先进储钠电极材料及其电化学储能应用
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摘要
钠离子电池具有资源丰富、成本低廉、环境友好等特点，被认为是替代锂离子电池作为下一代电动汽车动力电源及大规模储能电站配套电源的理想选择。因此，探寻高容量及优异循环性能的储钠电极材料已成为目前电池领域的研究热点。本论文旨在探索钠离子电池正负极材料新体系，主要研究内容和结果如下：
1.本论文首次提出采用过渡金属六氰配合物Na_4Fe(CN)_6及NaxMyFe(CN)_6M=(Fe，Co，Ni，Mn)作为钠离子电池正极材料。采用高能球磨法制备了Na_4Fe(CN)_6/C纳米复合物，该材料能实现理论上1个Na+的可逆脱嵌容量87mAhg~(-1)，电压平台为3.4V；在10C倍率下，仍可给出理论比容量的45%；500周循环容量保持率为88%，并具有卓越的大电流充放电性能和优异的长期循环稳定性。另外，采用溶液沉淀法制备了四种普鲁士蓝类钠盐NaxMyFe(CN)_6(M=Fe，Co，Ni，Mn)。电化学测试结果表明，当M为Fe、Co、Mn时，材料中Fe(CN)_64-和金属M离子两个活性中心都参与电化学氧化还原反应，首周可逆容量分别为113mAh g~(-1)、120mAh g~(-1)和113mAh g~(-1)，循环比较稳定。当M为Ni时，普鲁士蓝类材料的可逆容量仅为64mAh g~(-1)，但循环性能非常优异。这类无机配合物的可逆嵌钠能力为探索钠离子电池正极材料提供了新体系.
2.以聚苯胺(PAn)和聚三苯胺(PTPAn)两种共轭聚合材料为代表，本论文初步探索了聚合物储钠正极材料的可行性。采用化学氧化法合成了这两种聚合物材料，并研究了它们的结构、反应机理及电化学储钠性能。实验结果表明：这类聚合物的电化学氧化还原反应通过阴离子的掺杂/脱掺杂而实现； PAn电极在钠离子电解液中的首周放电比容量高达163mAh g~(-1),平均放电电压为3.16V，100周循环后容量稳定在118mAh g~(-1)。以300mA g~(-1)电流密度充放电，可逆容量仍有60mAh g~(-1)，超过了现有的无机正极材料；PTPAn电极在钠离子电解液中的首周放电容量93mAh g~(-1)，接近于理论上1个电子的转移反应，平均放电电压为3.56V；在500mA g~(-1)的大电流密度下充放电，可逆容量仍高达72mAh g~(-1)。由此可见，导电聚合物具有优异的循环稳定性和大电流充放电性能，且制备方法简单，原料易得，有望发展成为兼具高能量密度和高功率密度的钠离子电池正极材料。
3.为了寻找合适的嵌钠负极材料，本论文工作研究了几类不同碳材料的嵌钠行为和反应机理，进而发现硬碳类负极材料具有较好的储钠性能。无定形排列的碳层以及结构中的纳米微孔都可作为钠离子嵌入的活性位点，并具有不同的嵌钠电位。基于实验比较，本工作主要采用聚氯乙烯PVC和聚苯胺PAn两种聚合物为前驱体，通过改变煅烧条件来优化其储钠性能。结果表明：控制升温速率为1℃/min，煅烧温度为700℃，保温时间为2h制备的PVC热解碳具有最佳的储钠性能。该材料首周可逆容量为200mAh g~(-1)，循环100周后容量保持率为85%；在200mAg~(-1)电流密度下，仍有117mAh g~(-1)的可逆容量。采用聚苯胺(PAn)为前驱体制备的热解碳材料首周可逆脱钠容量为194mAh g~(-1)，循环200周后容量保持率为97%；在500mA g~(-1)下，可逆容量仍有103mAh g~(-1)，具有优异的储钠性能和循环稳定性。这些结果表明，通过调整碳材料的结构，包括体相晶格、尺寸形貌、表面织构和结构缺陷等，有望获得高性能的碳基储钠负极材料，以满足钠离子电池的实用化要求。
4.为了寻找更高性能的嵌钠负极材料，本论文将目光转向合金类负极材料。理论上，Na可与Sn、P、Sb等元素形成Na15Sn4(847mAh g~(-1))，Na3P(2596mAh g~(-1))，和Na3Sb (660mAh g~(-1))化合物，具有超常的理论比容量。但是，这些合金类负极材料在嵌脱钠过程中的体积变化巨大（Sn→Na15Sn4膨胀525%），容易引起材料粉化，丧失电化学活性，导致其无法直接用作钠离子电池负极材料。为了限制体积膨胀对电极的冲击，本论文工作采用纳米化、核壳结构、无定形化和碳包覆等手段进行改性研究。首先，采用原位置换法制备了核壳结构的Sn@Cu纳米复合物，利用表面包覆Cu的限制作用，缓解Na-Sn合金化过程的体积膨胀。该材料的可逆储钠容量为290mAh g~(-1)，20周循环后仍保持在200mAh g~(-1)以上。其次，以红磷和高比表面碳载体为原料，制备了无定形磷/碳复合物，该材料可逆储钠容量高达1764mAh g~(-1)，40周后容量保持率为96.7%，表现出优异的循环稳定性；并且在4000mA g~(-1)的超大电流密度下，放电容量仍有1725mAh g~(-1)，具有非常卓越的脱钠反应动力学。再次，采用高能球磨法制备了Sn4P3/C纳米复合材料，该材料的可逆储钠容量高达816mAh g~(-1)，实现了接近于理论24个Na离子的嵌入反应，100周后容量保持率为89%。最后，将单质Sb纳米化并分散在碳载体中制备了Sb/C纳米复合物，该材料实现了接近3个Na离子的可逆合金化反应，并具有优异的大电流充放电性能。另外，通过优化电解液的组成，加入5%的SEI成膜剂-FEC，使得Sb/C纳米复合电极经循环100周后容量保持率为95%，表现出非常优异的长期循环稳定性。以上工作证明了锡Sn，磷P，磷化锡Sn4P3和锑Sb四种材料都具有非常高的储钠容量、良好的倍率性能以及优异的循环稳定性，并且制备方法简单，原料易得，为发展实用化的高性能钠离子电池负极材料提供了可借鉴的经验和广阔的研究空间。
Sodium ion batteries are now actively pursued as the most attractive alternativeto Li-ion batteries for electric vehicle propulsion and renewable electric power storage,because of their potential advantages of low cost and widespread availability ofsodium resources. To realize Na-ion technology, a critical issue is to find out suitablehost materials that can accommodate sufficient Na ions for reversible electrochemicalinsertion reaction. In this thesis, we were aimed at exploring new anode and cathodematerials and optimize their performance to realize their potentionally high redoxcapacity for reversible Na-storage。The main results and new findings in this work aresummarized as follows：
1. A new family of sodium transition metal cyanides, such as hexacyanoferratesNa_4Fe(CN)_6and Prussian blue NaxMyFe(CN)_6(M=Fe，Co，Ni，Mn) were proposed ascathode materials for sodium ion batteries. Firstly, a Na_4Fe(CN)_6/C nanocompositewere prepared simply by mechanical ball-milling Na_4Fe(CN)_6and conductive carbonpowders. The as-prepared Na_4Fe(CN)_6/C composite displays a full utilization of itsredox capacity of87mAh g~(-1)at a high potential of~3.4V, an excellent cyclingstability with a88%capacity retention over500cycles and a superior high ratecapability with45%capacity delivery at a10C rate. Secondly, four types of Prussianblue NaxMyFe(CN)_6(M=Fe, Co, Ni, Mn) compounds were prepared simply bysolution precipitation method and tested as cathode materials for sodium-ion batteries.Electrochemical tests revealed very different electrochemical behaviors of these foursamples of NaxMyFe(CN)_6(M=Fe, Co, Ni, Mn). When M was Fe, Co and Mn, thespecific capacities of NaxFeyFe(CN)_6, NaxCoyFe(CN)_6and NaxMnyFe(CN)_6can reach113,120and113mAh g~(-1), respectively, indicating that both of the Fe(CN)_64-and M+2ions in the Prussian blue lattices were electrochemically activated. When M was Ni,Ni ions in the Prussian blue lattice was found to be electrochemically inactive and theNaxNiyFe(CN)_6delivered a specific capacity of only64mAh g~(-1)but with quite stablecyclability. These results suggest a possible use of the transition metal cyanides as lowcost and environmentally benign cathode materials for sodium-ion batteries.
2. Two typical conductive polymers: Polyaniline (PAn) and Polytriphenylamine(PTPAn) were chemically synthesized and suggested as promising cathode materials for sodium ion batteries, due to their good conductivity and electrochemical redoxproperty. It was found Na/PAn cell displays a quite high capacity of163mAh g~(-1)at anaverage discharge voltage of3.16V, an excellent cycling stability with118mAh g~(-1)reserved after100cycles and a superior high rate capability with60mAh g~(-1)deliveryat300mA g~(-1)current density, exceeding most of the current inorganic cathodes;Na/PTPAn cells also give a high capacity of93mAh g~(-1)and a quite high averagedischarge voltage of3.56V. Even cycled at a very high rate of500mA g~(-1), thepolymer can still deliver a capacity of72mAh g~(-1), that is78%of initial capacity.Overall, these conductive polymers can realize their potential high redox capacitieswith sufficient cycleability and superior high power capability, suggesting a promisingcathode for high energy density and power density sodium ion batteries.
3. In the search for suitable Na host materials for sodium ion batteries, weinvestigated the electrochemical sodium insertion behavior of several types ofcarbonaceous materials. Hard carbon materials were found to possess the best sodiuminsertion performance, as they contain random stacked carbon layers and significantquantities of nanosized pores, which can serve as active sites for sodium insertion.Base on these results, two kinds of polymers: polyvinyl chloride (PVC andpolyaniline (PAn, were selected as the precursors to make pyrolyzed hard carbon,and their performance were optimized by adjusting proper calcination condition. Itwas found that the PVC electrode can deliver quite a high reversible capacity of~200mAh g~(-1), corresponding to the formation of Na0.54C6, an excellent cycling stabilitywith85%reserved after100cycles and a high rate capability with117mAh g~(-1)delivered at a current density of200mA g~(-1). The PAn-pyrolysed carbon can also givea high capacity of194mAh g~(-1), and97%capacity reserved at200th cycle, and ahigh rate capability with103mAh g~(-1)delivery at500mA g~(-1). In principle, highperformance carbon anodes can be achieved by adjusting the structure of carbonmaterials, including crystal lattice, surface texture, and structural defect, so as to meetthe practical requirements of the sodium ion batteries.
4. Sodium alloying reactions with metals or semi-metals would be an effective wayto provide larger specific capacity and suitable thermodynamic potentials than carbonbased materials. For example, Na can alloy with Sn, P, Sb elements to produceNa15Sn4(847mAh g~(-1), Na3P (2560mAh g~(-1), and Na3Sb (660mAh g~(-1), respectively.In order to suppress enormous volume changes (i.e., a525%volume increase ongoing from Sn to Na15Sn4during sodium alloying reaction, several strategies, such as nanosizing, core-shell structure, amorphisizing and carbon coating, were adopted tooptimize their performances. Firstly, core-shell structured Sn@Cu nanocomposite wassynthesized by a simple substitutional reaction between Sn and Cu2+. The as preparedSn@Cu material can give an enhanced capacity of290mAh g~(-1), with200mAh g~(~(-1))reserved after20cycles. Secondly, an amorphous P/C nanocomposite was simplyprepared by mechanical ball-milling red P and conductive carbon powders. The a-P/Ccomposite displays an quite high capacity of1764mAh g~(-1)，an excellent cyclingstability with96.7%reserved after40cycles, and a superior fast sodiumdeintercalation kinetics with1725mAh g~(-1)achieved at a current density of4000mAg~(-1). Thirdly, a Sn4P3/C nanocomposite was synthesized by ball-milling method, andcan exhibit a reversible capacity of816mAh g~(-1), approaching to its theoretical24Na-storage capacity and retain89%of initial capacity after100cycles. Finally, weprepared a novel Sb/C nanocomposite, simply by mechanical ball-milling commercialSb powder with conductive carbon, which demonstrates a nearly full utilization of itstheoretical3Na storage capacity, a strong rate capability with50%capacity realizedat a very a very high current of2000mA g~(-1). Particularly, in the optimized electrolytewith a SEI film-forming additive, the Sb/C anode demonstrates a long-term cyclingstability with94%capacity retention over100cycles. Overall, these excellentelectrochemical performances of four samples represent the highest level of the Nastorage materials, offering a practical feasibility as a high capacity and cycling-stableanode for room temperature Na-ion batteries.
1.本论文首次提出采用过渡金属六氰配合物Na_4Fe(CN)_6及NaxMyFe(CN)_6M=(Fe，Co，Ni，Mn)作为钠离子电池正极材料。采用高能球磨法制备了Na_4Fe(CN)_6/C纳米复合物，该材料能实现理论上1个Na+的可逆脱嵌容量87mAhg~(-1)，电压平台为3.4V；在10C倍率下，仍可给出理论比容量的45%；500周循环容量保持率为88%，并具有卓越的大电流充放电性能和优异的长期循环稳定性。另外，采用溶液沉淀法制备了四种普鲁士蓝类钠盐NaxMyFe(CN)_6(M=Fe，Co，Ni，Mn)。电化学测试结果表明，当M为Fe、Co、Mn时，材料中Fe(CN)_64-和金属M离子两个活性中心都参与电化学氧化还原反应，首周可逆容量分别为113mAh g~(-1)、120mAh g~(-1)和113mAh g~(-1)，循环比较稳定。当M为Ni时，普鲁士蓝类材料的可逆容量仅为64mAh g~(-1)，但循环性能非常优异。这类无机配合物的可逆嵌钠能力为探索钠离子电池正极材料提供了新体系.
2.以聚苯胺(PAn)和聚三苯胺(PTPAn)两种共轭聚合材料为代表，本论文初步探索了聚合物储钠正极材料的可行性。采用化学氧化法合成了这两种聚合物材料，并研究了它们的结构、反应机理及电化学储钠性能。实验结果表明：这类聚合物的电化学氧化还原反应通过阴离子的掺杂/脱掺杂而实现； PAn电极在钠离子电解液中的首周放电比容量高达163mAh g~(-1),平均放电电压为3.16V，100周循环后容量稳定在118mAh g~(-1)。以300mA g~(-1)电流密度充放电，可逆容量仍有60mAh g~(-1)，超过了现有的无机正极材料；PTPAn电极在钠离子电解液中的首周放电容量93mAh g~(-1)，接近于理论上1个电子的转移反应，平均放电电压为3.56V；在500mA g~(-1)的大电流密度下充放电，可逆容量仍高达72mAh g~(-1)。由此可见，导电聚合物具有优异的循环稳定性和大电流充放电性能，且制备方法简单，原料易得，有望发展成为兼具高能量密度和高功率密度的钠离子电池正极材料。
3.为了寻找合适的嵌钠负极材料，本论文工作研究了几类不同碳材料的嵌钠行为和反应机理，进而发现硬碳类负极材料具有较好的储钠性能。无定形排列的碳层以及结构中的纳米微孔都可作为钠离子嵌入的活性位点，并具有不同的嵌钠电位。基于实验比较，本工作主要采用聚氯乙烯PVC和聚苯胺PAn两种聚合物为前驱体，通过改变煅烧条件来优化其储钠性能。结果表明：控制升温速率为1℃/min，煅烧温度为700℃，保温时间为2h制备的PVC热解碳具有最佳的储钠性能。该材料首周可逆容量为200mAh g~(-1)，循环100周后容量保持率为85%；在200mAg~(-1)电流密度下，仍有117mAh g~(-1)的可逆容量。采用聚苯胺(PAn)为前驱体制备的热解碳材料首周可逆脱钠容量为194mAh g~(-1)，循环200周后容量保持率为97%；在500mA g~(-1)下，可逆容量仍有103mAh g~(-1)，具有优异的储钠性能和循环稳定性。这些结果表明，通过调整碳材料的结构，包括体相晶格、尺寸形貌、表面织构和结构缺陷等，有望获得高性能的碳基储钠负极材料，以满足钠离子电池的实用化要求。
4.为了寻找更高性能的嵌钠负极材料，本论文将目光转向合金类负极材料。理论上，Na可与Sn、P、Sb等元素形成Na15Sn4(847mAh g~(-1))，Na3P(2596mAh g~(-1))，和Na3Sb (660mAh g~(-1))化合物，具有超常的理论比容量。但是，这些合金类负极材料在嵌脱钠过程中的体积变化巨大（Sn→Na15Sn4膨胀525%），容易引起材料粉化，丧失电化学活性，导致其无法直接用作钠离子电池负极材料。为了限制体积膨胀对电极的冲击，本论文工作采用纳米化、核壳结构、无定形化和碳包覆等手段进行改性研究。首先，采用原位置换法制备了核壳结构的Sn@Cu纳米复合物，利用表面包覆Cu的限制作用，缓解Na-Sn合金化过程的体积膨胀。该材料的可逆储钠容量为290mAh g~(-1)，20周循环后仍保持在200mAh g~(-1)以上。其次，以红磷和高比表面碳载体为原料，制备了无定形磷/碳复合物，该材料可逆储钠容量高达1764mAh g~(-1)，40周后容量保持率为96.7%，表现出优异的循环稳定性；并且在4000mA g~(-1)的超大电流密度下，放电容量仍有1725mAh g~(-1)，具有非常卓越的脱钠反应动力学。再次，采用高能球磨法制备了Sn4P3/C纳米复合材料，该材料的可逆储钠容量高达816mAh g~(-1)，实现了接近于理论24个Na离子的嵌入反应，100周后容量保持率为89%。最后，将单质Sb纳米化并分散在碳载体中制备了Sb/C纳米复合物，该材料实现了接近3个Na离子的可逆合金化反应，并具有优异的大电流充放电性能。另外，通过优化电解液的组成，加入5%的SEI成膜剂-FEC，使得Sb/C纳米复合电极经循环100周后容量保持率为95%，表现出非常优异的长期循环稳定性。以上工作证明了锡Sn，磷P，磷化锡Sn4P3和锑Sb四种材料都具有非常高的储钠容量、良好的倍率性能以及优异的循环稳定性，并且制备方法简单，原料易得，为发展实用化的高性能钠离子电池负极材料提供了可借鉴的经验和广阔的研究空间。
Sodium ion batteries are now actively pursued as the most attractive alternativeto Li-ion batteries for electric vehicle propulsion and renewable electric power storage,because of their potential advantages of low cost and widespread availability ofsodium resources. To realize Na-ion technology, a critical issue is to find out suitablehost materials that can accommodate sufficient Na ions for reversible electrochemicalinsertion reaction. In this thesis, we were aimed at exploring new anode and cathodematerials and optimize their performance to realize their potentionally high redoxcapacity for reversible Na-storage。The main results and new findings in this work aresummarized as follows：
1. A new family of sodium transition metal cyanides, such as hexacyanoferratesNa_4Fe(CN)_6and Prussian blue NaxMyFe(CN)_6(M=Fe，Co，Ni，Mn) were proposed ascathode materials for sodium ion batteries. Firstly, a Na_4Fe(CN)_6/C nanocompositewere prepared simply by mechanical ball-milling Na_4Fe(CN)_6and conductive carbonpowders. The as-prepared Na_4Fe(CN)_6/C composite displays a full utilization of itsredox capacity of87mAh g~(-1)at a high potential of~3.4V, an excellent cyclingstability with a88%capacity retention over500cycles and a superior high ratecapability with45%capacity delivery at a10C rate. Secondly, four types of Prussianblue NaxMyFe(CN)_6(M=Fe, Co, Ni, Mn) compounds were prepared simply bysolution precipitation method and tested as cathode materials for sodium-ion batteries.Electrochemical tests revealed very different electrochemical behaviors of these foursamples of NaxMyFe(CN)_6(M=Fe, Co, Ni, Mn). When M was Fe, Co and Mn, thespecific capacities of NaxFeyFe(CN)_6, NaxCoyFe(CN)_6and NaxMnyFe(CN)_6can reach113,120and113mAh g~(-1), respectively, indicating that both of the Fe(CN)_64-and M+2ions in the Prussian blue lattices were electrochemically activated. When M was Ni,Ni ions in the Prussian blue lattice was found to be electrochemically inactive and theNaxNiyFe(CN)_6delivered a specific capacity of only64mAh g~(-1)but with quite stablecyclability. These results suggest a possible use of the transition metal cyanides as lowcost and environmentally benign cathode materials for sodium-ion batteries.
2. Two typical conductive polymers: Polyaniline (PAn) and Polytriphenylamine(PTPAn) were chemically synthesized and suggested as promising cathode materials for sodium ion batteries, due to their good conductivity and electrochemical redoxproperty. It was found Na/PAn cell displays a quite high capacity of163mAh g~(-1)at anaverage discharge voltage of3.16V, an excellent cycling stability with118mAh g~(-1)reserved after100cycles and a superior high rate capability with60mAh g~(-1)deliveryat300mA g~(-1)current density, exceeding most of the current inorganic cathodes;Na/PTPAn cells also give a high capacity of93mAh g~(-1)and a quite high averagedischarge voltage of3.56V. Even cycled at a very high rate of500mA g~(-1), thepolymer can still deliver a capacity of72mAh g~(-1), that is78%of initial capacity.Overall, these conductive polymers can realize their potential high redox capacitieswith sufficient cycleability and superior high power capability, suggesting a promisingcathode for high energy density and power density sodium ion batteries.
3. In the search for suitable Na host materials for sodium ion batteries, weinvestigated the electrochemical sodium insertion behavior of several types ofcarbonaceous materials. Hard carbon materials were found to possess the best sodiuminsertion performance, as they contain random stacked carbon layers and significantquantities of nanosized pores, which can serve as active sites for sodium insertion.Base on these results, two kinds of polymers: polyvinyl chloride (PVC andpolyaniline (PAn, were selected as the precursors to make pyrolyzed hard carbon,and their performance were optimized by adjusting proper calcination condition. Itwas found that the PVC electrode can deliver quite a high reversible capacity of~200mAh g~(-1), corresponding to the formation of Na0.54C6, an excellent cycling stabilitywith85%reserved after100cycles and a high rate capability with117mAh g~(-1)delivered at a current density of200mA g~(-1). The PAn-pyrolysed carbon can also givea high capacity of194mAh g~(-1), and97%capacity reserved at200th cycle, and ahigh rate capability with103mAh g~(-1)delivery at500mA g~(-1). In principle, highperformance carbon anodes can be achieved by adjusting the structure of carbonmaterials, including crystal lattice, surface texture, and structural defect, so as to meetthe practical requirements of the sodium ion batteries.
4. Sodium alloying reactions with metals or semi-metals would be an effective wayto provide larger specific capacity and suitable thermodynamic potentials than carbonbased materials. For example, Na can alloy with Sn, P, Sb elements to produceNa15Sn4(847mAh g~(-1), Na3P (2560mAh g~(-1), and Na3Sb (660mAh g~(-1), respectively.In order to suppress enormous volume changes (i.e., a525%volume increase ongoing from Sn to Na15Sn4during sodium alloying reaction, several strategies, such as nanosizing, core-shell structure, amorphisizing and carbon coating, were adopted tooptimize their performances. Firstly, core-shell structured Sn@Cu nanocomposite wassynthesized by a simple substitutional reaction between Sn and Cu2+. The as preparedSn@Cu material can give an enhanced capacity of290mAh g~(-1), with200mAh g~(~(-1))reserved after20cycles. Secondly, an amorphous P/C nanocomposite was simplyprepared by mechanical ball-milling red P and conductive carbon powders. The a-P/Ccomposite displays an quite high capacity of1764mAh g~(-1)，an excellent cyclingstability with96.7%reserved after40cycles, and a superior fast sodiumdeintercalation kinetics with1725mAh g~(-1)achieved at a current density of4000mAg~(-1). Thirdly, a Sn4P3/C nanocomposite was synthesized by ball-milling method, andcan exhibit a reversible capacity of816mAh g~(-1), approaching to its theoretical24Na-storage capacity and retain89%of initial capacity after100cycles. Finally, weprepared a novel Sb/C nanocomposite, simply by mechanical ball-milling commercialSb powder with conductive carbon, which demonstrates a nearly full utilization of itstheoretical3Na storage capacity, a strong rate capability with50%capacity realizedat a very a very high current of2000mA g~(-1). Particularly, in the optimized electrolytewith a SEI film-forming additive, the Sb/C anode demonstrates a long-term cyclingstability with94%capacity retention over100cycles. Overall, these excellentelectrochemical performances of four samples represent the highest level of the Nastorage materials, offering a practical feasibility as a high capacity and cycling-stableanode for room temperature Na-ion batteries.
引文
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