 DOI: 10.1016/S1872-5805(24)60867-X

Graphitized carbon foams (GFms) were prepared using mesophase pitch (MP) as a raw material by foaming (450 °C), pre-oxidation (320 °C), carbonization (1 000 °C) and graphitization (2 800 °C). The differences in structure and properties of GFms prepared from different MP precursors pretreated by ball milling or liquid phase extraction were investigated and compared, and semi-quantitative calculations were conducted on the Raman and FTIR spectra of samples at each preparation stage. Semi-quantitative spectroscopic analysis provided detailed information on the structure and chemical composition changes of the MP and GFm derived from it. Combined with microscopic observations, the change from precursor to GFm was analyzed. The results showed that ball milling concentrated the distribution of aromatic molecules in the pitch, which contributed to uniform foaming to give a GFm with a uniform pore distribution and good properties. Liquid phase extraction helped remove light components while retaining large aromatics to form graphitic planes with the largest average size during post-treatment to produce a GFm with the highest degree of graphitization and the fewest open pores, giving the best compression resistance (2.47 MPa), the highest thermal conductivity (64.47 W/(m·K)) and the lowest electrical resistance (13.02 μΩ·m). Characterization combining semi-quantitative spectroscopic analysis with microscopic observations allowed us to control the preparation of the MP-derived GFms.

以介相沥青(MP)为原料,通过发泡(450 °C)、预氧化(320 °C)、碳化(1 000 °C)和石墨化(2 800 °C)制备了石墨化碳泡沫(GFms)。通过球磨或液相萃取预处理不同 MP 前体制备的 GFms 的结构和性质差异进行了研究和比较,并对各制备阶段样品的拉曼光谱和傅立叶变换红外光谱进行了半定量计算。半定量光谱分析提供了有关 MP 及其衍生 GFm 结构和化学成分变化的详细信息。结合显微镜观察,分析了从前驱体到 GFm 的变化。结果表明,球磨集中了沥青中芳香分子的分布,有助于均匀发泡,从而得到孔隙分布均匀、性能良好的 GFm。液相萃取有助于去除轻组分,同时保留大芳烃,从而在后处理过程中形成平均尺寸最大的石墨化平面,生产出石墨化程度最高、开放孔隙最少的 GFm,使其具有最佳的抗压性(2.47 兆帕)、最高的热导率(64.47 W/(m-K))和最低的电阻(13.02 μΩ-m)。半定量光谱分析与显微观察相结合的表征方法使我们能够控制 MP 衍生 GFms 的制备。
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引用次数: 0
Increasing the interlayer spacing and generating closed pores to produce petroleum coke-based carbon materials for sodium ion storage 增加层间间距并产生封闭孔隙,以生产用于钠离子储存的石油焦基碳材料
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-06-01 DOI: 10.1016/S1872-5805(24)60858-9
Hong-kun Zhuang, Wen-cui Li, Bin He, Jia-he Lv, Jing-song Wang, Ming-yuan Shen, An-hui Lu

Petroleum coke (PC) is a valuable precursor for sodium-ion battery (SIB) anodes due to its high carbon content and low cost. The regulation of the microcrystalline state and pore structure of the easily-graphitized PC-based carbon is crucial for creating abundant Na+ storage sites. Here we used a precursor transformation strategy to increase the carbon interlayer spacing and generate abundant closed pores in PC-based carbon, significantly increasing its Na+ storage capacity in the plateau region. This was achieved by introducing a large number of oxygen functional groups through mixed acid treatment and then using high-temperature carbonization to decompose the oxygen functional groups and rearrange the carbon microcrystallites, resulting in a transition from open to closed pores. The optimized samples provide a large reversible capacity of 356.0 mAh g−1 at 0.02 A g−1, of which approximately 93% is below 1.0 V. Galvanostatic intermittent titration (GITT) and in-situ X-ray diffraction (XRD) analysis indicate that the sodium storage capacity in the low voltage plateau region involves a joint contribution of interlayer insertion and closed pore filling processes. This study presents a comprehensive method for the development of high-performance carbon anodes using low-cost and highly aromatic precursors.

石油焦(PC)含碳量高且成本低廉,是钠离子电池(SIB)阳极的重要前驱体。调节易石墨化 PC 基碳的微晶状态和孔隙结构对于创造丰富的 Na+ 储存位点至关重要。在此,我们采用了一种前驱体转化策略来增加碳层间间距,并在 PC 基碳中产生大量封闭孔隙,从而显著提高其在高原区的 Na+ 储存能力。这是通过混合酸处理引入大量氧官能团,然后利用高温碳化分解氧官能团并重新排列碳微晶,从而实现从开放孔隙到封闭孔隙的转变。优化后的样品在 0.02 A g-1 的电压下具有 356.0 mAh g-1 的大可逆容量,其中约 93% 的容量低于 1.0 V。电位静态间歇滴定(GITT)和原位 X 射线衍射(XRD)分析表明,低电压高原区的钠存储容量涉及层间插入和闭孔填充过程的共同作用。本研究提出了一种利用低成本高芳香族前驱体开发高性能碳阳极的综合方法。
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引用次数: 0
Electrochemical methods for the removal of impurities from thegraphite anode in spent ternary lithium-ion batteries 去除废旧三元锂离子电池石墨负极中杂质的电化学方法
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-06-01 DOI: 10.1016/S1872-5805(24)60843-7
Rui Zhang , Yong Tian , Wei-li Zhang , Jia-yin Song , Jie Min , Bo Pang , Jian-jun Chen

The use of lithium-ion batteries (LIBs) is becoming increasingly widespread, and a large number are reaching their end of life. The recycling and re-use of spent LIBs has attracted great attention. Because of the unchanged layer structure of the graphite anode in these batteries, their recycling does not require high-temperature graphitization, and only focuses on the removal of internal impurities. We used electrochemical treatment for the deep removal of internal metal impurities after the heat treatment, ultrasonic separation, and acid leaching of spent graphite. By comparing and analyzing the graphite in different recovery stages, it was found that the presence of organic impurities seriously affects the electrochemical performance. The presence of trace inorganic impurities such as Cu and Fe has little effect on the initial discharge specific capacity, but reduces the cycling stability of graphite. The content of the main metal impurities in the final recycled graphite was less than 20 mg/kg. The discharge specific capacity reached358.7 mAh/g at 0.1 C, and the capacity remained at 95.85% after 150 cycles. Compared with the reported methods for recycling spent graphite, this method can efficiently remove impurities in the graphite, solve the current problems of high acid and alkali consumption, incomplete impurity removal and high energy consumption. The recycled graphite anode has a good electrochemical performance. Our work provides a new recycling and regeneration path for spent LIB graphite anodes.

锂离子电池(LIB)的使用越来越广泛,大量电池即将报废。废旧锂离子电池的回收和再利用引起了人们的极大关注。由于这些电池中的石墨负极层结构不变,因此其回收利用不需要高温石墨化,只需要去除内部杂质即可。在对废石墨进行热处理、超声波分离和酸浸后,我们采用电化学处理方法深度去除内部金属杂质。通过对比分析不同回收阶段的石墨,发现有机杂质的存在严重影响了电化学性能。痕量无机杂质(如 Cu 和 Fe)的存在对初始放电比容量影响不大,但会降低石墨的循环稳定性。最终再生石墨中主要金属杂质的含量小于 20 mg/kg。放电比容量在 0.1 C 时达到 358.7 mAh/g,循环 150 次后容量保持在 95.85%。与已报道的废石墨回收方法相比,该方法能有效去除石墨中的杂质,解决了目前废石墨酸碱消耗高、杂质去除不彻底、能耗高等问题。回收后的石墨阳极具有良好的电化学性能。我们的工作为废 LIB 石墨阳极的回收和再生提供了一条新的途径。
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引用次数: 0
Plasma-assisted preparation of NiCoAl-layered double hydroxides with alarge interlayer spacing on carbon cloth forelectrochemical deionization 等离子体辅助制备碳布上具有较大层间距的镍钴铝层双氢氧化物的电化学去离子技术
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-06-01 DOI: 10.1016/S1872-5805(24)60854-1
Qiu-tong Jiang , Guo-qing Wang , Yi Li , Hong-wei Huang , Qian Li , Jian Yang

Capacitive deionization has been considered an emerging desalination technique in recent years, especially for its economic and energy-saving characteristics for brackish water. However, there are currently few studies on chloride ion removal electrodes, and the slow desalination kinetics limits their development. Ar-NiCoAl- layered double hydroxide (LDH)@ACC materials with an increased interlayer spacing were prepared by the in-situ growth of NiCoAl-LDHs nanosheet arrays on acid-treated carbon cloth (ACC) and subsequent Ar plasma treatment. The carbon cloth suppresses the agglomeration of the NiCoAl-LDHs nanosheets and improves the electrical conductivity, while the plasma treatment increases the interlayer spacing of NiCoAl-LDHs and improves its hydrophilicity. This provides rapid diffusion channels and more interlayer active sites for chloride ions, achieving high desalination kinetics. A hybrid capacitive deionization (HCDI) cell was assembled using Ar-NiCoAl-LDHs@ACC as the chloride ion removal electrode and activated carbon as the sodium ion removal electrode. This HCDI cell achieved a high desalination capacity of 93.26 mg g−1 at 1.2 V in a 1000 mg L−1 NaCl solution, a remarkable desalination rate of 0.27 mg g−1 s−1, and a good charge efficiency of 0.97. The capacity retention remained above 85% after 100 cycles in a 300 mg L−1 NaCl solution at 0.8 V. The work provides new ideas for the controlled preparation of two-dimensional metal hydroxide materials with a large interlayer spacing and the design of high-performance electrochemical chlorine ion removal electrodes.

近年来,电容式去离子法一直被认为是一种新兴的海水淡化技术,特别是在苦咸水方面具有经济和节能的特点。然而,目前有关氯离子去除电极的研究很少,而且脱盐动力学缓慢,限制了其发展。通过在酸处理碳布(ACC)上原位生长镍钴铝-层状双氢氧化物(LDH)纳米片阵列并随后进行氩等离子处理,制备了层间距增大的氩镍钴铝-层状双氢氧化物(LDH)@ACC 材料。碳布抑制了镍钴铝-LDHs 纳米片的团聚并提高了导电性,而等离子体处理增加了镍钴铝-LDHs 的层间距并提高了其亲水性。这为氯离子提供了快速扩散通道和更多的层间活性位点,从而实现了较高的脱盐动力学性能。以 Ar-NiCoAl-LDHs@ACC 作为氯离子去除电极,以活性炭作为钠离子去除电极,组装了一个混合电容式去离子(HCDI)电池。在 1000 mg L-1 NaCl 溶液中,该 HCDI 电池在 1.2 V 电压下的脱盐容量高达 93.26 mg g-1,脱盐速率高达 0.27 mg g-1 s-1,充电效率高达 0.97。在 300 mg L-1 NaCl 溶液中以 0.8 V 的电压循环 100 次后,容量保持率仍在 85% 以上。该研究成果为控制制备具有较大层间距的二维金属氢氧化物材料和设计高性能电化学氯离子去除电极提供了新思路。
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引用次数: 0
A review of graphdiyne in aqueous ion batteries 水离子电池中的石墨二炔综述
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-06-01 DOI: 10.1016/S1872-5805(24)60852-8
Xian-min Xu , Wen-cong Feng , Jing-ke Ren , Wen Luo

Graphdiyne is a novel carbon material with a special carbon hybrid arrangement, unique chemical and electronic structure and numerous pores that has promising applications in electrochemical energy storage. Emerging aqueous ion batteries have advantages of low cost and high safety, but the development of high-performance electrode materials, the design of new membrane systems and ways of stabilizing the interface remain the main challenges in their manufacture. With its unique porous structure and excellent electrochemical properties, graphdiyne can improve ion transport, interface deposition behavior and electrolyte instability in the aspects of anode protection, cathode cladding, membrane design and stabilizing the pH value of the interface. A bottom-up molecular structural design strategy makes graphdiyne easy to modify and dope, improving the properties of its analogues and thus expanding their applications in aqueous ion batteries. We systematically summarize the structure, properties, and synthesis methods of graphdiyne, and summarize the research of graphdiyne in aqueous ion batteries. A comprehensive evaluation of the existing problems and challenges of the use of graphdiyne in aqueous ion batteries is given, and future trends and developments are suggested.

Graphdiyne 是一种新型碳材料,具有特殊的碳混合排列、独特的化学和电子结构以及众多孔隙,在电化学储能领域具有广阔的应用前景。新兴的水离子电池具有成本低、安全性高的优点,但高性能电极材料的开发、新型膜系统的设计以及稳定界面的方法仍是其制造过程中的主要挑战。石墨炔具有独特的多孔结构和优异的电化学性能,可在阳极保护、阴极包覆、膜设计和稳定界面 pH 值等方面改善离子传输、界面沉积行为和电解质不稳定性。自下而上的分子结构设计策略使石墨二炔易于改性和掺杂,改善了其类似物的性能,从而扩大了它们在水离子电池中的应用。我们系统地总结了石墨二炔的结构、性能和合成方法,并总结了石墨二炔在水离子电池中的研究。全面评估了石墨二炔在水离子电池中应用的现有问题和挑战,并提出了未来的趋势和发展。
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引用次数: 0
Sulfonyl chloride-intensified metal chloride intercalation of graphite for efficient sodium storage 磺酰氯强化金属氯化物插层石墨,实现高效钠储存
IF 5.7 3区 材料科学 Q2 Materials Science Pub Date : 2024-06-01 DOI: 10.1016/S1872-5805(24)60851-6
Shu-qin Lan , Wei-cheng Ren , Zhao Wang , Chang Yu , Jin-he Yu , Ying-bin Liu , Yuan-yang Xie , Xiu-bo Zhang , Jian-jian Wang , Jie-shan Qiu

Metal chloride-intercalated graphite with excellent conductivity and a large interlayer spacing is highly desired for use in sodium ion batteries. However, halogen vapor is usually indispensable in initiating the intercalation process, which makes equipment design and experiments challenging. In this work, SO2Cl2 was used as a chlorine generator to intensify the intercalation of BiCl3 into graphite (BiCl3-GICs), which avoided the potential risks, such as Cl2 leakage, in traditional methods. The operational efficiency in the experiment was also improved. After the reaction of SO2Cl2, BiCl3, and graphite at 200 oC for 20 h, the synthesized BiCl3-GICs had a large interlayer spacing (1.26 nm) and a high amount of BiCl3 intercalation (42%), which gave SIBs a high specific capacity of 213 mAh g−1 at 1 A g−1 and an excellent rate performance (170 mAh g−1 at 5 A g−1). In-situ Raman spectra revealed that the electronic interaction between graphite and intercalated BiCl3 is weakened during the first discharge, which is favorable for sodium storage. This work broadly enables the increased intercalation of other metal chloride-intercalated graphites, offering possibilities for developing advanced energy storage devices.

具有优异导电性和较大层间距的金属氯化物插层石墨非常适合用于钠离子电池。然而,卤素蒸汽通常是启动插层过程不可或缺的因素,这使得设备设计和实验具有挑战性。在这项工作中,使用 SO2Cl2 作为氯气发生器来强化 BiCl3 在石墨中的插层(BiCl3-GICs),避免了传统方法中 Cl2 泄漏等潜在风险。实验的运行效率也得到了提高。将 SO2Cl2、BiCl3 和石墨在 200 oC 下反应 20 h 后,合成的 BiCl3-GICs 具有较大的层间距(1.26 nm)和较高的 BiCl3 插层量(42%),从而使 SIBs 在 1 A g-1 时具有 213 mAh g-1 的高比容量和优异的速率性能(5 A g-1 时为 170 mAh g-1)。原位拉曼光谱显示,石墨与插层 BiCl3 之间的电子相互作用在第一次放电过程中减弱,这有利于钠的储存。这项研究成果广泛地促进了其他金属氯化物插层石墨的插层,为开发先进的储能设备提供了可能性。
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引用次数: 0
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New Carbon Materials
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