储能用电极材料的制备及其电化学性能的研究
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摘要
能源问题是推动经济发展的源动力也是制约经济发展的瓶颈,以国内主流储能装置如锂电池和电容器来说,关键性电极材料的制造成本价格高昂。实现储能材料加工利用的技术突破、降低储能用电极材料的成本,是储能实现产业化的关键。本文以磷酸铁锂和超级电容器用电极材料的制备作为研究目标,系统地对其合成工艺、材料改性、结构表征、电化学性能以及电极动力学性能等方面进行了研究。利用TG、XRD、SEM、Raman、CV、EIS以及充放电测试等方法研究了电极材料的合成工艺及其电化学性能。通过对产物的生长机理确定了合成过程中所用原料、反应时间、反应溶剂等工艺参数进行了优化,确定了合成电极材料的最佳的工艺条件。
(1)首次采用Fe203为铁源,抗坏血酸作碳源,通过在200℃下水热反应并经煅烧后制备出LiFePO4/C纳米复合材料。抗坏血酸在水热反应体系中不但作为最终反应产物的炭源,而且还起到了限制LiFePO4颗粒生长的作用。抗坏血酸的用量对产物的形貌、结构、碳含量有重要影响,进而影响产物的电化学性能。该方法兼顾固相合成方法中的原料成本低,以及合成过程中的原料分布均匀,可以在较短时间内得到均匀稳定的LiFePO4的产物。当抗坏血酸质量为1g时,制得的LiFePO4/C纳米复合材料的粒径在220-280nm。该材料用作锂离子电池的正极材料时,在0.1C的电流密度下循环500次后其放电容量仍保持159mAh/g,并且具有较好的倍率性能。
(2)采用无模板法在以Fe2(SO4)3为铁源,LiOH为锂源,P2O5为磷源,乙二醇和水作为共溶剂,通过在200℃下水热反应并经煅烧后制备出空心LiFePO4/C纳米复合材料。乙二醇在水热反应体系中不但作为还原剂的作用,而且还起到了作为最终反应产物炭前驱体作用。通过控制不同的反应条件,研究了其反应机理。其中抗坏血酸的用量对产物的形貌、结构、碳含量有重要影响,进而影响产物的电化学性能。
(3)通过采用乙二醇和水作为双溶剂,以Fe(NO3)3为铁源,制备了堆积密度相对较高的笼状LiFePO4/C微球,乙二醇在反应体系中不仅作为还原剂,而且还可以作为一种碳化剂包覆在LiFePO4的表面。通过控制反应时间、反应温度、反应溶剂和反应物,研究了笼状LiFeP04/C的生长机理。在0.1C下,第一次充放电后,材料的放电容量为161mAh/g,300次循环后材料仍然能够保持157mAh/g笼状LiFeP04/C复合材料在0.5、1、5和10C下的可逆容量分别为150、140、130和120mAh/g,相对O.1C下的放电容量,其在各倍率下的放电容量保持率为93、87、80和75%。当充放电电流密度再恢复至0.1C,材料的放电容量可以恢复到160mAh/g。而商品材料随着充放电电流密度从5C提高到10C,商品化材料的放电容量只能保持72%和62%。
(4)通过溶剂热法在较短的反应时间内得到了纯的LiFePO4相,经过600℃和7h的热处理可以得到鸟巢状的具有纳米片层结构的LiFePO4/C复合物。由于溶剂热反应后的产物为纯相,因此后续的热处理时间可以在一定的程度上缩短。反应时间虽然不能改变得到产物的相组成,但改变了产物中的残存的乙二醇的量。在热处理过程中,残留在颗粒表面的乙二醇在氮气的保护下在高温下发生了一个炭化分解作用,乙二醇在本实验过程中既作为一种还原剂,又作为一种碳化剂。与商品化LiFePO4相比,本实验制得的材料的电化学性能更佳。
(5)先合成具有立方结构的金属有机框架,然后采用两种不同的加炭的方法再加以高温热处理方法去除金属有机框架,制备两种不同的多孔碳材料。研究了其制备过程中的各种合成条件对材料的形貌及结构的影响。根据两种材料的结构研究它们在不同的电解液中的电化学性能,发现针对不同的孔结构,片状多孔炭材料更适合在无机电解液中进行充放电,而3D蜂窝状多孔炭材料由于其发达的中孔的结构更适合在有机电解液中发挥其电容性能。
Along with the rapid development of the economy, there are more and more renewable energy deveice are used, such as the lithium ion battery and supercapacitor. However, the high manufacture cost of their electode materials become a big issue in the corresponding industry. Therefore, the development of low cost electrode mateials becomes the foucs of our research. We used TG, XRD, SEM, Raman, CV, EIS, as well as electrochemical testing method to study the optimized synthesis process of the electrode mateials and the detailed information are listed as following:
(1) LiFePO4nanoparticles coated with a carbon layer have been synthesized by a hydrothermal reaction-calcination process, using Fe2O3as an iron source and ascorbic acid as carbon source. The amount of ascorbic acid can have an effect on the structure, phase and carbon amount of the final product. With1g ascorbic acid used in the reaction, the particle sizes of synthesized LiFePO4/C nanocomposites are in a range of220-280nm. When used as cathode materials for the lithium-ion batteries, the as-prepared material shows high capacity and good cycle stability (159mAh/g at0.1C over500cycles), as well as good rate capability.
(2) FeSO4was used as the iron source, LiOH as lithium source, P2O5as the phosphorus source, ethylene glycol and water were used as co-solvent for the preparation of the LiFePO4. After hydrothermal reaction at200℃and calcined at700℃, hollow LiFePO4/C nano-composites were obtained. After investigating the reaction conditions on the final product, the reaction mechanism of the LiFePO4/C compostite was illustrated. Electrochemcial perfoamce demonstreated the material can be a good candidate for the lithium ion battery.
(3) A simple and convenient Ostwald ripening route to the morphology and phase controlled preparation of cage-like LiFePO4/C microspheres is developed. By selecting appropriate experiment conditions for ripening, the phase of the microspheres can be controlled. The possible formation mechanism for the LiFePO4hierarchical microstructures have been presented in detail. As the cathode material for lithium batteries, the as-prepared LiFePO4/C composite exhibits excellent cycle stability (163mAh/g at0.1C up to100cycles) and good rate capacity (119mAh/g,10C).
(4) Self-assembled hierarchical nest-like LiFePO4microstructures from nanoplates have been synthesized by an ethylene glycol-mediated solvothermal route using Li2SO4,Fe(NO3)3·9H2O and P2O5as raw materials. It was found that EG not only played multifold roles in the formation process of such unique LiFePO4hierarchical microstructures, but also acted as carbon source during the heat treatment and forms conductive carbon coating on the surface of the LiFePO4nanoplates. In addition, employing P2O5instead of other phosphorus sources was necessary for the formation of such unique microstructures. The possible formation mechanism for the LiFePO4hierarchical microstructures have been presented in detail. As the cathode material for lithium batteries, the as-prepared LiFePO4architectures exhibit excellent cycle stability (158mAh/g at0.1C up to100cycles) and good rate capacity (120mAh/g,10C). The desirable electrochemical performance can be attributed to such unique microstructure, which could remain structural stability for long-term cycling. Furthermore, the nanoplates as the building blocks can improve the electrochemical reaction kinetics and finally promote the rate performance.
(5) A green and efficient method is present to synthesize porous carbon with different morphologies from metal organic framework (MOF) using glucose, resorcinol and formaldehyde as carbon precursors, respecively. Two methods were adopted to introduce the carbon to the MOF. All the carbon precusros were demonstrarted to penetrate into the external surface and/or voids of cubic-shape MOF, then polymerized and carbonized. Meantime, MOF was decomposed into ZnO, which was further reduced by carbon (or CO) into Zn. And Zn would evaporate during the carbonization process, forming a continuous carbon texture. When the synthesized porous carbons were applied as electrode materials for electric double layer capacitor, we found the materiasls can be performance better in a suitable electrolyte.
(1)首次采用Fe203为铁源,抗坏血酸作碳源,通过在200℃下水热反应并经煅烧后制备出LiFePO4/C纳米复合材料。抗坏血酸在水热反应体系中不但作为最终反应产物的炭源,而且还起到了限制LiFePO4颗粒生长的作用。抗坏血酸的用量对产物的形貌、结构、碳含量有重要影响,进而影响产物的电化学性能。该方法兼顾固相合成方法中的原料成本低,以及合成过程中的原料分布均匀,可以在较短时间内得到均匀稳定的LiFePO4的产物。当抗坏血酸质量为1g时,制得的LiFePO4/C纳米复合材料的粒径在220-280nm。该材料用作锂离子电池的正极材料时,在0.1C的电流密度下循环500次后其放电容量仍保持159mAh/g,并且具有较好的倍率性能。
(2)采用无模板法在以Fe2(SO4)3为铁源,LiOH为锂源,P2O5为磷源,乙二醇和水作为共溶剂,通过在200℃下水热反应并经煅烧后制备出空心LiFePO4/C纳米复合材料。乙二醇在水热反应体系中不但作为还原剂的作用,而且还起到了作为最终反应产物炭前驱体作用。通过控制不同的反应条件,研究了其反应机理。其中抗坏血酸的用量对产物的形貌、结构、碳含量有重要影响,进而影响产物的电化学性能。
(3)通过采用乙二醇和水作为双溶剂,以Fe(NO3)3为铁源,制备了堆积密度相对较高的笼状LiFePO4/C微球,乙二醇在反应体系中不仅作为还原剂,而且还可以作为一种碳化剂包覆在LiFePO4的表面。通过控制反应时间、反应温度、反应溶剂和反应物,研究了笼状LiFeP04/C的生长机理。在0.1C下,第一次充放电后,材料的放电容量为161mAh/g,300次循环后材料仍然能够保持157mAh/g笼状LiFeP04/C复合材料在0.5、1、5和10C下的可逆容量分别为150、140、130和120mAh/g,相对O.1C下的放电容量,其在各倍率下的放电容量保持率为93、87、80和75%。当充放电电流密度再恢复至0.1C,材料的放电容量可以恢复到160mAh/g。而商品材料随着充放电电流密度从5C提高到10C,商品化材料的放电容量只能保持72%和62%。
(4)通过溶剂热法在较短的反应时间内得到了纯的LiFePO4相,经过600℃和7h的热处理可以得到鸟巢状的具有纳米片层结构的LiFePO4/C复合物。由于溶剂热反应后的产物为纯相,因此后续的热处理时间可以在一定的程度上缩短。反应时间虽然不能改变得到产物的相组成,但改变了产物中的残存的乙二醇的量。在热处理过程中,残留在颗粒表面的乙二醇在氮气的保护下在高温下发生了一个炭化分解作用,乙二醇在本实验过程中既作为一种还原剂,又作为一种碳化剂。与商品化LiFePO4相比,本实验制得的材料的电化学性能更佳。
(5)先合成具有立方结构的金属有机框架,然后采用两种不同的加炭的方法再加以高温热处理方法去除金属有机框架,制备两种不同的多孔碳材料。研究了其制备过程中的各种合成条件对材料的形貌及结构的影响。根据两种材料的结构研究它们在不同的电解液中的电化学性能,发现针对不同的孔结构,片状多孔炭材料更适合在无机电解液中进行充放电,而3D蜂窝状多孔炭材料由于其发达的中孔的结构更适合在有机电解液中发挥其电容性能。
Along with the rapid development of the economy, there are more and more renewable energy deveice are used, such as the lithium ion battery and supercapacitor. However, the high manufacture cost of their electode materials become a big issue in the corresponding industry. Therefore, the development of low cost electrode mateials becomes the foucs of our research. We used TG, XRD, SEM, Raman, CV, EIS, as well as electrochemical testing method to study the optimized synthesis process of the electrode mateials and the detailed information are listed as following:
(1) LiFePO4nanoparticles coated with a carbon layer have been synthesized by a hydrothermal reaction-calcination process, using Fe2O3as an iron source and ascorbic acid as carbon source. The amount of ascorbic acid can have an effect on the structure, phase and carbon amount of the final product. With1g ascorbic acid used in the reaction, the particle sizes of synthesized LiFePO4/C nanocomposites are in a range of220-280nm. When used as cathode materials for the lithium-ion batteries, the as-prepared material shows high capacity and good cycle stability (159mAh/g at0.1C over500cycles), as well as good rate capability.
(2) FeSO4was used as the iron source, LiOH as lithium source, P2O5as the phosphorus source, ethylene glycol and water were used as co-solvent for the preparation of the LiFePO4. After hydrothermal reaction at200℃and calcined at700℃, hollow LiFePO4/C nano-composites were obtained. After investigating the reaction conditions on the final product, the reaction mechanism of the LiFePO4/C compostite was illustrated. Electrochemcial perfoamce demonstreated the material can be a good candidate for the lithium ion battery.
(3) A simple and convenient Ostwald ripening route to the morphology and phase controlled preparation of cage-like LiFePO4/C microspheres is developed. By selecting appropriate experiment conditions for ripening, the phase of the microspheres can be controlled. The possible formation mechanism for the LiFePO4hierarchical microstructures have been presented in detail. As the cathode material for lithium batteries, the as-prepared LiFePO4/C composite exhibits excellent cycle stability (163mAh/g at0.1C up to100cycles) and good rate capacity (119mAh/g,10C).
(4) Self-assembled hierarchical nest-like LiFePO4microstructures from nanoplates have been synthesized by an ethylene glycol-mediated solvothermal route using Li2SO4,Fe(NO3)3·9H2O and P2O5as raw materials. It was found that EG not only played multifold roles in the formation process of such unique LiFePO4hierarchical microstructures, but also acted as carbon source during the heat treatment and forms conductive carbon coating on the surface of the LiFePO4nanoplates. In addition, employing P2O5instead of other phosphorus sources was necessary for the formation of such unique microstructures. The possible formation mechanism for the LiFePO4hierarchical microstructures have been presented in detail. As the cathode material for lithium batteries, the as-prepared LiFePO4architectures exhibit excellent cycle stability (158mAh/g at0.1C up to100cycles) and good rate capacity (120mAh/g,10C). The desirable electrochemical performance can be attributed to such unique microstructure, which could remain structural stability for long-term cycling. Furthermore, the nanoplates as the building blocks can improve the electrochemical reaction kinetics and finally promote the rate performance.
(5) A green and efficient method is present to synthesize porous carbon with different morphologies from metal organic framework (MOF) using glucose, resorcinol and formaldehyde as carbon precursors, respecively. Two methods were adopted to introduce the carbon to the MOF. All the carbon precusros were demonstrarted to penetrate into the external surface and/or voids of cubic-shape MOF, then polymerized and carbonized. Meantime, MOF was decomposed into ZnO, which was further reduced by carbon (or CO) into Zn. And Zn would evaporate during the carbonization process, forming a continuous carbon texture. When the synthesized porous carbons were applied as electrode materials for electric double layer capacitor, we found the materiasls can be performance better in a suitable electrolyte.
引文
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