类普鲁士蓝基正极材料的优化制备及其性能研究

目前以锂离子电池为代表的电化学储能技术已经得到了广泛的开发及应用。然而，随着电子器件、电动汽车等的逐渐普及，锂资源匮乏与分布不均而导致的成本问题严重阻碍了锂离子电池的进一步应用。钠作为锂的同主族、相邻周期的金属，其储量丰富、成本低廉，因此钠离子电池的开发和应用得到了科研工作者和新能源行业的特别关注。钠离子电池具有与锂离子电池类同的工作机理和结构，其负极材料和电解液的研究较为成熟，而正极材料的开发与制备则逐渐成为钠离子电池发展的瓶颈。

类普鲁士蓝材料因其三维框架结构利于钠离子可逆穿梭而被视为一种极具应用前景的正极材料。但由于传统共沉淀方法所制备的类普鲁士蓝材料其结构中存在大量的亚铁氰根空位和水分子，严重影响了其电化学性能。目前常用的解决办法为添加螯合剂来降低沉淀速率，但此种方法容易造成粒径偏大，钠离子在其晶体结构中传输较为困难，从而造成倍率性能较差。本论文主要集中在纳米类普鲁士蓝材料的优化制备及其储钠性能研究，旨在通过不同纳米化方法降低类普鲁士蓝尺寸，增大活性位点并加快离子扩散，最终提升材料的循环性能和倍率性能。具体研究内容如下：

（1）两步水热法制备石墨烯包覆类普鲁士蓝复合材料：通过先合成石墨烯包覆的过渡金属氢氧化物前驱体，再将其与亚铁氰化钠反应，利用固相前驱体和类普鲁士蓝的缓慢转化导致类普鲁士蓝材料粒径减小，石墨烯包覆有利于增加电导率。制备出的Ni_0.33Co_0.67HCF@rGO复合正极材料粒径为100~200 nm，在钠离子半电池中能够提供97.7 mAh g^-1的容量；在50 mA g^-1的电流密度下经2000圈循环后容量保持率为80.2%；在10 C的充放电倍率下，仍具有70.8 mAh g^-1的放电容量。

（2）限域空间合成纳米尺寸类普鲁士蓝材料：将亚铁氰根离子嵌入层状双金属氢氧化物层间，再将其与过渡金属盐反应获得晶粒尺寸小至几纳米的类普鲁士蓝材料，作为钠离子半电池的正极材料能够提供82.9 mAh g^-1的容量，在50 mA g^-1的电流密度下经1750圈循环后容量保持率为74.3%；在10 C的充放电倍率下，仍具有35.6 mAh g^-1的放电容量。

At present, the electrochemical energy storage technology has been well developed and widely applied, especially lithium-ion batteries. However, with the gradual popularization of electronic devices, electric vehicles, etc., the cost problem caused by the scarcity and uneven distribution of lithium resources has seriously hindered the further application of lithium-ion batteries. Sodium, a metal element with adjacent period in the same group of lithium, has abundant reserves and low cost. Therefore, the development and application of sodium-ion batteries has received special attention from researchers and new energy enterprises. Na-ion batteries have the same working mechanism and component as lithium-ion batteries. The research on anode materials and electrolytes is relatively mature, while the development and preparation of cathode materials has gradually become a bottleneck in the development of sodium-ion batteries.

Prussian blue analogue materials are regarded as a promising cathode material because of its three-dimensional framework that facilitates the reversible migration of sodium ions. However, prussian blue analogue materials prepared by the traditional co-precipitation method have a large number of ferrocyanide vacancies and water molecules in their structure, which seriously affect their electrochemical performance. The commonly used solution is to add a chelating agent to reduce the precipitation rate; however, this method usually causes large particle size, which would result in poor rate performance. This paper mainly focuses on the optimal preparation of nano-prussian blue analogue materials and their sodium storage properties, aiming to reduce the size of prussian blue analogue materials, increase the active site and facilitate the sodium ion diffusion, and finally improve the cycling performance and rate performance of the materials .The specific research content is as follows:

(1) Preparation and performance of graphene-coated prussian blue analogue composites by two-step hydrothermal method: the material can be fabricated by reacting pre-obtained graphene-coated transition metal hydroxide precursor with sodium ferrocyanide. The slow conversion rate of the solid phase precursor and prussian blue analogue leads to the reduction of prussian blue analogue particle size, and the graphene coating can be benefit for charge transfor. As a result, the Ni_0.33Co_0.67HCF@rGO composite cathode material with a particle size of 100 to 200 nm can provide a capacity of 97.7 mAh g^-1 in a sodium-ion half-cell, and the capacity retention rate is 80.2% after 2000 cycles at a current density of 50 mA g^-1; it still has a discharge capacity of 70.8 mAh g^-1 at a rate of 1 A g^-1.

(2) Confined synthesis of prussian blue analogue nanomaterials: the ferrocyanide ions embedded in the slabs of layered double hydroxide can react with transition metal salts to obtain prussian blue analogue materials with a small grain size of around a few nanometers. As the anode material for sodium ion half-cell, it can provide a capacity of 82.9 mAh g^-1, and the capacity retention rate is 74.3% after 1750 cycles; at a rate of 1 A g^-1, it still has a discharge capacity of 35.6 mAh g^-1.

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