铁（Ⅲ）氧化物修饰微生物燃料电池阳极及其电容特性研究
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摘要
微生物燃料电池(Microbial fuel cell, MFC)在污水处理的同时可回收清洁能源——电能,是一种真正意义上的可持续的绿色能源技术,成为当今世界科学工作者的研究热点之一,为合理解决水体污染以及能源危机问题提供了新思路。然而考虑到MFC的未来应用,存在着功率密度低、电极成本高等诸多问题,其中阳极与电化学活性微生物间的电子传递过程成为关键限制因素。
MFC阳极的电化学活性微生物主要由异化金属还原菌构成。研究指出铁(III)氧化物与异化金属还原菌的胞外细胞色素C具有高度亲和性,能够作为电子受体而被还原；此外,不锈钢网金属集流体的机械强度高,导电性能优于常规碳电极,成为目前电极材料发展的主方向。
本论文首次以不锈钢网作为集流体,超级电容活性炭作为阳极微生物的载体,采用辊压工艺,通过聚四氟乙烯乳液的粘结作用,开发了新型阳极(AcM),以乙酸钠人工模拟废水为底物,构建单室无膜空气阴极微生物燃料电池。研究表明,AcM价格相对低廉,机械强度高,与阳极为碳纤维布的相同构型的MFC体系相比,其输出功率略高3.0%,可见该新型阳极有利于MFC技术的市场化推广,商业化应用前景广阔。
纳米半导体α-FeOOH修饰AcM电极,电化学测试发现MFC体系极化内阻减小、交换电流密度及阳极峰电流增加,表明α-FeOOH促进了阳极与微生物间的电子传递；阳极常相位角元件增加、韦伯阻抗减小,表明α-FeOOH提高了阳极表面电子扩散能力,增大了阳极电容；在α-FeOOH质量百分含量由0、2.5%增长到5.0%时,MFC体系的最大输出功率密度从508±40mW/m2上升到637士51mW/m2、并进一步增加到693士20mW／m2,然而∝-FeOOH含量继续增加到7.5%时,最大输出功率密度反而下降至(?)639±30mW/m2,原因可能是生物还原的Fe(II)吸附沉积在电极表面,降低了阳极的导电性、扩散性及电容性能。
针对纳米Fe304修饰的AcM阳极(AcFeM),电化学Tafel测试表明AcFeM的动力学活性增加,最大输出功率密度由664士17mW/m2(AcM)上升到809士5mW/m2(Fe3O4wt.%=5.0%),提高了约22%；此外,本论文首次提出体系中Fe304的动力学活性起主导作用,证实Fe304的存在提高了MFC阳极的电容存储性能,且其电荷存储能力随MFC开路间隔的增加先增加后减少；当开路时间为20min时,AcFeM获得的最大电荷存储量为574.6C／m2。电化学循环伏安技术分析表明AcFeM的电容主要来源于碳的孔隙结构、阳极生物膜的类电容性以及可能充当固体中介体的Fe3O4/Fe(Ⅱ)氧化还原电对。
MFC极化曲线性能逆转的存在降低了其性能评估的准确性,基于阳极生物膜的类电容特性,以超级电容活性炭、普通活性炭、导电炭黑制备了电容大小不同的阳极UAC、PAC和CB1,研究了阳极材料电容对MFC极化曲线性能逆转的影响。结果表明,UAC的无菌阳极电容(Cmabiotic)最大(2.1F/cm2),在Cycle2～4内,UAC-MFC体系的极化曲线均未出现逆转现象；而PAC的Cmabiotic次之(1.6F/cm2), PAC-MFC体系的性能逆转在Cycle3时消失；CB1的Cmabiotic最小(0.5F/cm2), CB1-MFC体系的性能逆转在Cycle4时才得到消除,从而提出阳极材料的孔结构充当中介体而存储电子的作用机理,借以消除极化曲线的性能逆转现象。
为证明上述实验结果的可信性,对另一种小电容的炭黑材料(CB2)进行KOH、HN03的化学活化处理,并与5%的Fe304粉末制备成复合阳极,用以增加炭黑自身电容。研究发现,化学活化使炭黑表面引入了含氧官能团,改变了表面元素组成,提高了电极的亲水性,增加了阳极的Cmabiotic；但电极经Fe304修饰后,其电容仅略有增加；结果表明,无论是采用化学活化,还是通过生物富集或Fe304添加的方式补偿阳极电容,只有当炭黑阳极Cm≥1.1F/cm2时,极化曲线才不会出现逆转现象,从而进一步证实阳极材料电容不足会导致极化曲线性能逆转的产生。
It is well recognized that microbial fuel cell (MFC) is specified as the green energy technology due to its wastewater treatment accompanying with energy recovery. This provides a new trial for resolving water pollution and energy crisis. However, considering the practical application for the future, high cost and low power are still the main problems. Especially, the electron transfer rate between anode and bacteria is the key factor.
The exoelectrogenic bacteria in MFC mainly consists of dissimilatory metal-reducing bacteria (DIRB). It has been experimentally demonstrated that outer membrane c-type cytochromes (OMCs) have a high binding affinity to iron(Ⅲ) oxides. Furthermore, iron(Ⅲ) oxides can be recognized by DIRB and utilized as extracellular electron acceptor to be reduced. What's more, stainless steel mesh (SSM) is superior to conventional carbon electrode with higher mechanism and conductivity, and already being the research tide in electrode materials.
For the first time, a new type of anode (AcM) is composed of ultracapacitor activated carbon (UAC)/SSM and a polytetrafluoroethylene (PTFE) emulsion by a rolling press method. Sodium acetate is used as the synthetic substrate in single-chamber membrane-less air-cathode MFC. Comparing with carbon mesh (CM) as anode, it is lower cost and better mechanical strength with3.0%higher performance in power generation. Thus, there is bright prospect in favour of market promotion for MFC.
For AcM modified by nanosemconductor goethite, based on the decrease of polar resistance and the increases of both exchange current density and anodic peak current, it is verified that α-FeOOH added AcM kinetically promotes the extracellular electron transfer. The increase of constant-phase element and decrease of Warburg element manifest that the capacitance and diffusion condition on the surface of anode are enhanced. So, the maximum power density (MPD) arrives to the biggest increase of36%from508±40mW/m2(the control) to637±51mW/m2(2.5%α-FeOOH added), and then to693±20mW/m2(5.0%α-FeOOH added). Whereas, with the excess increment of7.5%, the MPD inversely decreases to639±30mW/m2, probably due to the lower conductivity, diffusion and capacitance under the adsorption of biogenic iron(Ⅱ) on the anodic surface.
For AcM modified by nano magnetite (AcFeM), Tafel tests indicate that AcFeM is also kinetically more advantageous, and the MPD of AcFeM (809±5mW/m2,5.0%Fe3O4added) is22%higher than that of AcM (664±17mW/m2) by polarization tests. It is the first time to point out that the dynamic activity of Fe3O4plays a leading role in accelerating the electron transfer, and beneficial to boost the transient charge storage of the anode. Furthermore, the net storage capacity initially increases followed by a decrease with the maximum capacitance of574.6C/m2for AcFeM under20min of open circuit interval. The cyclic voltammetry curves explain that the capacitance of AcFeM can be from three aspects:pore structure of carbon, capacitor-like behavior of anodic biofilm and the redox couple of Fe3O4/Fe(Ⅱ) as a solid-state electron shuttle.
Power overshoot commonly makes the MFC performance evaluation inaccurate. Based on the capacitive characteristic of anodic biofilm, three types of carbon with different capacitance (UAC, plain activated carbon (PAC) and carbon black (CB1)) are rolled on SSM as anodes to investigate the relationship between overshoot and anodic capacitance. It is exciting that the overshoot is not observed for UAC-MFC from Cycle2to4, while the phenomenon is eliminated in PAC-MFC from Cycle3and in CB[-MFC from Cycle4. This is relevant with the Cmabiotic of the anode following the order of UAC (2.1F/cm2)> PAC (1.6F/cm2)> CB1(0.5F/cm2). It is inferred that the Cmabiotlc of anode stores charges and function as electron shuttle to overcome the phenomenon.
In order to prove the credibility of the result above, another carbon black (CB2) with enhanced capacitance is produced via chemical activation with potassium hydroxide and nitric acid, and simultaneously made into composite anode with5.0%addition. It has been found that oxygen-containing functional groups are introduced and both the hydrophilicity and Cmabiotic of the electrode are also improved. But, before and after Fe3O4addition, there is a slight increase in anodic capacitance. It indicates that the overshoot phenomenon disappears only when Cm is larger than1.1F/cm2, in spite of through chemical activation or capacitance compensation from bacterial colonization and Fe3O4. This further strengthens that insufficient capacity of anode leads to the power overshoot.
MFC阳极的电化学活性微生物主要由异化金属还原菌构成。研究指出铁(III)氧化物与异化金属还原菌的胞外细胞色素C具有高度亲和性,能够作为电子受体而被还原；此外,不锈钢网金属集流体的机械强度高,导电性能优于常规碳电极,成为目前电极材料发展的主方向。
本论文首次以不锈钢网作为集流体,超级电容活性炭作为阳极微生物的载体,采用辊压工艺,通过聚四氟乙烯乳液的粘结作用,开发了新型阳极(AcM),以乙酸钠人工模拟废水为底物,构建单室无膜空气阴极微生物燃料电池。研究表明,AcM价格相对低廉,机械强度高,与阳极为碳纤维布的相同构型的MFC体系相比,其输出功率略高3.0%,可见该新型阳极有利于MFC技术的市场化推广,商业化应用前景广阔。
纳米半导体α-FeOOH修饰AcM电极,电化学测试发现MFC体系极化内阻减小、交换电流密度及阳极峰电流增加,表明α-FeOOH促进了阳极与微生物间的电子传递；阳极常相位角元件增加、韦伯阻抗减小,表明α-FeOOH提高了阳极表面电子扩散能力,增大了阳极电容；在α-FeOOH质量百分含量由0、2.5%增长到5.0%时,MFC体系的最大输出功率密度从508±40mW/m2上升到637士51mW/m2、并进一步增加到693士20mW／m2,然而∝-FeOOH含量继续增加到7.5%时,最大输出功率密度反而下降至(?)639±30mW/m2,原因可能是生物还原的Fe(II)吸附沉积在电极表面,降低了阳极的导电性、扩散性及电容性能。
针对纳米Fe304修饰的AcM阳极(AcFeM),电化学Tafel测试表明AcFeM的动力学活性增加,最大输出功率密度由664士17mW/m2(AcM)上升到809士5mW/m2(Fe3O4wt.%=5.0%),提高了约22%；此外,本论文首次提出体系中Fe304的动力学活性起主导作用,证实Fe304的存在提高了MFC阳极的电容存储性能,且其电荷存储能力随MFC开路间隔的增加先增加后减少；当开路时间为20min时,AcFeM获得的最大电荷存储量为574.6C／m2。电化学循环伏安技术分析表明AcFeM的电容主要来源于碳的孔隙结构、阳极生物膜的类电容性以及可能充当固体中介体的Fe3O4/Fe(Ⅱ)氧化还原电对。
MFC极化曲线性能逆转的存在降低了其性能评估的准确性,基于阳极生物膜的类电容特性,以超级电容活性炭、普通活性炭、导电炭黑制备了电容大小不同的阳极UAC、PAC和CB1,研究了阳极材料电容对MFC极化曲线性能逆转的影响。结果表明,UAC的无菌阳极电容(Cmabiotic)最大(2.1F/cm2),在Cycle2～4内,UAC-MFC体系的极化曲线均未出现逆转现象；而PAC的Cmabiotic次之(1.6F/cm2), PAC-MFC体系的性能逆转在Cycle3时消失；CB1的Cmabiotic最小(0.5F/cm2), CB1-MFC体系的性能逆转在Cycle4时才得到消除,从而提出阳极材料的孔结构充当中介体而存储电子的作用机理,借以消除极化曲线的性能逆转现象。
为证明上述实验结果的可信性,对另一种小电容的炭黑材料(CB2)进行KOH、HN03的化学活化处理,并与5%的Fe304粉末制备成复合阳极,用以增加炭黑自身电容。研究发现,化学活化使炭黑表面引入了含氧官能团,改变了表面元素组成,提高了电极的亲水性,增加了阳极的Cmabiotic；但电极经Fe304修饰后,其电容仅略有增加；结果表明,无论是采用化学活化,还是通过生物富集或Fe304添加的方式补偿阳极电容,只有当炭黑阳极Cm≥1.1F/cm2时,极化曲线才不会出现逆转现象,从而进一步证实阳极材料电容不足会导致极化曲线性能逆转的产生。
It is well recognized that microbial fuel cell (MFC) is specified as the green energy technology due to its wastewater treatment accompanying with energy recovery. This provides a new trial for resolving water pollution and energy crisis. However, considering the practical application for the future, high cost and low power are still the main problems. Especially, the electron transfer rate between anode and bacteria is the key factor.
The exoelectrogenic bacteria in MFC mainly consists of dissimilatory metal-reducing bacteria (DIRB). It has been experimentally demonstrated that outer membrane c-type cytochromes (OMCs) have a high binding affinity to iron(Ⅲ) oxides. Furthermore, iron(Ⅲ) oxides can be recognized by DIRB and utilized as extracellular electron acceptor to be reduced. What's more, stainless steel mesh (SSM) is superior to conventional carbon electrode with higher mechanism and conductivity, and already being the research tide in electrode materials.
For the first time, a new type of anode (AcM) is composed of ultracapacitor activated carbon (UAC)/SSM and a polytetrafluoroethylene (PTFE) emulsion by a rolling press method. Sodium acetate is used as the synthetic substrate in single-chamber membrane-less air-cathode MFC. Comparing with carbon mesh (CM) as anode, it is lower cost and better mechanical strength with3.0%higher performance in power generation. Thus, there is bright prospect in favour of market promotion for MFC.
For AcM modified by nanosemconductor goethite, based on the decrease of polar resistance and the increases of both exchange current density and anodic peak current, it is verified that α-FeOOH added AcM kinetically promotes the extracellular electron transfer. The increase of constant-phase element and decrease of Warburg element manifest that the capacitance and diffusion condition on the surface of anode are enhanced. So, the maximum power density (MPD) arrives to the biggest increase of36%from508±40mW/m2(the control) to637±51mW/m2(2.5%α-FeOOH added), and then to693±20mW/m2(5.0%α-FeOOH added). Whereas, with the excess increment of7.5%, the MPD inversely decreases to639±30mW/m2, probably due to the lower conductivity, diffusion and capacitance under the adsorption of biogenic iron(Ⅱ) on the anodic surface.
For AcM modified by nano magnetite (AcFeM), Tafel tests indicate that AcFeM is also kinetically more advantageous, and the MPD of AcFeM (809±5mW/m2,5.0%Fe3O4added) is22%higher than that of AcM (664±17mW/m2) by polarization tests. It is the first time to point out that the dynamic activity of Fe3O4plays a leading role in accelerating the electron transfer, and beneficial to boost the transient charge storage of the anode. Furthermore, the net storage capacity initially increases followed by a decrease with the maximum capacitance of574.6C/m2for AcFeM under20min of open circuit interval. The cyclic voltammetry curves explain that the capacitance of AcFeM can be from three aspects:pore structure of carbon, capacitor-like behavior of anodic biofilm and the redox couple of Fe3O4/Fe(Ⅱ) as a solid-state electron shuttle.
Power overshoot commonly makes the MFC performance evaluation inaccurate. Based on the capacitive characteristic of anodic biofilm, three types of carbon with different capacitance (UAC, plain activated carbon (PAC) and carbon black (CB1)) are rolled on SSM as anodes to investigate the relationship between overshoot and anodic capacitance. It is exciting that the overshoot is not observed for UAC-MFC from Cycle2to4, while the phenomenon is eliminated in PAC-MFC from Cycle3and in CB[-MFC from Cycle4. This is relevant with the Cmabiotic of the anode following the order of UAC (2.1F/cm2)> PAC (1.6F/cm2)> CB1(0.5F/cm2). It is inferred that the Cmabiotlc of anode stores charges and function as electron shuttle to overcome the phenomenon.
In order to prove the credibility of the result above, another carbon black (CB2) with enhanced capacitance is produced via chemical activation with potassium hydroxide and nitric acid, and simultaneously made into composite anode with5.0%addition. It has been found that oxygen-containing functional groups are introduced and both the hydrophilicity and Cmabiotic of the electrode are also improved. But, before and after Fe3O4addition, there is a slight increase in anodic capacitance. It indicates that the overshoot phenomenon disappears only when Cm is larger than1.1F/cm2, in spite of through chemical activation or capacitance compensation from bacterial colonization and Fe3O4. This further strengthens that insufficient capacity of anode leads to the power overshoot.
引文
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