磷酸铁纳米材料的制备及在生物传感和锂离子电池正极材料中的应用
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摘要
磷酸铁(FePO4)具有良好的生物相容性、丰富的P043-和稳定的3D骨架结构,已广泛应用于催化领域,并在生物传感和新能源领域有着潜在的应用。因此,研究FePO4及其纳米复合物的制备方法并应用于生物传感和新能源领域,有利于生态环境的保护。本文以FePO4为研究对象,发展了简单、快速制备FePO4纳米材料及其复合材料的方法,并研究了FePO4及其纳米复合材料在生物传感和锂离子电池中的应用,拓展了FePO4的应用范围。本论文的主要研究内容及结果有：
     (1)利用微波法制备了FePO4纳米材料并研究了其在蛋白质固定及生物传感方面的应用
     利用快速简单的微波法制备了FePO4纳米材料。用透射电镜(TEM)、扫描电镜(SEM)、能量散射光谱仪(EDS)、X(?)衬线光电子能谱(XPS)、X--射线粉末衍射(XRD)、红外光谱光谱(FT-IR)和紫外可见光谱(UV-vis)等技术对产物进行了表征；结果表明,所得FePO4纳米材料的形貌和尺寸受表面活性剂的种类和前驱体(Fe2+/PO43-)物质的量的比的影响。当使用阳离子表面活性剂CTAB作为稳定剂时,得到分散均匀的FePO4纳米球；如使用阴离子表面活性剂SDS或非离子表面活性剂PEG和PVP时,产物易团聚。当Fe2+/PO43-物质的量的比为1：2时,得到平均粒径约(50±10)nm的FePO4纳米球；当前驱体物质的量的比为1：1和2：1时,FePO4纳米球的平均粒径分别增加到(80±20)和(150±20)nin。将血红素类蛋白质(以肌红蛋白Mb为例)固定在FePO4纳米材料表面,制备了Mb-FePO4/GC电极,研究了Mb在FePO4纳米材料表面的直接电子转移及对H202还原的电催化性能,结果表明,固定在FePO4纳米材料表面的Mb能够保持其原有的天然结构,其循环伏安曲线上呈现出了一对良好的、准可逆的氧化还原峰,峰电位分别为Epa=-284mV,Epc=-373mV (100mVs-1),式量电位Eo’约为-(330±3.0)mV(pH6.8),电子转移表观速率常数约为ks=5.54s-1,说明Mb在FePO4纳米材料表面能进行有效的直接电子转移反应。Mb-FePO4/GC电极对H202的还原表现出良好的电催化性能,催化电流与H202浓度在0.01-2.5mmol L-1的范围内成良好的线性关系,最低检测限约(5±1)μmol L-1,灵敏度为(85±3) μA (mmol L-1)-1cm-2,并具有良好的重现性和稳定性,可作为检测H202的生物传感器。因此,FePO4纳米材料能够促进蛋白质／酶和电极间的直接电子转移,可用于构建检测H202的生物传感,拓宽了其在生物电化学中的应用范围。
     (2)普鲁士蓝(PB)对FePO4纳米材料表面的修饰及用于胆碱氧化酶(ChOx)的固定和胆碱的电化学测定
     胆碱是脑组织中类胆碱功能活性的标识物,在生物和临床分析中,特别是在神经变性疾病的临床检测中非常重要。我们提出通过电化学方法基于普鲁士蓝(PB)修饰的FePO4纳米复合材料(PB-FePO4)实现对胆碱的检测。用透射电镜(TEM)、X-射线粉末衍射(XRD)、红外光谱光谱(FT-IR)和紫外可见光谱(UV-vis)等技术对产物进行了表征；结果表明,通过简单的方法可以在FePO4纳米材料的表面修饰PB形成PB-FePO4纳米复合材料。将胆碱氧化酶(ChOx)固定在PB-FePO4纳米材料表面制备了ChOx-PDDA-PB-FePO4/GC电极,研究了ChOx对胆碱的电催化性能,结果表明固定在PB-FePO4纳米复合材料表面的ChOx能够保持其生物活性,对胆碱表现出良好的电催化性能。研究了溶液的pH、温度和检测电压对修饰电极响应的影响,结果表明当溶液pH为8.0、温度为37℃和检测电位为-0.05V时具有最佳响应,催化电流与胆碱浓度在2μmol L-1-3.2mmol L-1范围内呈良好的线性关系,最低检测限约(0.4±0.05)灵敏度约为75.2μA (mmol L-1)-1cm-2,并具有良好的重现性和稳定性。另外,当检测电位为-0.05V(相对于饱和甘汞电极)时能够有效避免常见的干扰物质如抗坏血酸、尿酸和4-乙酰氨基苯酚的干扰。因此,该纳米复合材料能够作为合适的平台构建基于其他氧化酶的生物传感。
     (3)制备了壳厚可调的FePO4纳米空心球并用于锂离子电池的正极材料
     利用水热法一步合成了FePO4纳米空心球。用透射电镜(TEM)、高分辨透射电镜(HRTEM)、扫描电镜(SEM)、能量散射光谱仪(EDS)、X-射线光电子能谱(XPS)、X-射线粉末衍射(XRD)等技术对产物进行了表征；结果表明产物为非晶态的FePO4纳米空心球(平均粒径约250nm),壳壁厚度为40nm。研究了前驱体(Fe2+/PO43-)物质的量的比、表面活性剂SDS的量和反应时间对产物形貌的影响,结果表明,SDS的量和反应时间是合成纳米空心球的关键条件；在0.05g SDS和反应时间为12h时,通过调节反应前驱体(Fe2+/PO43-)的物质的量比可以实现对纳米球的形貌和壳壁厚度的可控合成；当Fe2+/PO43-物质的量的比为1：1时,得到FePO4纳米实心球(平均粒径约250nm)；当前驱体物质的量的比大于1：l时,得到平均粒径约250nm的FePO4空心球,且随着前驱体物质的量的比的增加,空心球的壳壁厚度减小；当前驱体物质的量的比为1：2时,空心球的壳壁厚约40nm；当前驱体物质的量的比增加到1：3和1：4时,空心球的壳壁厚分别减少至22和10nm。以该非晶态FePO4纳米空心球作为锂离子电池的正极材料,研究了其循环性能和倍率性能。电流密度为20mA g-1时,壳壁厚为10nm、22nm和40nm的纳米空心球,其放电比容量分别为170.5、166.2和159.4mAh g-1;50次循环后,比容量分别保持在167.1、163.8和156.6mAh g-1,表现出良好的循环稳定性；壳壁厚为10nm的FePO4纳米空心球在100、200、500、1000和2000mAg-1的电流密度下,放电比容量分别为141.8.135.6.118.5.100.3.76.3mAh g1;随着空心球壳壁厚度的增加,倍率性能略有降低。FePO4纳米空心球的比容量、循环性能和倍率性能明显优于纳米实心球,独特的空心结构有利于Li+的快速扩散,大的比表面积增加了电极和电解质的接触面,有效降低电流密度,减少大电流充放电下对电极材料的破坏程度。因此,FePO4纳米空心球是最具开发和应用潜力的新一代锂离子正极材料,同时该方法还为提高锂离子电池电极材料特别是低电导率电极材料的比容量和倍率性能提供了一种有效、方便的途径。
     (4)制备了石墨烯-FePO4纳米空心球复合物并用于锂离子电池的正极材料
     通过一步合成法制备了石墨烯-FePO4纳米空心球复合物(非晶态FePO4纳米空心球直接生长在石墨烯的表面)。用透射电镜(TEM)、高分辨透射电镜(HRTEM).扫描电镜(SEM)、能量散射光谱仪(EDS)、X-射线光电子能谱(XPS)、X-射线粉末衍射(XRD)、红外光谱光谱(FT-IR)等技术对产物进行了表征；结果表明非晶态FePO4纳米空心球均匀地分散在石墨烯上,空心球粒径约50nm,壁厚约4nm。研究了表面活性剂对产物形貌的影响,结果表明适量的SDS有利于FePO4空心球的形成,当SDS为0.1g时,可以制备出石墨烯-FePO4空心球复合物。以该复合物作为锂离子电池的正极材料,研究了其循环性能和倍率性能。电流密度为20mA g-1时,放电比容量为174.1mAhg-1;50次循环后,放电比容量仍保持在173.3mAh g-1,表现出良好的循环稳定性；电流密度为100、200、500和1000mA g-1时,放电比容量分别为157.2、149.1、121.4和99.2mAhg-1,表现出高倍率性能。该复合材料促进了Li+的快速扩散和电子的传递,具有高比容量、良好的循环稳定性和高倍率性能,有望成为最具开发和应用潜力的新一代锂离子正极材料。这种直接生长在石墨烯上方法为提高锂离子电池电极材料特别是高度绝缘的电极材料的比容量和倍率性能提供了一种有效、方便的途径,同时该方法也适合于工业合成各种基于石墨烯的纳米复合材料。
With good biocompatibility, abundant PO43-, and3D skeleton structure, FePO4has been widely applicated in catalysis, which also has potential application in biosenseor and new energy. Research of FePO4and its composite is beneficial to the protection of the ecological environment. This work develops the facile synthesis of FePO4and its composite. Their application in sensors and lithium ion battery is investigated, which expand the platform of application. The main conclusions are summarized as following:
     (1) Iron phosphate nanostructures synthesized by microwave method and their applications in biosensing
     A fast, simple microwave heating method has been developed for synthesizing iron phosphate (FePO4) nanostructures. The nanostructures were characterized and confirmed by transmission electronic microscope (TEM), scanning electronic microscope (SEM), energy dispersive x-ray spectroscopy (EDS), x-ray photoelectron spectroscopy (XPS), x-ray powder diffraction (XRD), Fourier transform infrared (FT-IR), and UV-vis spectroscopy. The morphology and the size of the nanomaterials are significantly influenced by the concentration of the precursors and the kinds of surfactants. CTAB plays a crucial role in controlling the spherical morphology of the product, as well as preventing the nanomaterials from aggregation. The nanoparticles are easily aggregated in the course of their growth in the case of SDS, PEG and PVP. The nanospheres with the average diameters of (50±10) nm are obtained at the molar ratio of1:2. The average size of the nanomaterials increases to (80±20) and (150±20) nm, respectively, at the molar ratio of1:1and2:1. The nanostructures have been employed as electrode substrate to immobilize myoglobin (Mb) and to facilitate the direct electron transfer (DET) reaction of the protein. After immobilized on the nanomaterials, Mb can keep its natural structure and undergo effective DET reaction with a pair of well-defined redox peak, the anodic (Epa) and cathodic (Epc) peak potentials of at ca.-284and-373mV, respectively, at a scan rate of100mV s-1. The formal potential, E0' is found to be-(330±3.0) mV (pH6.8) and the apparent electron transfer rate constant of5.54s-1. The Mb-FePO4/GC electrode displays good features in electrocatalytic reduction of H2O2, and thus can be used as a biosensor for detecting the substrate. The response displays a good linear range from0.01to2.5mM, the sensitivity is evaluated to be ca.(85±3) μA mM-1cm-2. The detection limit is estimated to be ca.(5±1) μM with good stability and reproducibility. Therefore, FePO4 nanomaterials can be become a simple and effective biosensing platform for the integration of proteins/enzymes and electrodes, which can provide analytical access to a large group of enzymes for a wide range of bioelectrochemical applications.
     (2) Indirect electrocatalytic determination of choline by monitoring hydrogen peroxide at the choline oxidase-prussian blue modified iron phosphate nanostructures
     Choline, as a marker of cholinergic activity in brain tissue, is very important in biological and clinical analysis, especially in the clinic detection of the neurodegenerative disorders disease. This work presents an electrochemical approach for the detection of choline based on Prussian blue (PB) modified iron phosphate (FePO4) nanostructures (PB-FePO4). The nanostructures were characterized and confirmed by transmission electronic microscope (TEM), x-ray powder diffraction (XRD), Fourier transform infrared (FT-IR), and UV-vis spectroscopy. The nanostructures have been employed as electrode substrate to immobilize ChOx. After immobilized on the nanomaterials, ChOx can keep its electrocatalytic reduction of Choline. The response current of the biosensor usually depends on the solution pH, performance temperature, and detection potential. The pH8.0、temperature37℃and the detection potential of-0.05V are chosen as the optimal condition for the ChOx-PDDA-PB-FePO4/GC electrode sensing choline chloride. The response current displays a good linear range2μM-3.2mM. The sensitivity is evaluated to be-75.2μA mM-1cm-2. The detection limit is estimated to be ca.0.4±0.05μM. The electrode displays good stability and repeatability. In addition, the common interfering species, such as ascorbic acid, uric acid and4-acetamidophenol did not cause obvious interference due to the low detection potential (-0.05V vs. saturated calomel electrode). This nanostructure could be used as a platform for the construction of other oxidase-based biosensors.
     (3) Enhanced cathode performances of amorphous FePO4hollow nanospheres with tunable shell thickness in lithium ion batteries
     We report the facile synthesis of an amorphous FePO4hollow nanosphere with tunable shell thickness for use as a cathode material in lithium ion batteries (LIBs). The nanostructures were characterized and confirmed by transmission electronic microscope (TEM, HRTEM), scanning electronic microscope (SEM), energy dispersive x-ray spectroscopy (EDS), x-ray photoelectron spectroscopy (XPS) and x-ray powder diffraction (XRD). The morphology and the size of the nanomaterials are significantly influenced by the amount of surfactant SDS and reaction time. The0.05g SDS and12h are chosen as the optimal condition. The thickness of the shell of the prepared sample can be easily controlled by adjusting the molar ratio of the precursors. When the samples were prepared at the Fe2+/PO43-ratio of1:1, FePO4solid nanospheres with the average diameters of (250±20) nm were obtained. While the samples were prepared at the Fe2+/PO43-ratio higher than1:1, FePO4hollow nanospheres were obtained. Moreover, the shell thickness of the nanospheres significantly depends on the ratio of the precursors. It decreases from approximately40nm at the ratio of1:2to about10nm at the ratio of1:4. At a current rate of20mA g-1The first discharge-charge cycle delivered specific capacities of170.5,166.2and159.4mAh g-1, respectively, for the hollow nanosphere with shell thickness of10nm,22and40nm, respectively. The discharge capacity maintains a reversible capacity after50cycles of approximately167.1,163.8and156.6mAh g-1, respectively. The discharge capacities were approximately166,150,133,114, and90mAh g-1at current rates of100,200,500,1000, and2000mA g-1, respectively, for the nanospheres with shell thickness of10nm. Moreover, with increase of the shell thickness, the rate capacities have only slight decrease. These results indicate good cycling stability and a good rate performance of the hollow nanosphere. The electrochemical performance of these hollow nanospheres was much better than that of the solid nanospheres.The high rate capacity is due to the unique hollow structure of the FePO4nanospheres, which shortens the diffusion path for both electrons and Li+ions, ensures a high electrode-electrolyte contact area, and offers more active sites for electrochemical reactions. The approach offers an effective route to improve the performance of highly insulating electrode materials for batteries.
     (4) Graphene-Amorphous Hollow FePO4Nanosphere Hybrids as Cathode Materials for Lithium Ion Batteries
     A facile one-step synthesis approach to prepare the graphene-amorphous hollow FePO4nanosphere hybrids (amorphous hollow FePO4nanospheres were directly grew on graphene) for use as cathode materials in lithium ion batteries (LIBs) is developed. The nanostructures were characterized and confirmed by transmission electronic microscope (TEM, HRTEM), scanning electronic microscope (SEM), energy dispersive x-ray spectroscopy (EDS), x-ray photoelectron spectroscopy (XPS), x-ray powder diffraction (XRD) and Fourier transform infrared (FT-IR). The0.1g SDS is chosen as the optimal condition.This hybrid exhibits good electrochemical performance with high specific capacity up to174.1mAh g-1(at a current rate of20mA g-1), the discharge capacity maintains a reversible capacity after50cycles of approximately173.3mAh g-1. The discharge capacities were approximately157.2,149.1,121.4, and99.2mAh g-1based on the weight of amorphous FePO4hollow nanospheres at current rates of100,200,500, and1000mA g-1, respectively, indicating good capacity retention and high rate capability upon cycling due to facile Li+ions diffusion through the thin wall of the hollow FePO4nanospheres and fast electron transport through the graphene. The hybrid could be a promising candidate material for a high-capacity, low-cost, and environmentally friendly cathode for LIBs. The growth-on-graphene approach offers an effective and convenient technique to improve the specific capacities and rate capabilities of highly insulating electrode material in battery area, and is also beneficial to the industrial-scale synthesis of various graphene-based hybrid nanomaterials.
引文
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