富锂层状材料Li-Ni-Mn-O的合成和电化学性能研究
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摘要
在富锂材料xLi_2MnO_3.(1-x) LiMO（2M=Ni、Mn、Co、Ni_(1/2)Mn_(1/2)、Ni_(1/3)Mn_(1/3)Co_(1/3),0≤x≤1）的合成过程中，前躯体对终产物的电化学性质有很大影响，因此合成过渡金属元素分散均匀的前躯体是很有必要的。富锂材料的首次充电电压高于4.5V（vs Li~+/Li）时，Li~+从锂层和过渡金属层共同脱出，同时锂层两侧的氧也一起脱出，相当于脱出了Li2O，而在放电过程中，脱出的Li~+不能全部嵌入富锂材料的晶格中，导致首次的不可逆容量损失。本论文选取富锂材料中的Li-Ni-Mn-O体系为研究对象，探索了新的合成方法，并通过表面包覆或植入尖晶石相提高了富锂材料首圈的库伦效率，吸收了首次充电时Li_2MnO_3相释放的O2。
采用以尿素为沉淀剂的均匀沉淀法合成了Ni_xMn_(1-x)CO_3（0 采用以尿素为沉淀剂的均匀沉淀法制备了富锂材料Li[Ni_xLi_((1-2x)/3)Mn_((2-x)/3])O_2（其中x=0.1、0.25、0.3和0.4）。分析了不同Ni含量（x值）对前躯体和富锂材料结构和形貌的影响，并研究了材料在2.0-4.8V充放电区间内的电化学性能。当x=0.25（Ni含量）时，材料首次放电比容量为254mAh g~(-1)，从第2圈开始容量保持在263mAh g~(-1)左右，表现出了良好的循环稳定性。
通过降低合成过程中锂盐的用量，在富锂材料Li_(1.17)Ni_(0.25)Mn_(0.583)O_2（或0.4Li_2MnO_3.0.6LiNi_(0.5)Mn_(0.5)O_2）中形成了尖晶石相，使得材料的首次库伦效率接近了100%。当放电至2.8V时，尖晶石相LiM_2O_4（M=Mn或Ni0.5Mn1.5）可以嵌入第二个Li~+，形成Li2M2O4相，致使部分无法嵌入富锂材料的Li~+可以嵌入尖晶石结构中，有效提高了首圈的库伦效率。生成尖晶石相后材料在0.1C时的放电比容量保持在275mAh g~(-1)左右，表现出了良好的循环稳定性。
通过水热还原法在Li_(1.17)Ni_(0.25)Mn_(0.583)O_2颗粒表面包覆不同比例的VO_2。当VO_2包覆量为10at%时，首圈的库伦效率为96.5%，远远高于未包覆的样品。在首次充电过程中，VO_2吸收了Li_2MnO_3相释放的氧原子，被氧化为V2O5；在放电过程中，V2O5可以嵌入Li~+，形成Li_xV_2O_5，致使部分无法嵌入富锂材料的Li~+可以嵌入V2O5中。因此表面包覆VO_2在提高富锂材料首圈库伦效率的同时，吸收了首次充电过程中释放的氧元素。
In the preparation of xLi_2MnO_3.(1-x) LiMO2(M=Ni、Mn、Co、Ni_(1/2)Mn_(1/2)、Ni_(1/3)Mn_(1/3)Co_(1/3),0≤x≤1), precursors play important roles on electrochemicalperformances of the final products. So it is necessary to prepare precursors withconstant contents of the transition metal elements. During the initial charge, lithiumextracts from the Li_2MnO_3component (Li2O·MnO2) with a simultaneous release ofoxygen above4.5V，which results in a net loss of Li2O to yield MnO2. But only one Li~+per MnO2unit embeds into the lattice during first discharge. So these materials undergoa huge irreversible capacity loss in the first cycle. In this dissertation, we selectedLi-Ni-Mn-O system as the objective and explored new method to prepare materials.Meanwhile, with aim to eliminate the huge irreversible capacity loss, the lithiumcontent was decreased to yield integrated layered-spinel structures, and VO_2was coatedon the surface by hydrothermal reduction to absorb the released oxygen.
We successfully developed a urea-based homogeneous precipitation method forpreparation spherical carbonate precursors of Ni_xMn_(1-x)CO_3(0≤x≤1). Thedecomposition of urea releases precipitating anions (mainly OH-and CO_3~(2-)) slowly andhomogeneously into the reaction systems at elevated temperature, and thus results in thehomogeneous precipitation of the precursor particles even without stirring. Theconditions that influence the morphology of carbonate precursors and theelectrochemical performance of the final material were also investigated.
Li[Li(1-2x)/3NixMn(2-x)/3]O2(x=0.1,0.25,0.3and0.4) were synthesized by aurea-based homogeneous precipitation method, and the structures, morphologies andelectrochemical behaviors (between2.0V and4.8V) of samples with different Nicontents (x) were studied. When x=0.25, the sample delivered a discharge capacity of254mAh g~(-1)in the initial cycle, and it also showed a stable discharge capacity of267mAh g~(-1)after20cycles.
We report a method to eliminate the irreversible capacity by decreasing lithiumcontent of0.4Li_2MnO_3.0.6LiNi_(0.5)Mn_(0.5)O_2(Li_(1.17)Ni_(0.25)Mn_(0.583)O_2) to yield integratedlayered-spinel structures. When discharged to about2.8V, the spinel phase of LiM_2O_4(M=Ni, Mn) can transform to rock-salt phase of Li2M2O4(M=Ni, Mn) during which the tetravalent manganese ions are reduced to an oxidation state of3.0. So the spinelphase can act as a host to insert back the extracted lithium ions (from the layered matrix)that could not embed back into the layered lattice to eliminate the irreversible capacityloss and increase the discharge capacity. Their electrochemical properties at roomtemperature showed a high capacity (about275mAh g~(-1)at0.1C) and exhibited goodcycling performance.
VO_2was coated on the surface of Li_(1.17)Ni_(0.25)Mn_(0.583)O_2,by hydrothermal reduction.When10at%VO_2were used, the initial columbic efficiency is96.5%, which is muchhigher than that for the bare material. During the initial charge, the Li~+was extractedfrom the Li_2MnO_3component; at the same time, oxygen ions are immediatelyincorporated into VO_2to form V2O5-like phase. In the subsequent discharge process,V2O5-like phase host allows the reversible Li ions intercalation to form Li_xV_2O_5-likephase. So the VO_2coating layer improves the initial coulombic efficiency as well asabsorbing the released oxygen from Li_2MnO_3.
采用以尿素为沉淀剂的均匀沉淀法合成了Ni_xMn_(1-x)CO_3（0
通过降低合成过程中锂盐的用量，在富锂材料Li_(1.17)Ni_(0.25)Mn_(0.583)O_2（或0.4Li_2MnO_3.0.6LiNi_(0.5)Mn_(0.5)O_2）中形成了尖晶石相，使得材料的首次库伦效率接近了100%。当放电至2.8V时，尖晶石相LiM_2O_4（M=Mn或Ni0.5Mn1.5）可以嵌入第二个Li~+，形成Li2M2O4相，致使部分无法嵌入富锂材料的Li~+可以嵌入尖晶石结构中，有效提高了首圈的库伦效率。生成尖晶石相后材料在0.1C时的放电比容量保持在275mAh g~(-1)左右，表现出了良好的循环稳定性。
通过水热还原法在Li_(1.17)Ni_(0.25)Mn_(0.583)O_2颗粒表面包覆不同比例的VO_2。当VO_2包覆量为10at%时，首圈的库伦效率为96.5%，远远高于未包覆的样品。在首次充电过程中，VO_2吸收了Li_2MnO_3相释放的氧原子，被氧化为V2O5；在放电过程中，V2O5可以嵌入Li~+，形成Li_xV_2O_5，致使部分无法嵌入富锂材料的Li~+可以嵌入V2O5中。因此表面包覆VO_2在提高富锂材料首圈库伦效率的同时，吸收了首次充电过程中释放的氧元素。
In the preparation of xLi_2MnO_3.(1-x) LiMO2(M=Ni、Mn、Co、Ni_(1/2)Mn_(1/2)、Ni_(1/3)Mn_(1/3)Co_(1/3),0≤x≤1), precursors play important roles on electrochemicalperformances of the final products. So it is necessary to prepare precursors withconstant contents of the transition metal elements. During the initial charge, lithiumextracts from the Li_2MnO_3component (Li2O·MnO2) with a simultaneous release ofoxygen above4.5V，which results in a net loss of Li2O to yield MnO2. But only one Li~+per MnO2unit embeds into the lattice during first discharge. So these materials undergoa huge irreversible capacity loss in the first cycle. In this dissertation, we selectedLi-Ni-Mn-O system as the objective and explored new method to prepare materials.Meanwhile, with aim to eliminate the huge irreversible capacity loss, the lithiumcontent was decreased to yield integrated layered-spinel structures, and VO_2was coatedon the surface by hydrothermal reduction to absorb the released oxygen.
We successfully developed a urea-based homogeneous precipitation method forpreparation spherical carbonate precursors of Ni_xMn_(1-x)CO_3(0≤x≤1). Thedecomposition of urea releases precipitating anions (mainly OH-and CO_3~(2-)) slowly andhomogeneously into the reaction systems at elevated temperature, and thus results in thehomogeneous precipitation of the precursor particles even without stirring. Theconditions that influence the morphology of carbonate precursors and theelectrochemical performance of the final material were also investigated.
Li[Li(1-2x)/3NixMn(2-x)/3]O2(x=0.1,0.25,0.3and0.4) were synthesized by aurea-based homogeneous precipitation method, and the structures, morphologies andelectrochemical behaviors (between2.0V and4.8V) of samples with different Nicontents (x) were studied. When x=0.25, the sample delivered a discharge capacity of254mAh g~(-1)in the initial cycle, and it also showed a stable discharge capacity of267mAh g~(-1)after20cycles.
We report a method to eliminate the irreversible capacity by decreasing lithiumcontent of0.4Li_2MnO_3.0.6LiNi_(0.5)Mn_(0.5)O_2(Li_(1.17)Ni_(0.25)Mn_(0.583)O_2) to yield integratedlayered-spinel structures. When discharged to about2.8V, the spinel phase of LiM_2O_4(M=Ni, Mn) can transform to rock-salt phase of Li2M2O4(M=Ni, Mn) during which the tetravalent manganese ions are reduced to an oxidation state of3.0. So the spinelphase can act as a host to insert back the extracted lithium ions (from the layered matrix)that could not embed back into the layered lattice to eliminate the irreversible capacityloss and increase the discharge capacity. Their electrochemical properties at roomtemperature showed a high capacity (about275mAh g~(-1)at0.1C) and exhibited goodcycling performance.
VO_2was coated on the surface of Li_(1.17)Ni_(0.25)Mn_(0.583)O_2,by hydrothermal reduction.When10at%VO_2were used, the initial columbic efficiency is96.5%, which is muchhigher than that for the bare material. During the initial charge, the Li~+was extractedfrom the Li_2MnO_3component; at the same time, oxygen ions are immediatelyincorporated into VO_2to form V2O5-like phase. In the subsequent discharge process,V2O5-like phase host allows the reversible Li ions intercalation to form Li_xV_2O_5-likephase. So the VO_2coating layer improves the initial coulombic efficiency as well asabsorbing the released oxygen from Li_2MnO_3.
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