氢氧化镍材料的合成、修饰及其电化学性能研究
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摘要
化石能源危机和环境危机所产生的双重压力促使电动车(包括纯电动车和混合动力电动车)得到极为广泛的重视。在电动车中,高功率蓄电池占有非常重要的地位。具有“高比能绿色电池”之称的金属氢化物一镍电池(MH/Ni电池)在作为混合动力电动汽车的车用电池方面具有明显的优势,也是最早作为混合动力电动车用电池进入商业化阶段的电池系统。由于MH/Ni电池在设计上采用的是正极容量限制方式,因此,其正极材料氢氧化镍综合性能的提高对电池整体性能的提升至关重要。本论文以提高氢氧化镍材料的大电流充放电性能及其质量比容量为目的,采用不同的制备方法分别合成了片状纳米氢氧化镍、纳米氢氧化镍／碳复合材料、α相纳米片状Ni-Co氢氧化物以及表面覆钻的微米球形氢氧化镍,并对它们各自的电化学性能进行了深入细致的研究。
1.纳米Ni(OH)2具有特殊的结构特性,被认为具有比微米级球形氢氧化镍更好的电化学性能。但目前系统研究纳米Ni(OH)2的制备及其形貌、结构等因素与其电化学性能关系的还很少。为了对纳米Ni(OH)2的这种关系有进一步的了解,本文采用水热法控制合成了系列均匀片状纳米Ni(OH)2,对合成的系列纳米Ni(OH)2的循环伏安、倍率放电等性能作了详尽的研究,并与商业化球形氢氧化镍进行了对比,结合XRD、SEM和HRTEM等结构分析方法得出以下的结论：①纳米Ni(OH)2有更高的电化学反应活性和快速活化能力,但并非所有的纳米级氢氧化镍均较微米级的球形氢氧化镍在电化学性能方面表现出优势。②降低纳米Ni(OH)2在垂直于[100]晶轴方向的结晶性,可以提高其电化学活性和比容量。③在理解纳米Ni(OH)2的粒径对其电化学性能的影响方面,不能单纯地追求单个颗粒整体的大小对电化学性能的影响,还应该考虑到颗粒中存在的不完全的结晶和优先生长可能对其电化学性能带来的影响。
2.纳米Ni(OH)2具有电化学活性高、充电效率高及放电平台高等优点,但存在易于团聚、在使用过程中难与导电剂均匀混合等问题导致其纳米特性难以得到很好的体现。为了克服上述问题,我们利用超声波处理方法,在液相中把现场生成的纳米Ni(OH)2微粒直接均匀地分散负载于纳米级的碳基微粒材料表面,使两者均匀复合成一种新型材料。不仅解决了现有技术中存在的纳米Ni(OH)2活性材料的分散问题,确保了Ni(OH)2纳米特性,同时也使其导电性得到提高。电化学测试证实此种复合材料具有优异的大电流充放电特性,活性材料的利用率也得到明显提高。
3. a-Ni(OH)2中的Ni元素在电化学反应中的理论交换电子数约为1.7,远大于β-Ni(OH)2的1个交换电子,故合成稳定的a-Ni(OH)2是提高MH/Ni电池正极比容量的重要途径。我们首次采用部分阳离子交换法制备出一系列α相Ni-Co氢氧化物。循环伏安研究表明所合成的a相Ni-Co氢氧化物比共沉淀法合成的β相Ni-Co氢氧化物具有更低的电阻和更好的电化学可逆性。充放电测试表明所合成的α相Ni-Co氢氧化物的比容量远高于β-Ni(OH)2的理论比容量,并且在500周循环后仍保持有很好的容量特性和充放电性能。通过调节Ni-Co氢氧化物的组成,还可以调控其电化学性能。此外,阳离子交换反应还可以可逆进行。阳离子交换方法是一个构筑不同组成的双金属氢氧化物的简便的新方法,并且以此方法制备的材料呈现出不同于传统方法所得产物的优异电化学性能。
4.在微米级球形Ni(OH)2表面进行钴元素的包覆,可在其表面形成导电网络,有效提高其导电性。通常采用的覆钴方法主要是化学沉积法和电沉积法。本文采用了一种新方法—阳离子交换方法,成功地合成了系列具有核-壳结构的Ni(OH)2@CoOOH样品。这种原位的阳离子交换合成过程使得产物Ni(OH)2@CoOOH完好地保持了初始球形Ni(OH)2的结构和形貌,并且表层CoOOH与内部Ni(OH)2核是通过过渡相a-Ni(OH)2贯通起来的。这种结构不仅增强了CoOOH与Ni(OH)2之间接合的牢固度,使得此种材料的循环稳定性得到了明显的提高,而且还使其作为MH/Ni电池的正极材料时的比容量得到提高,超过了β-Ni(OH)2的理论比容量。覆钴材料的导电性和活化特性也得到了极大的提高,可用0.5-2C的倍率在几周内完全活化。此外,还探讨了Ni(OH)2@CoOOH的制备方法所涉及的反应机理。
鉴于所开发的核-壳结构Ni(OH)2@CoOOH的制备方法简单,所得到的材料具有导电性高、易于活化、比容量高、循环性能好等优点,我们对此种材料的单批合成量成功地进行了放大,并采用所制备的大批量Ni(OH)2@CoOOH材料组装了方形动力电池(6Ah)。电化学测试结果表明,当电池的放电倍率提高到30C时仍保持有74.19%的放电效率,而用以制备核-壳结构Ni(OH)2@CoOOH材料的原料球形Ni(OH)2加入CoO作为导电添加剂所制作的对比电池在30C放电时的放电效率降到了1.86%。
The increasing concerns over air pollution and depletion of natural energy resources reserves have spurred renewed interest in electric vehicles (EV), where high power batteries are playing important role. MH/Ni batteries named as high specific energy green power sources are considered to be one of the most promising choices for EV and hybrid electric vehicle (HEV) applications. Furthermore, MH/Ni batteries are the first one which was used as power batteries in commercial HEVs. These batteries are usually designed with capacity limited by positive electrode for reasons of proper gas recombination reactions and battery safety. It follows that increasing the comprehensive performance of the nickel hydroxide electrode is essential for raising the performance of MH/Ni batteries. It's the purpose of this thesis that increasing the high rate dischargeability and energy density of nickel hydroxide electrode by the synthesis of plate like nano-scale nickel hydroxide, nickel hydroxide/carbon composites and nanosheets ofα-Ni/Co hydroxides through various methods and modifying macro-spherical nickel hydroxide with cobalt oxyhydroxide via a new method.
1. Owing to the special structural characteristics, nickel hydroxide with nanostructural multiphase was considered to have better electrochemical properties than that of spherical nickel hydroxide. However, as far as we know, few researches touch on the synthesis of a series of nano-scale nickel hydroxides and the systematical investigation of the structure/function relationships in nano-scale nickel hydroxides. For the purpose of understanding the structure/function relationships in nano-scale nickel hydroxides, a series of large-scale nickel hydroxide nanoplates with differences in size and crystallinity were synthesized in this work. Through cyclic voltammetry and rate-discharge electrochemistry tests combining the XRD、SEM and HR-TEM analysis of the structure of nano-scale nickel hydroxides, the conclusions was obtained as followings:①Nickel hydroxides with nanostructure have higher electrochemical reaction activity and are more easily activated than macro-spherical nickel hydroxide. However, not all nano-scale nickel hydroxides behave better electrochemical properties than macro-spherical Ni(OH)2.②Electrochemical activity and specific capacity of nano-scale nickel hydroxides could be improved by reducing the crystalline in the direction perpendicular to the axis of [100].③Not only the size of single nanometer nickel hydroxide but also the defects in crystals and un-perfect crystallization of single particles have influence on its electrochemical properties.
2. Numerous researches have indicated that nanometer nickel hydroxides have better electrochemical reaction activity, higher charging efficiency and higher discharge potential than macro-spherical Ni(OH)2. However, the nature that nanometer Ni(OH)2 is prone to aggregate, which causes nanometer Ni(OH)2 to be difficult to mix with conductive materials effectively, blocks the behaving of the characteristics of nanometer Ni(OH)2. To overcome this problem, a new kind of composite was synthesized by loading the nanometer Ni(OH)2 uniformly onto the surface of nano-scale spherical carbon particles via sonochemical technique. In this way, not only the dispersion problem of nanometer Ni(OH)2 is resolved which guarantees the behaving of the characteristics of nanometer Ni(OH)2, but also the conductivity of nanometer Ni(OH)2 is improved intensively. In addition, the electrochemical tests show that this kind of material behaves excellent high rate dischargeability, and the utilization of the active material is raised.
3. The number of theoretical exchangeable electrons per nickel atom inα-Ni(OH)2 reaches about 1.7 which is far larger than that ofβ-Ni(OH)2 (1). Therefore, synthesing stabilizedα-Ni(OH)2 is an effective way to increase the specific capacity of Ni(OH)2 cathode. Here, as far as we known, the partial cation exchange method was firstly and successfully adopted for the synthesis of a series of 2D Co-Ni bimetallic hydroxides. The cyclic voltammetry tests show that the synthesizedαphase Co-Ni bimetallic hydroxides have lower resistance and better reversibility than that ofβphase Co-Ni bimetallic hydroxides prepared by co-deposition method. In addition, the charge-discharge tests display that the synthesized a phase Co-Ni bimetallic hydroxides have higher specific capacity than the theoretical specific capacity ofβ-Ni(OH)2 and demonstrate outstanding cycling durability even after 500 cycles. Furthermore, the cation exchange process is reversible. This simple method gives a novel way to construct nanostructural Co-Ni hydroxides with different compositions which behave excellent electrochemical properties different from that of nanostructural Co-Ni hydroxides prepared by traditional method.
4. Modifying the surface of macro-spherical Ni(OH)2 powder by forming a conductive network with metal cobalt, cobalt oxides or cobalt hydroxides can enhance the conductivity of macro-spherical Ni(OH)2 powder intensely. The coating methods regularly used only include plating and precipitation. Here, we successfully introduced cation-exchange method as a simple and versatile way to modify the surface layer of macro-spherical Ni(OH)2 particles to form the core-shell Ni(OH)2@CoOOH. Because the cation-exchange process takes place in situ, the shape and morphology of the precursor can ben preserved well in the resulting core-shell Ni(OH)2@CoOOH. The prepared core-shell structured Ni(OH)2@CoOOH exhibits unusual firm combination between shell CoOOH and the core of Ni(OH)2, which are considered to be linked by a traditional phase of a-Ni(OH)2. This type of structure not only enhances the firm combination between shell CoOOH and the core of Ni(OH)2 leading outstanding electrochemical cycling durability of Ni(OH)2@CoOOH, but also increases the specific capacity which is higher than the theoretical specific capacity ofβ-Ni(OH)2.The conductivity of starting Ni(OH)2 is improved highly by the modification of CoOOH in the surface of Ni(OH)2. The electrochemical tests show that the as-synthesized core-shell Ni(OH)2@CoOOH can be activated easily in a few cycles using currents of 0.5-2C when used as positive electrode material in MH-Ni batteries.In addition, the reaction mechanism concerned in the synthesis process was discussed.
Given to the simple synthesis process of Ni(OH)2@CoOOH and the advantages of it, such as the high conductivity, easy to be activated, larger specific capacity, outstanding cycling durability, the produce of Ni(OH)2@CoOOH is magnified to tens of grams for exploring the feasibility in industrial production. When obtained Ni(OH)2@CoOOH sample was chosen as cathode material in a 6Ah prismatic power battery, discharge efficiency of 74.19% at the discharge current rate of 30C was achieved as compared to the discharge efficiency (1.86%) of a 6Ah prismatic power battery with normal commercial spherical Ni(OH)2 as positive material and with adding of CoO as conductive additive in the paste for producing CoOOH.
1.纳米Ni(OH)2具有特殊的结构特性,被认为具有比微米级球形氢氧化镍更好的电化学性能。但目前系统研究纳米Ni(OH)2的制备及其形貌、结构等因素与其电化学性能关系的还很少。为了对纳米Ni(OH)2的这种关系有进一步的了解,本文采用水热法控制合成了系列均匀片状纳米Ni(OH)2,对合成的系列纳米Ni(OH)2的循环伏安、倍率放电等性能作了详尽的研究,并与商业化球形氢氧化镍进行了对比,结合XRD、SEM和HRTEM等结构分析方法得出以下的结论：①纳米Ni(OH)2有更高的电化学反应活性和快速活化能力,但并非所有的纳米级氢氧化镍均较微米级的球形氢氧化镍在电化学性能方面表现出优势。②降低纳米Ni(OH)2在垂直于[100]晶轴方向的结晶性,可以提高其电化学活性和比容量。③在理解纳米Ni(OH)2的粒径对其电化学性能的影响方面,不能单纯地追求单个颗粒整体的大小对电化学性能的影响,还应该考虑到颗粒中存在的不完全的结晶和优先生长可能对其电化学性能带来的影响。
2.纳米Ni(OH)2具有电化学活性高、充电效率高及放电平台高等优点,但存在易于团聚、在使用过程中难与导电剂均匀混合等问题导致其纳米特性难以得到很好的体现。为了克服上述问题,我们利用超声波处理方法,在液相中把现场生成的纳米Ni(OH)2微粒直接均匀地分散负载于纳米级的碳基微粒材料表面,使两者均匀复合成一种新型材料。不仅解决了现有技术中存在的纳米Ni(OH)2活性材料的分散问题,确保了Ni(OH)2纳米特性,同时也使其导电性得到提高。电化学测试证实此种复合材料具有优异的大电流充放电特性,活性材料的利用率也得到明显提高。
3. a-Ni(OH)2中的Ni元素在电化学反应中的理论交换电子数约为1.7,远大于β-Ni(OH)2的1个交换电子,故合成稳定的a-Ni(OH)2是提高MH/Ni电池正极比容量的重要途径。我们首次采用部分阳离子交换法制备出一系列α相Ni-Co氢氧化物。循环伏安研究表明所合成的a相Ni-Co氢氧化物比共沉淀法合成的β相Ni-Co氢氧化物具有更低的电阻和更好的电化学可逆性。充放电测试表明所合成的α相Ni-Co氢氧化物的比容量远高于β-Ni(OH)2的理论比容量,并且在500周循环后仍保持有很好的容量特性和充放电性能。通过调节Ni-Co氢氧化物的组成,还可以调控其电化学性能。此外,阳离子交换反应还可以可逆进行。阳离子交换方法是一个构筑不同组成的双金属氢氧化物的简便的新方法,并且以此方法制备的材料呈现出不同于传统方法所得产物的优异电化学性能。
4.在微米级球形Ni(OH)2表面进行钴元素的包覆,可在其表面形成导电网络,有效提高其导电性。通常采用的覆钴方法主要是化学沉积法和电沉积法。本文采用了一种新方法—阳离子交换方法,成功地合成了系列具有核-壳结构的Ni(OH)2@CoOOH样品。这种原位的阳离子交换合成过程使得产物Ni(OH)2@CoOOH完好地保持了初始球形Ni(OH)2的结构和形貌,并且表层CoOOH与内部Ni(OH)2核是通过过渡相a-Ni(OH)2贯通起来的。这种结构不仅增强了CoOOH与Ni(OH)2之间接合的牢固度,使得此种材料的循环稳定性得到了明显的提高,而且还使其作为MH/Ni电池的正极材料时的比容量得到提高,超过了β-Ni(OH)2的理论比容量。覆钴材料的导电性和活化特性也得到了极大的提高,可用0.5-2C的倍率在几周内完全活化。此外,还探讨了Ni(OH)2@CoOOH的制备方法所涉及的反应机理。
鉴于所开发的核-壳结构Ni(OH)2@CoOOH的制备方法简单,所得到的材料具有导电性高、易于活化、比容量高、循环性能好等优点,我们对此种材料的单批合成量成功地进行了放大,并采用所制备的大批量Ni(OH)2@CoOOH材料组装了方形动力电池(6Ah)。电化学测试结果表明,当电池的放电倍率提高到30C时仍保持有74.19%的放电效率,而用以制备核-壳结构Ni(OH)2@CoOOH材料的原料球形Ni(OH)2加入CoO作为导电添加剂所制作的对比电池在30C放电时的放电效率降到了1.86%。
The increasing concerns over air pollution and depletion of natural energy resources reserves have spurred renewed interest in electric vehicles (EV), where high power batteries are playing important role. MH/Ni batteries named as high specific energy green power sources are considered to be one of the most promising choices for EV and hybrid electric vehicle (HEV) applications. Furthermore, MH/Ni batteries are the first one which was used as power batteries in commercial HEVs. These batteries are usually designed with capacity limited by positive electrode for reasons of proper gas recombination reactions and battery safety. It follows that increasing the comprehensive performance of the nickel hydroxide electrode is essential for raising the performance of MH/Ni batteries. It's the purpose of this thesis that increasing the high rate dischargeability and energy density of nickel hydroxide electrode by the synthesis of plate like nano-scale nickel hydroxide, nickel hydroxide/carbon composites and nanosheets ofα-Ni/Co hydroxides through various methods and modifying macro-spherical nickel hydroxide with cobalt oxyhydroxide via a new method.
1. Owing to the special structural characteristics, nickel hydroxide with nanostructural multiphase was considered to have better electrochemical properties than that of spherical nickel hydroxide. However, as far as we know, few researches touch on the synthesis of a series of nano-scale nickel hydroxides and the systematical investigation of the structure/function relationships in nano-scale nickel hydroxides. For the purpose of understanding the structure/function relationships in nano-scale nickel hydroxides, a series of large-scale nickel hydroxide nanoplates with differences in size and crystallinity were synthesized in this work. Through cyclic voltammetry and rate-discharge electrochemistry tests combining the XRD、SEM and HR-TEM analysis of the structure of nano-scale nickel hydroxides, the conclusions was obtained as followings:①Nickel hydroxides with nanostructure have higher electrochemical reaction activity and are more easily activated than macro-spherical nickel hydroxide. However, not all nano-scale nickel hydroxides behave better electrochemical properties than macro-spherical Ni(OH)2.②Electrochemical activity and specific capacity of nano-scale nickel hydroxides could be improved by reducing the crystalline in the direction perpendicular to the axis of [100].③Not only the size of single nanometer nickel hydroxide but also the defects in crystals and un-perfect crystallization of single particles have influence on its electrochemical properties.
2. Numerous researches have indicated that nanometer nickel hydroxides have better electrochemical reaction activity, higher charging efficiency and higher discharge potential than macro-spherical Ni(OH)2. However, the nature that nanometer Ni(OH)2 is prone to aggregate, which causes nanometer Ni(OH)2 to be difficult to mix with conductive materials effectively, blocks the behaving of the characteristics of nanometer Ni(OH)2. To overcome this problem, a new kind of composite was synthesized by loading the nanometer Ni(OH)2 uniformly onto the surface of nano-scale spherical carbon particles via sonochemical technique. In this way, not only the dispersion problem of nanometer Ni(OH)2 is resolved which guarantees the behaving of the characteristics of nanometer Ni(OH)2, but also the conductivity of nanometer Ni(OH)2 is improved intensively. In addition, the electrochemical tests show that this kind of material behaves excellent high rate dischargeability, and the utilization of the active material is raised.
3. The number of theoretical exchangeable electrons per nickel atom inα-Ni(OH)2 reaches about 1.7 which is far larger than that ofβ-Ni(OH)2 (1). Therefore, synthesing stabilizedα-Ni(OH)2 is an effective way to increase the specific capacity of Ni(OH)2 cathode. Here, as far as we known, the partial cation exchange method was firstly and successfully adopted for the synthesis of a series of 2D Co-Ni bimetallic hydroxides. The cyclic voltammetry tests show that the synthesizedαphase Co-Ni bimetallic hydroxides have lower resistance and better reversibility than that ofβphase Co-Ni bimetallic hydroxides prepared by co-deposition method. In addition, the charge-discharge tests display that the synthesized a phase Co-Ni bimetallic hydroxides have higher specific capacity than the theoretical specific capacity ofβ-Ni(OH)2 and demonstrate outstanding cycling durability even after 500 cycles. Furthermore, the cation exchange process is reversible. This simple method gives a novel way to construct nanostructural Co-Ni hydroxides with different compositions which behave excellent electrochemical properties different from that of nanostructural Co-Ni hydroxides prepared by traditional method.
4. Modifying the surface of macro-spherical Ni(OH)2 powder by forming a conductive network with metal cobalt, cobalt oxides or cobalt hydroxides can enhance the conductivity of macro-spherical Ni(OH)2 powder intensely. The coating methods regularly used only include plating and precipitation. Here, we successfully introduced cation-exchange method as a simple and versatile way to modify the surface layer of macro-spherical Ni(OH)2 particles to form the core-shell Ni(OH)2@CoOOH. Because the cation-exchange process takes place in situ, the shape and morphology of the precursor can ben preserved well in the resulting core-shell Ni(OH)2@CoOOH. The prepared core-shell structured Ni(OH)2@CoOOH exhibits unusual firm combination between shell CoOOH and the core of Ni(OH)2, which are considered to be linked by a traditional phase of a-Ni(OH)2. This type of structure not only enhances the firm combination between shell CoOOH and the core of Ni(OH)2 leading outstanding electrochemical cycling durability of Ni(OH)2@CoOOH, but also increases the specific capacity which is higher than the theoretical specific capacity ofβ-Ni(OH)2.The conductivity of starting Ni(OH)2 is improved highly by the modification of CoOOH in the surface of Ni(OH)2. The electrochemical tests show that the as-synthesized core-shell Ni(OH)2@CoOOH can be activated easily in a few cycles using currents of 0.5-2C when used as positive electrode material in MH-Ni batteries.In addition, the reaction mechanism concerned in the synthesis process was discussed.
Given to the simple synthesis process of Ni(OH)2@CoOOH and the advantages of it, such as the high conductivity, easy to be activated, larger specific capacity, outstanding cycling durability, the produce of Ni(OH)2@CoOOH is magnified to tens of grams for exploring the feasibility in industrial production. When obtained Ni(OH)2@CoOOH sample was chosen as cathode material in a 6Ah prismatic power battery, discharge efficiency of 74.19% at the discharge current rate of 30C was achieved as compared to the discharge efficiency (1.86%) of a 6Ah prismatic power battery with normal commercial spherical Ni(OH)2 as positive material and with adding of CoO as conductive additive in the paste for producing CoOOH.
引文
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