锂离子电池正极材料电极界面反应机制研究
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摘要
具有高容量、高能量密度和快速充放电能力的锂离子电池是未来绿色二次能源发展的重要方向之一，与上述要求相一致的锂离子电池脱嵌锂容量、循环特性及倍率性能均与电极界面发生的电化学反应相关，因此研究锂离子电池电极界面反应机制对阐明其容量衰减机理、提高脱嵌锂容量及倍率性能等具有重要意义。
为了使研究能够对商业化锂离子电池材料的改进提高提供理论依据，本文首先采用商业化常用的高温固相法合成了LiCoO_2材料，并运用电化学阻抗谱(EIS)对其电极界面反应机制进行研究。研究发现，LiCoO_2电极在脱嵌锂过程中，Nyquist图中始终存在一个代表材料电子电导率变化的半圆。在首次脱锂中期，Nyquist图按频率由高至低包含高频区半圆、中频区半圆、低频区半圆及一条斜线共四部分。通过合适的等效电路对阻抗谱进行拟合并对拟合值进行分析发现这四部分分别代表锂离子通过电极表面的SEI膜、材料电子电导率、电荷传递过程及锂离子在电极内部的扩散，并且通过EIS证实了LiCoO_2电极在脱嵌锂过程中其电导率确实存在一个“绝缘体-金属性”转变，此转变随着脱嵌锂次数的增加逐渐减弱。
同样，运用EIS对固相法合成的LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2材料的电极界面反应机制进行研究。结果表明，LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2电极在脱嵌锂过程中其阻抗谱也由三个半圆及一条斜线四部分组成，通过等效电路拟合各部分数值并分析发现，中频区半圆应归属于电极材料电子电导率的变化，并计算出LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2电极在脱嵌锂过程中电导率变化范围为1.3×10~(-6)~7.3×10~(-4)S·cm~(-1)，即LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2材料在脱嵌锂过程中电导率会发生1~2个数量级的变化，首次发现LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2在脱嵌锂过程中也存在“绝缘体-金属性”转变。
通过固相法合成了近期商业化研究用于替代石墨的热点材料——Li_4Ti_5O_(12)，并运用EIS对其电极界面反应机制进行研究。结果表明，Li_4Ti_5O_(12)电极在首次嵌锂过程中阻抗谱存在三个半圆及一条斜线四部分，经拟合分析得到以上四部分按频率由高至低分别归属于肖特基接触、电极材料的电子电导率、电荷传递过程及锂离子在电极内部的扩散。但在首次脱锂过程1.55V以上，Nyquist图在中低频区域又衍生出一个半圆，即此时阻抗谱由四个半圆及一条斜线共五部分组成。经分析可知，在脱锂阶段衍生出的中低频半圆应归因于Li_4Ti_5O_(12)电极相关的产气副反应，此副反应是由于脱锂过程中伴随锂离子脱出的电子一部分被溶剂组分中的羟基获得，产生了H2。通过对新鲜电极和产气过后的Li_4Ti_5O_(12)电极进行充放电、红外等测试发现，产气副反应在电极表面的残留物会强烈影响Li_4Ti_5O_(12)电极的电化学性能。
富锂电极材料以其高容量、高能量密度等优点在近年来受到广泛关注，但富锂材料首周充放电过程中全新的充放电机制并不明晰。本文通过共沉淀法合成了微纳米级百褶结构的富锂材料Li[Ni1/3Li1/9Mn5/9]O_2及传统层状材料Li[Ni1/2Mn1/2]O_2，运用微分容量、EIS等方法对它们的电极界面反应机制进行了研究。微分容量结果表明，富锂电极材料在首次脱锂阶段存在三个反应峰，分别为4.5V之前Ni~(2+/4+)的氧化，4.5V之后的氧元素脱出过程及质子交换过程，后两个过程在随后的充放电循环中消失，三个过程对材料首次脱锂容量的贡献率分别为65.2%、25.6%、9.2%。EIS结果分析表明，富锂材料在高电压下电极表面的SEI膜会发生部分破裂、分解，但总体上富锂材料表面仍可形成较为稳定的SEI膜；富锂材料的电子电导率会随Ni~(2+/4+)的氧化及材料相变发生相应变化；电荷传递电阻随着循环过程不断增大，这也可能是富锂材料倍率性能差的主要原因。
为了深入认识材料的电极界面反应机制，我们对几种嵌合物电极材料脱嵌锂过程中的动力学参数进行了研究。首先，运用EIS研究了尖晶石LiMn_2O_4正极在1mol/L LiPF_6-EC: DEC: DMC、1mol/L LiPF_6-EC: DEC: EMC和1mol/LLiPF_6-EC: DMC电解液中阻抗谱特征由-20℃随温度升高至20℃发生的变化，通过合适的等效电路拟合分析了LiMn_2O_4电极脱嵌锂过程及相应的锂离子迁移通过SEI膜阻抗、活性材料的电子电阻以及电荷传递电阻随温度的变化情况，并测定了相关的离子跳跃能垒W、热激活化能Ea以及嵌入反应活化能ΔG三个动力学参数。研究发现，电解液组分对锂离子在电极中脱嵌过程影响较大。在上述三种电解液中，LiMn_2O_4电极在1mol/L LiPF_6-EC: DMC电解液中具有最高的离子跳跃能垒、热激活化能和嵌入反应活化能，说明在此电解液中锂离子脱嵌所需克服的能量最高，这也与LiMn_2O_4电极在1mol/L LiPF_6-EC: DMC电解液中充放电性能最差相吻合。
本文通过EIS从动力学角度研究了添加剂VC对LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2电极嵌脱过程的影响。研究结果表明，VC作为添加剂利于在电极表面形成非常稳定的SEI膜；可提高电解液的导离子率，易于锂离子在电解液中的传输；有利于锂离子在电极内部的扩散迁移。另外，本文还研究了LiCoO_2正极在1mol/L LiPF_6-EC:DMC电解液中0~30℃范围内EIS谱特征随温度的变化。测得LiCoO_2正极在上述电解液中的锂离子迁移通过固体电解质相界面膜的离子跳跃能垒为37.7kJ/mol；电子电导率的热激活化能为39.1kJ/mol；嵌入反映活化能平均值为69.0kJ/mol。
该论文有图77幅，表9个，参考文献210篇。
The lithium-ion battery, with the high capacity, high energy density and rapidcharge/discharge, is one of the important directions for green secondary energy in thefuture. The charge/discharge capacity, cycle ability and rate capability are associatedwith the electrochemical reactions at the electrode/electrolyte interfaces, so it isnecessary to understand the electrode/electrolyte interfaces reaction mechanisms forclarifying the capacity fading mechanisms, improving the charge/discharge capacityand the rate capability of the electrode material.
In order to provide the theoretical evidence for improvement of commercialapplications, the LiCoO_2material with commercialization level was synthesized byhigh temperature solid-state reaction. The electrode/electrolyte interfaceelectrochemical reactions in the LiCoO_2cathode were investigated by electrochemicalimpedance spectroscopy (EIS). The Nyquist plots involved a semicircle attributed tothe electronic properties of the material. At intermediate degrees of delithiation, thespectra exhibited three semicircles and a slightly inclined line that appearedsuccessively as the frequency decreases. Based on detail analysis of the change ofkinetic parameters obtained from simulating the experimental EIS data as functions ofpotentials, the high-frequency, the middle-frequency, and the low-frequencysemicircles can be attributed to the migration of the lithium ions through the SEI film,the electronic properties of the material and the charge transfer step, respectively. Theslightly inclined line arises from the solid state diffusion process. At early delithiationthere was a dramatic change in the electrical conductivity of the layered LiCoO_2thatwas caused by an insulator-to-metal transition, which would be weak after the firstdelithiation/lithiation process.
The LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2material with commercialization level was alsosynthesized by high temperature solid-state reaction. The EIS of thedelithiation/lithiation process in LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2cathode were obtained atdifferent potentials during the first cycle. The EIS spectra exhibited three semicirclesand a slightly inclined line that appeared successively along with decrease infrequency. The middle-frequency semicircle should be attributed to the electronicproperties of the material. Along with raising potential from3.5to4.4V, the electricalconductivities of LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2increased by two orders of magnitude, from1.3×10~(-6)to7.3×10~(-4)S·cm~(-1). It was firstly proved that at early delithiation a dramaticchange in the electrical conductivity of the LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2electrode was caused by an insulator-to-metal transition.
The spinel Li_4Ti_5O_(12), suggested as one of the most promising alternatives forgraphite anode, was synthesized by high temperature solid-state reaction. Atintermediate degrees of lithiation process, the EIS spectra exhibited three semicirclesand a slightly inclined reflecting solid state diffusion process. It had been revealedthese three semicircles appearing successively along with decrease in frequencyshould be attributed respectively to the Schottky contact, the electronic properties ofthe material and the charge transfer step. At intermediate degrees of delithiationprocess, above1.55V, an interesting and significant phenomenon was that themiddle-frequency semicircle turn into two joint semicircles, and this phenomenon wasattributed to the gas generation in LTO cells, due to the chemical reduction reaction ofsolvent by Li7Ti5O12with the help of LiPF_6and release H2. The fresh and after gasgeneration electrodes were investigated by galvanostatic cycling and FTIRS, and theresults illustrated that the electrochemical properties were strongly influenced by theresidue after gas generation.
The new generation of Li-rich solid solution materials are received extensiveattention due to their high capacity and high energy density. But their newelectrochemical charge/discharge mechanism is not clear. The cathode materialsLi[Ni1/3Li1/9Mn5/9]O_2and Li[Ni1/2Mn1/2]O_2were synthesized by co-precipitationreaction. The differential capacitance curves showed three major reactions in the firstcharge process of the Li-rich material: the oxidation of Ni~(2+/4+)below4.5V, theextraction of oxygen and the exchange of proton above4.5V, and the capacitycontribution of them were65.2%,25.6%and9.2%, respectively. The oxidation ofNi~(2+/4+)is the only reaction in the following charge processes. The processes of thefirst delithiation/lithiation of Li[Ni_xLi_((1/3-2x/3))Mn_((2/3-x/3))]O_2(x=1/3) cathode wereinvestigated by electrochemical impedance spectroscopy (EIS). The EIS results showthat Li-rich material can form a stable SEI film in the charge/discharge process eventhough the breakdown or dissolution of the resistive SEI film occurs in the highvoltage; the electronic properties change with oxidation reactions and phase transition;the continuing increase of the charge transfer resistance may be the major reason thatthe Li-rich materials have a poor performance in the high current rate.
To further elucidate the delithiation/lithiation mechanisms of the intercalationcompound, EIS was used to measure variations of spectra of LiMn_2O_4electrode withthe temperature in the range-20~20℃in1mol/L LiPF_6-EC: DEC: DMC,1mol/L LiPF_6-EC: DEC: EMC and1mol/L LiPF_6-EC: DMC electrolyte solutions. Theresistance of the SEI film, the electronic resistance as well as the charge transferreaction resistance with variations of temperature were studied and the related kineticparameters the energy barriers for the ion jump relating to migration of Li-ion throughthe SEI film, the thermal active energy of the electronic conductivities and thedelithiation/lithiation reaction active energies were determined. In above threeelectrolyte solutions, LiMn_2O_4electrode had the largest kinetic parameters in1mol/LLiPF_6-EC: DMC electrolyte solution, which was consistent with the worstelectrochemical properties in this electrolyte solution.
Influences of VC in the delithiation/lithiation process of LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2electrode with different experiment condition were investigated by EIS from the pointof kinetic view. It was found that VC was favor of producing an stable SEI film on theelectrode, increasing the ion conductivity and the diffusion process inside of theelectrode. In addition, the activation energy of the ion jump, the thermal activationenergy of the electrical conductivity as well as the activation energy of thedelithiation/lithiation reaction of LiCoO_2electrode were determined to be37.7,39.1and69.0kJ/mol respectively with the temperature in the range0~30℃in1mol/LLiPF_6-EC: DMC electrolyte solution.
为了使研究能够对商业化锂离子电池材料的改进提高提供理论依据，本文首先采用商业化常用的高温固相法合成了LiCoO_2材料，并运用电化学阻抗谱(EIS)对其电极界面反应机制进行研究。研究发现，LiCoO_2电极在脱嵌锂过程中，Nyquist图中始终存在一个代表材料电子电导率变化的半圆。在首次脱锂中期，Nyquist图按频率由高至低包含高频区半圆、中频区半圆、低频区半圆及一条斜线共四部分。通过合适的等效电路对阻抗谱进行拟合并对拟合值进行分析发现这四部分分别代表锂离子通过电极表面的SEI膜、材料电子电导率、电荷传递过程及锂离子在电极内部的扩散，并且通过EIS证实了LiCoO_2电极在脱嵌锂过程中其电导率确实存在一个“绝缘体-金属性”转变，此转变随着脱嵌锂次数的增加逐渐减弱。
同样，运用EIS对固相法合成的LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2材料的电极界面反应机制进行研究。结果表明，LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2电极在脱嵌锂过程中其阻抗谱也由三个半圆及一条斜线四部分组成，通过等效电路拟合各部分数值并分析发现，中频区半圆应归属于电极材料电子电导率的变化，并计算出LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2电极在脱嵌锂过程中电导率变化范围为1.3×10~(-6)~7.3×10~(-4)S·cm~(-1)，即LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2材料在脱嵌锂过程中电导率会发生1~2个数量级的变化，首次发现LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2在脱嵌锂过程中也存在“绝缘体-金属性”转变。
通过固相法合成了近期商业化研究用于替代石墨的热点材料——Li_4Ti_5O_(12)，并运用EIS对其电极界面反应机制进行研究。结果表明，Li_4Ti_5O_(12)电极在首次嵌锂过程中阻抗谱存在三个半圆及一条斜线四部分，经拟合分析得到以上四部分按频率由高至低分别归属于肖特基接触、电极材料的电子电导率、电荷传递过程及锂离子在电极内部的扩散。但在首次脱锂过程1.55V以上，Nyquist图在中低频区域又衍生出一个半圆，即此时阻抗谱由四个半圆及一条斜线共五部分组成。经分析可知，在脱锂阶段衍生出的中低频半圆应归因于Li_4Ti_5O_(12)电极相关的产气副反应，此副反应是由于脱锂过程中伴随锂离子脱出的电子一部分被溶剂组分中的羟基获得，产生了H2。通过对新鲜电极和产气过后的Li_4Ti_5O_(12)电极进行充放电、红外等测试发现，产气副反应在电极表面的残留物会强烈影响Li_4Ti_5O_(12)电极的电化学性能。
富锂电极材料以其高容量、高能量密度等优点在近年来受到广泛关注，但富锂材料首周充放电过程中全新的充放电机制并不明晰。本文通过共沉淀法合成了微纳米级百褶结构的富锂材料Li[Ni1/3Li1/9Mn5/9]O_2及传统层状材料Li[Ni1/2Mn1/2]O_2，运用微分容量、EIS等方法对它们的电极界面反应机制进行了研究。微分容量结果表明，富锂电极材料在首次脱锂阶段存在三个反应峰，分别为4.5V之前Ni~(2+/4+)的氧化，4.5V之后的氧元素脱出过程及质子交换过程，后两个过程在随后的充放电循环中消失，三个过程对材料首次脱锂容量的贡献率分别为65.2%、25.6%、9.2%。EIS结果分析表明，富锂材料在高电压下电极表面的SEI膜会发生部分破裂、分解，但总体上富锂材料表面仍可形成较为稳定的SEI膜；富锂材料的电子电导率会随Ni~(2+/4+)的氧化及材料相变发生相应变化；电荷传递电阻随着循环过程不断增大，这也可能是富锂材料倍率性能差的主要原因。
为了深入认识材料的电极界面反应机制，我们对几种嵌合物电极材料脱嵌锂过程中的动力学参数进行了研究。首先，运用EIS研究了尖晶石LiMn_2O_4正极在1mol/L LiPF_6-EC: DEC: DMC、1mol/L LiPF_6-EC: DEC: EMC和1mol/LLiPF_6-EC: DMC电解液中阻抗谱特征由-20℃随温度升高至20℃发生的变化，通过合适的等效电路拟合分析了LiMn_2O_4电极脱嵌锂过程及相应的锂离子迁移通过SEI膜阻抗、活性材料的电子电阻以及电荷传递电阻随温度的变化情况，并测定了相关的离子跳跃能垒W、热激活化能Ea以及嵌入反应活化能ΔG三个动力学参数。研究发现，电解液组分对锂离子在电极中脱嵌过程影响较大。在上述三种电解液中，LiMn_2O_4电极在1mol/L LiPF_6-EC: DMC电解液中具有最高的离子跳跃能垒、热激活化能和嵌入反应活化能，说明在此电解液中锂离子脱嵌所需克服的能量最高，这也与LiMn_2O_4电极在1mol/L LiPF_6-EC: DMC电解液中充放电性能最差相吻合。
本文通过EIS从动力学角度研究了添加剂VC对LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2电极嵌脱过程的影响。研究结果表明，VC作为添加剂利于在电极表面形成非常稳定的SEI膜；可提高电解液的导离子率，易于锂离子在电解液中的传输；有利于锂离子在电极内部的扩散迁移。另外，本文还研究了LiCoO_2正极在1mol/L LiPF_6-EC:DMC电解液中0~30℃范围内EIS谱特征随温度的变化。测得LiCoO_2正极在上述电解液中的锂离子迁移通过固体电解质相界面膜的离子跳跃能垒为37.7kJ/mol；电子电导率的热激活化能为39.1kJ/mol；嵌入反映活化能平均值为69.0kJ/mol。
该论文有图77幅，表9个，参考文献210篇。
The lithium-ion battery, with the high capacity, high energy density and rapidcharge/discharge, is one of the important directions for green secondary energy in thefuture. The charge/discharge capacity, cycle ability and rate capability are associatedwith the electrochemical reactions at the electrode/electrolyte interfaces, so it isnecessary to understand the electrode/electrolyte interfaces reaction mechanisms forclarifying the capacity fading mechanisms, improving the charge/discharge capacityand the rate capability of the electrode material.
In order to provide the theoretical evidence for improvement of commercialapplications, the LiCoO_2material with commercialization level was synthesized byhigh temperature solid-state reaction. The electrode/electrolyte interfaceelectrochemical reactions in the LiCoO_2cathode were investigated by electrochemicalimpedance spectroscopy (EIS). The Nyquist plots involved a semicircle attributed tothe electronic properties of the material. At intermediate degrees of delithiation, thespectra exhibited three semicircles and a slightly inclined line that appearedsuccessively as the frequency decreases. Based on detail analysis of the change ofkinetic parameters obtained from simulating the experimental EIS data as functions ofpotentials, the high-frequency, the middle-frequency, and the low-frequencysemicircles can be attributed to the migration of the lithium ions through the SEI film,the electronic properties of the material and the charge transfer step, respectively. Theslightly inclined line arises from the solid state diffusion process. At early delithiationthere was a dramatic change in the electrical conductivity of the layered LiCoO_2thatwas caused by an insulator-to-metal transition, which would be weak after the firstdelithiation/lithiation process.
The LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2material with commercialization level was alsosynthesized by high temperature solid-state reaction. The EIS of thedelithiation/lithiation process in LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2cathode were obtained atdifferent potentials during the first cycle. The EIS spectra exhibited three semicirclesand a slightly inclined line that appeared successively along with decrease infrequency. The middle-frequency semicircle should be attributed to the electronicproperties of the material. Along with raising potential from3.5to4.4V, the electricalconductivities of LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2increased by two orders of magnitude, from1.3×10~(-6)to7.3×10~(-4)S·cm~(-1). It was firstly proved that at early delithiation a dramaticchange in the electrical conductivity of the LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2electrode was caused by an insulator-to-metal transition.
The spinel Li_4Ti_5O_(12), suggested as one of the most promising alternatives forgraphite anode, was synthesized by high temperature solid-state reaction. Atintermediate degrees of lithiation process, the EIS spectra exhibited three semicirclesand a slightly inclined reflecting solid state diffusion process. It had been revealedthese three semicircles appearing successively along with decrease in frequencyshould be attributed respectively to the Schottky contact, the electronic properties ofthe material and the charge transfer step. At intermediate degrees of delithiationprocess, above1.55V, an interesting and significant phenomenon was that themiddle-frequency semicircle turn into two joint semicircles, and this phenomenon wasattributed to the gas generation in LTO cells, due to the chemical reduction reaction ofsolvent by Li7Ti5O12with the help of LiPF_6and release H2. The fresh and after gasgeneration electrodes were investigated by galvanostatic cycling and FTIRS, and theresults illustrated that the electrochemical properties were strongly influenced by theresidue after gas generation.
The new generation of Li-rich solid solution materials are received extensiveattention due to their high capacity and high energy density. But their newelectrochemical charge/discharge mechanism is not clear. The cathode materialsLi[Ni1/3Li1/9Mn5/9]O_2and Li[Ni1/2Mn1/2]O_2were synthesized by co-precipitationreaction. The differential capacitance curves showed three major reactions in the firstcharge process of the Li-rich material: the oxidation of Ni~(2+/4+)below4.5V, theextraction of oxygen and the exchange of proton above4.5V, and the capacitycontribution of them were65.2%,25.6%and9.2%, respectively. The oxidation ofNi~(2+/4+)is the only reaction in the following charge processes. The processes of thefirst delithiation/lithiation of Li[Ni_xLi_((1/3-2x/3))Mn_((2/3-x/3))]O_2(x=1/3) cathode wereinvestigated by electrochemical impedance spectroscopy (EIS). The EIS results showthat Li-rich material can form a stable SEI film in the charge/discharge process eventhough the breakdown or dissolution of the resistive SEI film occurs in the highvoltage; the electronic properties change with oxidation reactions and phase transition;the continuing increase of the charge transfer resistance may be the major reason thatthe Li-rich materials have a poor performance in the high current rate.
To further elucidate the delithiation/lithiation mechanisms of the intercalationcompound, EIS was used to measure variations of spectra of LiMn_2O_4electrode withthe temperature in the range-20~20℃in1mol/L LiPF_6-EC: DEC: DMC,1mol/L LiPF_6-EC: DEC: EMC and1mol/L LiPF_6-EC: DMC electrolyte solutions. Theresistance of the SEI film, the electronic resistance as well as the charge transferreaction resistance with variations of temperature were studied and the related kineticparameters the energy barriers for the ion jump relating to migration of Li-ion throughthe SEI film, the thermal active energy of the electronic conductivities and thedelithiation/lithiation reaction active energies were determined. In above threeelectrolyte solutions, LiMn_2O_4electrode had the largest kinetic parameters in1mol/LLiPF_6-EC: DMC electrolyte solution, which was consistent with the worstelectrochemical properties in this electrolyte solution.
Influences of VC in the delithiation/lithiation process of LiNi_(1/)3Co_(1/3)Mn_(1/3)O_2electrode with different experiment condition were investigated by EIS from the pointof kinetic view. It was found that VC was favor of producing an stable SEI film on theelectrode, increasing the ion conductivity and the diffusion process inside of theelectrode. In addition, the activation energy of the ion jump, the thermal activationenergy of the electrical conductivity as well as the activation energy of thedelithiation/lithiation reaction of LiCoO_2electrode were determined to be37.7,39.1and69.0kJ/mol respectively with the temperature in the range0~30℃in1mol/LLiPF_6-EC: DMC electrolyte solution.
引文
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