基于镍钴锰前驱体的锂离子电池正极材料LiNi_（1/3）Co_（1/3）Mn_（1/3）O_2制备与改性研究
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摘要
目前锂离子电池正极材料LiCoO2仍在市场中占据主导地位,但由于其自身缺陷及资源限制,在市场竞争中迫切需要开发一种新的正极材料,而三元复合LiNi1/3Co1/3Mn1/3O2基于自身性能优势及与LiCoO2结构相似性成为最有可能的LiCoO2替代品。作者在详细评述LiNi1/3Co1/3O2正极材料的结构、电化学性能、制备工艺及其发展方向的基础上,以提高电化学性能为目标,研究了基于镍钴锰前驱体采用高温固相反应法制备LiNi1/3Co1/3O2正极材料的新工艺,并对其进行了体相掺杂和表面包覆改性研究。本论文主要叙述如下研究内容。
首先,论述了共沉淀法合成前驱体的理论基础。根据同时平衡原理和质量守恒定律推导Ni(Ⅱ)-Co(Ⅱ)-Mn(Ⅱ)-NH4+-NH3-C2O42--H2O系和Ni(Ⅱ)-Co(Ⅱ)-Mn(Ⅱ)-NH4+-NH3-H2O系的热力学平衡数学模型,绘制出相关金属的log[Me]T-pH图,研究了溶液中总草酸根浓度、总氨浓度和pH值对该平衡体系的影响,探讨了镍、钴、锰草酸盐和氢氧化物的共沉淀机理。在此基础上,根据热力学平衡模拟结果,以镍、钴、锰硫酸盐、草酸和氨水为原料,采用正向加料方式,液相共沉淀法合成了组分精确、形貌单一、粒径分布均匀的Ni1/3Co1/3Mn1/3C2 O4·2H2O前驱体。采用控制结晶法,利用NH3与Ni2+、Co2+和Mn2+离子配合作用,合成了球形Ni1/3Co1/3Mn1/3(OH)2前驱体；研究还发现,通过添加抗氧化剂A,能解决氢氧化物共沉淀反应过程中Mn2+氧化致使产物化学组分偏析的难题,有效抑制Mn2+离子的氧化,实现镍钴锰复合共沉淀。
其次,以优化条件下合成的镍钴锰草酸盐前驱体和LiOH·H2O为原料,采用高温固相反应制备出层状LiNi1/3Co1/3Mn1/3O2正极材料,详细考察了前驱体预处理、合成时间、烧结温度、锂金属摩尔比、空气流量等条件对正极材料性能的影响,获得了最佳工艺条件。对制备的LiNi1/3Co1/3Mn1/3O2正极材料进行电化学性能检测,在0.1C、2.75V-4.3V下充放电,材料的首次放电比容量达168.8mAh／g,20次循环后容量保持率为95.4%,在2.75V-4.4V、4.5V、4.6V、4.8V下首次放电比容量分别为176.1mAh／g、189.1mAh/g、200.8 mAh/g和223.6mAh／g；在1C和2C、2.75V-4.3V下的首次放电比容量则分别为124.8mAh/g和104.6mAh/g。而以Ni1/3Co1/3 Mn1/3(OH)2前驱体与锂盐为原料,采用相同方法合成的正极材料,在0.1C、2.75V-4.3V下的首次放电比容量为163.4 mAh／g。
再次,采用草酸盐共沉淀法制备了Ti4+、Mg2+离子掺杂的LiNi1/3 Co1/3-XMn1/3TixO2、LiNi1/3Co1/3-xMn1/3MgxO2正极材料,考察了Ti4+、Mg2+离子体相掺杂对LiNi1/3Co1/3Mn1/3O2正极材料电化学性能的影响。经XRD和SEM检测表明,Ti4+、Mg2+离子掺杂量x=0.01-0.1时未改变正极材料结构和形貌,而电化学测试结果表明当掺杂量x=0.025时提高了正极材料的高倍率充放电性能,尤以掺杂钛为佳。在2.75V-4.3V电压区间、1C充放电时,LiNi1/3Co1/3-0.025Mn1/3Ti0.025O2和Li Ni1/3 Co1/3-0.025Mn1/3Mg0.025O2首次放电容量分别为140.3mAh/g和129.7 mAh／g,100次循环后的容量保持率分别为92.5%和91.1%；2C充放电时,两者的首次放电容量则分别为126.9mAh/g和114.8 mAh／g,经100次循环后容量保持率分别为90.8%和88.3%。利用恒电位阶跃法研究了Li-在正极材料中的扩散系数发现,嵌锂电位为3.7V时,LiNi1/3Co1/3 Mn1/3O2中锂离子扩散系数为2.63×10-11cm2／s,LiNi1/3Co1/3-xMn1/3TixO2中为3.27×10-10cm2／s,LiNi1/3Co1/3-xMn1/3MgxO2中为7.63×10-11cm2/s。结果表明Ti4+、Mg2+离子掺杂可提高锂离子在材料中的扩散系数。
最后,首次研究低热固相化学反应法对LiNi1/3Co1/3Mn1/3O2表面SnO2包覆。该法是一种工艺简单、行之有效的正极材料表面包覆改性方法。研究确定SnO2包覆量以3wt%为最佳,经TEM、XPS检测分析证实,包覆后在正极材料表面形成了约20nm厚的均匀包覆层。在0.1C、2.75V-4.6V下,3wt%SnO2包覆LiNi1/3Co1/3Mn1/3O2正极材料的首次放电比容量为188.6mAh/g,30次循环后容量保持率为88.17%。采用交流阻抗法对LiNi1/3Co1/3Mn1/3O2正极材料界面反应特性进行研究发现,充放电循环过程中电池容量衰减与电荷传输电阻(Rct)增大有关, SnO2包覆后Rct显著降低,由此提出了LiNi1/3Co1/3Mn1/3O2正极材料包覆改性的机理模型。
At present LiCoO2 still dominates the lithium-ion battery cathode material market, but due to its own shortcomings and resource constraints, there is an urgent need to develop a new cathode material in the market competition. Ternary complex LiNi1/3Co1/3Mn1/3O2is the best alternative with LiCoO2 cathode material due to its excellent electrochemical properties and similar structure to that of LiCoO2. The structure, electrochemical performance, preparation technology and developing trends of LiNi1/3Co1/3Mn1/3O2 cathode material were described by author. LiNi1/3Co1/3Mn1/3O2 based on Ni-Co-Mn precursor was prepared by solid-state reaction at high temperature, followed with ion-doping and surface coating to improve its electrochemical performance. The contents of this study were described in this dissertation.
First of all, theoretical basis for co-precipitation synthesis of Ni-Co-Mn precursor was discussed. According to the principle of simultaneity balance and mass conservation, the mathematic model of thermodynamic equilibrium for the system of Ni(Ⅱ)-Co(Ⅱ)-Mn(Ⅱ)-NH4+-NH3-C2O42--H2O and Ni(Ⅱ)-Co(Ⅱ)-Mn(Ⅱ)-NH4+-NH3-H2O has been built, respectively. The log[Me]T-pH diagram of the related metal ion was drawn, and effect of total oxalate concentration, total ammonia concentration and pH value on the co-precipitation of Ni, Co, Mn oxalate and hydroxide was investigated, respectively. Using oxalic acid and stoichiometric mixed solution of NiSO4, CoSO4 and MnSO4 as starting materials, triple oxalate precursor of nickel, cobalt, and manganese with homo-morphology and uniform particle size distribution was synthesized with liquid-phase co-precipitation method. The obtained oxalate precursor was characterized by chemical element analysis, XRD and DSC-TGA, respectively, and the molecular formula of precursor was determined as Ni1/3Co1/3Mn1/3C2O4·2H2O. In order to prevent oxidation of Mn2+ ion, anti-oxidative agent was added during co-precipitation. As a result, Ni2+, Co2+, and Mn2+ were co-precipitated with stoichiometric ratio.
And Secondly, the mixtures of oxalate precursor and LiOH·H2O was used as raw materials to prepare layered LiNi1/3Co1/3Mn1/3O2 cathode material by solid-state reaction at high temperature. Effect of precursor pre-treatment, reaction time, sintering temperature, the molar ratio of lithium to metal and air flow on the properties of obtained cathode material was investigated in detail. The results of electrochemical performance tests show that the first discharge specific capacity of LiNi1/3Co1/3Mn1/3O2 obtained under optimum conditions can reach 168.8mAh/g at 0.1C in voltages of 2.75V-4.3V, and the capacity maintenance rate is 95.4% after 20 charge-discharge circles. In voltages of 2.75V-4.4V,4.5V,4.6V or 4.8V, the first discharge specific capacity of obtained cathode material is 176.1mAh/g,189.1mAh/g,200.8mAh/g or 223.6mAh/g, respectively. At 1C and 2C, the first discharge specific capacity is 124.8mAh/g and 104.6mAh/g, respectively in voltages of 2.75V-4.3V. Using Ni1/3Co1/3Mn1/3(OH)2 precursor and LiOH·H2O as starting material, LiNi1/3Co1/3Mn1/3O2 was prepared with solid-state reaction method, and in voltages of 2.75V-4.3V its first discharge specific capacity is 163.4mAh/g at 0.1C.
Once again, LiNi1/3Co1/3-xMn1/3TixO2 and LiNi1/3Co1/3-xMn1/3MgxO2 were synthesized with oxalate co-precipitation method. Effect of Ti4+ Mg2+ ion-doping on the electrochemical properties of LiNi1/3Co1/3Mn1/3O2 cathode material was investigated. The results show that x=0.01-1amount of Ti4+ or Mg2+ ion-doping has little influence on the crystal structure and morphology of obtained sample. The charge-discharge performance at high rate is improved when the doping amount x=0.025, especially in titanium-doped battery. At 1C, the first discharge capacity of LiNi1/3Co1/3-0.025Mn1/3Ti0.025O2 and LiNi1/3Co1/3-0.025Mn1/3Mg0.025O2 is 140.3mAh/g and 129.7mAh/g, respectively, and the capacity maintenance rate is 92.5% and 91.1% after 100 charge-discharge cycles. At 2C, the first discharge capacity is decreased to 126.9mAh/g and 114.8mAh/g, respectively, and the capacity maintenance rate is 90.8% and 88.3% after 100 charge-discharge cycles. The influence of Ti4+ or Mg2+ ion-doping on the diffusion coefficient of Li+ was studied with constant potential step method. It was found that the diffusion coefficient of lithium-ion was increased after Ti4+, Mg2+ ion-doping. When the lithium potential was 3.7V, lithium-ion diffusion coefficient of un-doped sample was 2.63x10-11cm2/s. After Ti4+ and Mg2+ ion-doping, the lithium-ion diffusion coefficient was enhanced to 3.27×10-10 cm2/s and 7.63×10-11 cm2/s, respectively.
Finally, the LiNi1/3Co1/3Mn1/3O2 cathode material coated with SnO2 film was firstly prepared with low-heating solid-state reaction method. It is shown this method is a kind of simple and effective method for cathode material coated modification. The results show that a uniform 20nm thick coating layer formed on the surface of cathode material was confirmed by TEM and XPS when SnO2-coated amount of 3wt%. At 0.1C, the first discharge capacity is 188.6mAh/g in voltages of 2.75V-4.6V, and the capacity maintenance rate is 88.17%after 30 charge-discharge cycles. AC impedance method was adopted to study the interfacial reaction characteristics of LiNi1/3Co1/3Mn1/3O2 cathode material. The results show that the battery capacity decays during charge-discharge cycle due to charge-transfer resistance (Rct) increasing, and Rct significantly decreases after SnO2-coating. Therefore, the mechanism model of LiNi1/3Co1/3 Mn1/3O2 cathode material coating modification was proposed.
首先,论述了共沉淀法合成前驱体的理论基础。根据同时平衡原理和质量守恒定律推导Ni(Ⅱ)-Co(Ⅱ)-Mn(Ⅱ)-NH4+-NH3-C2O42--H2O系和Ni(Ⅱ)-Co(Ⅱ)-Mn(Ⅱ)-NH4+-NH3-H2O系的热力学平衡数学模型,绘制出相关金属的log[Me]T-pH图,研究了溶液中总草酸根浓度、总氨浓度和pH值对该平衡体系的影响,探讨了镍、钴、锰草酸盐和氢氧化物的共沉淀机理。在此基础上,根据热力学平衡模拟结果,以镍、钴、锰硫酸盐、草酸和氨水为原料,采用正向加料方式,液相共沉淀法合成了组分精确、形貌单一、粒径分布均匀的Ni1/3Co1/3Mn1/3C2 O4·2H2O前驱体。采用控制结晶法,利用NH3与Ni2+、Co2+和Mn2+离子配合作用,合成了球形Ni1/3Co1/3Mn1/3(OH)2前驱体；研究还发现,通过添加抗氧化剂A,能解决氢氧化物共沉淀反应过程中Mn2+氧化致使产物化学组分偏析的难题,有效抑制Mn2+离子的氧化,实现镍钴锰复合共沉淀。
其次,以优化条件下合成的镍钴锰草酸盐前驱体和LiOH·H2O为原料,采用高温固相反应制备出层状LiNi1/3Co1/3Mn1/3O2正极材料,详细考察了前驱体预处理、合成时间、烧结温度、锂金属摩尔比、空气流量等条件对正极材料性能的影响,获得了最佳工艺条件。对制备的LiNi1/3Co1/3Mn1/3O2正极材料进行电化学性能检测,在0.1C、2.75V-4.3V下充放电,材料的首次放电比容量达168.8mAh／g,20次循环后容量保持率为95.4%,在2.75V-4.4V、4.5V、4.6V、4.8V下首次放电比容量分别为176.1mAh／g、189.1mAh/g、200.8 mAh/g和223.6mAh／g；在1C和2C、2.75V-4.3V下的首次放电比容量则分别为124.8mAh/g和104.6mAh/g。而以Ni1/3Co1/3 Mn1/3(OH)2前驱体与锂盐为原料,采用相同方法合成的正极材料,在0.1C、2.75V-4.3V下的首次放电比容量为163.4 mAh／g。
再次,采用草酸盐共沉淀法制备了Ti4+、Mg2+离子掺杂的LiNi1/3 Co1/3-XMn1/3TixO2、LiNi1/3Co1/3-xMn1/3MgxO2正极材料,考察了Ti4+、Mg2+离子体相掺杂对LiNi1/3Co1/3Mn1/3O2正极材料电化学性能的影响。经XRD和SEM检测表明,Ti4+、Mg2+离子掺杂量x=0.01-0.1时未改变正极材料结构和形貌,而电化学测试结果表明当掺杂量x=0.025时提高了正极材料的高倍率充放电性能,尤以掺杂钛为佳。在2.75V-4.3V电压区间、1C充放电时,LiNi1/3Co1/3-0.025Mn1/3Ti0.025O2和Li Ni1/3 Co1/3-0.025Mn1/3Mg0.025O2首次放电容量分别为140.3mAh/g和129.7 mAh／g,100次循环后的容量保持率分别为92.5%和91.1%；2C充放电时,两者的首次放电容量则分别为126.9mAh/g和114.8 mAh／g,经100次循环后容量保持率分别为90.8%和88.3%。利用恒电位阶跃法研究了Li-在正极材料中的扩散系数发现,嵌锂电位为3.7V时,LiNi1/3Co1/3 Mn1/3O2中锂离子扩散系数为2.63×10-11cm2／s,LiNi1/3Co1/3-xMn1/3TixO2中为3.27×10-10cm2／s,LiNi1/3Co1/3-xMn1/3MgxO2中为7.63×10-11cm2/s。结果表明Ti4+、Mg2+离子掺杂可提高锂离子在材料中的扩散系数。
最后,首次研究低热固相化学反应法对LiNi1/3Co1/3Mn1/3O2表面SnO2包覆。该法是一种工艺简单、行之有效的正极材料表面包覆改性方法。研究确定SnO2包覆量以3wt%为最佳,经TEM、XPS检测分析证实,包覆后在正极材料表面形成了约20nm厚的均匀包覆层。在0.1C、2.75V-4.6V下,3wt%SnO2包覆LiNi1/3Co1/3Mn1/3O2正极材料的首次放电比容量为188.6mAh/g,30次循环后容量保持率为88.17%。采用交流阻抗法对LiNi1/3Co1/3Mn1/3O2正极材料界面反应特性进行研究发现,充放电循环过程中电池容量衰减与电荷传输电阻(Rct)增大有关, SnO2包覆后Rct显著降低,由此提出了LiNi1/3Co1/3Mn1/3O2正极材料包覆改性的机理模型。
At present LiCoO2 still dominates the lithium-ion battery cathode material market, but due to its own shortcomings and resource constraints, there is an urgent need to develop a new cathode material in the market competition. Ternary complex LiNi1/3Co1/3Mn1/3O2is the best alternative with LiCoO2 cathode material due to its excellent electrochemical properties and similar structure to that of LiCoO2. The structure, electrochemical performance, preparation technology and developing trends of LiNi1/3Co1/3Mn1/3O2 cathode material were described by author. LiNi1/3Co1/3Mn1/3O2 based on Ni-Co-Mn precursor was prepared by solid-state reaction at high temperature, followed with ion-doping and surface coating to improve its electrochemical performance. The contents of this study were described in this dissertation.
First of all, theoretical basis for co-precipitation synthesis of Ni-Co-Mn precursor was discussed. According to the principle of simultaneity balance and mass conservation, the mathematic model of thermodynamic equilibrium for the system of Ni(Ⅱ)-Co(Ⅱ)-Mn(Ⅱ)-NH4+-NH3-C2O42--H2O and Ni(Ⅱ)-Co(Ⅱ)-Mn(Ⅱ)-NH4+-NH3-H2O has been built, respectively. The log[Me]T-pH diagram of the related metal ion was drawn, and effect of total oxalate concentration, total ammonia concentration and pH value on the co-precipitation of Ni, Co, Mn oxalate and hydroxide was investigated, respectively. Using oxalic acid and stoichiometric mixed solution of NiSO4, CoSO4 and MnSO4 as starting materials, triple oxalate precursor of nickel, cobalt, and manganese with homo-morphology and uniform particle size distribution was synthesized with liquid-phase co-precipitation method. The obtained oxalate precursor was characterized by chemical element analysis, XRD and DSC-TGA, respectively, and the molecular formula of precursor was determined as Ni1/3Co1/3Mn1/3C2O4·2H2O. In order to prevent oxidation of Mn2+ ion, anti-oxidative agent was added during co-precipitation. As a result, Ni2+, Co2+, and Mn2+ were co-precipitated with stoichiometric ratio.
And Secondly, the mixtures of oxalate precursor and LiOH·H2O was used as raw materials to prepare layered LiNi1/3Co1/3Mn1/3O2 cathode material by solid-state reaction at high temperature. Effect of precursor pre-treatment, reaction time, sintering temperature, the molar ratio of lithium to metal and air flow on the properties of obtained cathode material was investigated in detail. The results of electrochemical performance tests show that the first discharge specific capacity of LiNi1/3Co1/3Mn1/3O2 obtained under optimum conditions can reach 168.8mAh/g at 0.1C in voltages of 2.75V-4.3V, and the capacity maintenance rate is 95.4% after 20 charge-discharge circles. In voltages of 2.75V-4.4V,4.5V,4.6V or 4.8V, the first discharge specific capacity of obtained cathode material is 176.1mAh/g,189.1mAh/g,200.8mAh/g or 223.6mAh/g, respectively. At 1C and 2C, the first discharge specific capacity is 124.8mAh/g and 104.6mAh/g, respectively in voltages of 2.75V-4.3V. Using Ni1/3Co1/3Mn1/3(OH)2 precursor and LiOH·H2O as starting material, LiNi1/3Co1/3Mn1/3O2 was prepared with solid-state reaction method, and in voltages of 2.75V-4.3V its first discharge specific capacity is 163.4mAh/g at 0.1C.
Once again, LiNi1/3Co1/3-xMn1/3TixO2 and LiNi1/3Co1/3-xMn1/3MgxO2 were synthesized with oxalate co-precipitation method. Effect of Ti4+ Mg2+ ion-doping on the electrochemical properties of LiNi1/3Co1/3Mn1/3O2 cathode material was investigated. The results show that x=0.01-1amount of Ti4+ or Mg2+ ion-doping has little influence on the crystal structure and morphology of obtained sample. The charge-discharge performance at high rate is improved when the doping amount x=0.025, especially in titanium-doped battery. At 1C, the first discharge capacity of LiNi1/3Co1/3-0.025Mn1/3Ti0.025O2 and LiNi1/3Co1/3-0.025Mn1/3Mg0.025O2 is 140.3mAh/g and 129.7mAh/g, respectively, and the capacity maintenance rate is 92.5% and 91.1% after 100 charge-discharge cycles. At 2C, the first discharge capacity is decreased to 126.9mAh/g and 114.8mAh/g, respectively, and the capacity maintenance rate is 90.8% and 88.3% after 100 charge-discharge cycles. The influence of Ti4+ or Mg2+ ion-doping on the diffusion coefficient of Li+ was studied with constant potential step method. It was found that the diffusion coefficient of lithium-ion was increased after Ti4+, Mg2+ ion-doping. When the lithium potential was 3.7V, lithium-ion diffusion coefficient of un-doped sample was 2.63x10-11cm2/s. After Ti4+ and Mg2+ ion-doping, the lithium-ion diffusion coefficient was enhanced to 3.27×10-10 cm2/s and 7.63×10-11 cm2/s, respectively.
Finally, the LiNi1/3Co1/3Mn1/3O2 cathode material coated with SnO2 film was firstly prepared with low-heating solid-state reaction method. It is shown this method is a kind of simple and effective method for cathode material coated modification. The results show that a uniform 20nm thick coating layer formed on the surface of cathode material was confirmed by TEM and XPS when SnO2-coated amount of 3wt%. At 0.1C, the first discharge capacity is 188.6mAh/g in voltages of 2.75V-4.6V, and the capacity maintenance rate is 88.17%after 30 charge-discharge cycles. AC impedance method was adopted to study the interfacial reaction characteristics of LiNi1/3Co1/3Mn1/3O2 cathode material. The results show that the battery capacity decays during charge-discharge cycle due to charge-transfer resistance (Rct) increasing, and Rct significantly decreases after SnO2-coating. Therefore, the mechanism model of LiNi1/3Co1/3 Mn1/3O2 cathode material coating modification was proposed.
引文
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