全钒液流储能电池非氟隔膜的制备与性能研究
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摘要
化石能源的枯竭和环境恶化迫使人们去开发太阳能、风能等可再生能源。然而,这些再生能源受气候变化而具有不稳定和不连续的特点,因而,储能技术备受国内外研究者的广泛关注。与其它储能技术相比,全钒液流氧化还原电池(VRB)由于具有绿色安全环保、快速响应、可深度充放电、容量可设计性好、能量效率高、成本低、不受地域限制等优点被认为是最具有应用前景的储能技术之一。作为VRB核心组件的隔膜的性能和价格是制约电池效能和大规模推广应用的关键因素之一。本文围绕高离子传导率、高选择性、长寿命和低价格的隔膜的制备和性能方面展开研究,主要内容如下：
利用交流阻抗测试了几种商用膜的面电阻,结果发现,Nafion的面电阻最小,国产膜中,异相膜的面电阻值明显大于均相膜面电阻值,阳离子交换膜的面电阻值小于阴离子交换膜。VO2+渗透率和水迁移测试表明阴离子膜由于Donnan效应更利于阻钒离子,相应地,水迁移也小。电池测试表明,Nafion膜的充放电性能好,容量大；国产膜中,小电流密度下,阴离子膜具有更好的充放电性能和更高的容量；大电流密度下,阳离子交换膜体现出更好的充放电性能。化学稳定性测试表明,聚苯醚类阴膜DF-a化学稳定性较其它国产膜高。综合评价,Nafion膜和DF-a膜更适用于钒电池中。
采用水热法以Ti(SO4)2和尿素为前体对Nafion膜改性,制备了Nafion/TiO2杂化膜。与Nafion膜相比,杂化膜的含水率降低,而离子交换容量(IEC)、厚度、面电阻基本不变。SEM-EDS和XRD表明杂化膜中Ti02粒子分布均匀,TG测试发现水热改性没有显著降低Nafion膜的热稳定性。Nafion/TiO2膜中的钒离子V02+渗透率由改性前的2.26×10-5cm2·min-1下降到6.72×10-6cm2·min-1。Nafion/TiO2膜组装的单电池具有更小的自放电率(37h vs.14h),更高库仑效率(88.8%vs.86.3%),和更高的能量效率(71.5%vs.69.6%)。
利用后磺化法对PPES聚合物进行了磺化,以特性粘度和磺化度为评价指标,发现在40℃下磺化4-6h得到的SPPES较好地满足离子交换膜的要求,磺化后的聚合物特性粘度变大,能溶于大多数非质极性溶剂。IR, TG和DSC证实了磺化产物的主链上成功引入了-SO3H,导致了聚合物的热性能降低(Td=300℃)和玻璃化温度提高。与Nafion膜相比,SPPES膜具有更高的IEC；而具有较低的含水率、电解质的吸附率和质子传导率；SPPES膜具有显著低钒离子渗透率(1.24×10-7vs.22.63×10-7cm2·min-1); SPPES膜组装的钒电池具有更高的库仑效率和能量效率和良好的稳定性。
利用水热法以NaWO3作为前体对SPPEK膜改性制备SPPEK/WO3杂化膜。SEM-EDS表明W03微粒均匀分布于杂化膜内。与SPPEK膜相比,杂化膜的钒离子的渗透率基本不变。与Nafion膜相比,杂化膜的选择性更高(5.81×104vs.0.22×104min·S·cm-3)。电池测试表明,SPPEK/WO3组成VRB的CE和EE(98.07%和78.60%)高于Nafion膜(92.81%和76.19%)。电池循环测试和化学稳定性测试表明SPPEK/WO3杂化膜具有较好的化学稳定性。
利用共混法制备了SPPEK/TPA(磷钨酸)复合膜。SEM和XRD表明复合膜中的TPA与SPPEK具有良好的相容性,膜呈均相状态。基本性能测试表明复合膜中TPA含量增加时,复合膜离子交换容量降低,含水率增大,溶胀率降低,拉伸强度变化不大。钒离子对膜的渗透实验表明,TPA含量增大时,离子传输率变大,选择性降低,而阻钒性仍高于Nafion膜二个数量级；钒离子从五价依次降低到三价,钒离子渗透率依次增大,Nafion膜的增幅最大。静态电池和动态电池测试表明,与Nafion膜相比,SPPEK-TPA-17复合膜具有更低的自放电率和容量衰减,更高的库仑效率和能量效率。充放电循环和化学稳定性测试,表明SPPEK-TPA-17复合膜具有较好的稳定性。
With fossil supplies increasingly exhausted and the environment highly deteriorated by their consumption, renewable energy sources such as solar energy and wind energy have been developed. However, these energies have instability and discontinuous interrupt due to the climate change. So the energy conservation technologies have drawn great attention. Compared to the other energy conservation technologies, all vanadium redox flow battery (VRB) has been accepted as a very promising energy conversion device due to its green safety, fast response, deep charge-discharge ability, easily designed capacity, high energy efficiency, low cost, and no limit in geographical position. As a key component in VRB, the separator is vital to restrain the VRB's performance and its large-scale application. In this paper, the research work was focused on the preparation and properties of the membranes with high ionic conductivity and selectivity, long life, and low price. The main points in this research can be summarized as follows.
The area resistance (AR) for several commercial ionic exchange membranes (IEM) was determined by electrochemical impedance spectroscopy (EIS). The results showed Nafion membrane had the least AR value in all samples, in the domestic membranes AR values of heterogeneous membranes were markedly higher than homogeneous ones, and AR values of cationic exchange membranes (CEM) were lower than that of anionic exchange membranes (AEM). The AEM had a significant reduction in crossover of vanadium ions compared with the CEM due to the Donnan effect of AEM. Correspondingly, the AEM had a lower water transfer than the CEM. Cell test indicated that Nafion exhibited a superior charge-discharge performance and a higher capacity. For the domestic membranes, the VRB with the AEM showed a better charge-discharge performance and higher capacity than that of CEM at the lower current density, and at higher current density the cell with CEM exhibited a superior charge-discharge performance to that of AEM. The chemical stability tests showed the Poly(aryl ether)s AEM (DF-a) possessed more chemical stability and was more suitable for VRB than the other domestic IEM.
A Nafion/TiO2hybrid membrane was fabricated by a hydrothermal method. The primary properties of the hybrid membrane were measured and compared with the Nafion membrane. The results of Scanning Electron Microscope (SEM), Energy Dispersive X-Ray Spectroscopy (EDS) and X-Ray Diffraction (XRD) of the hybrid membrane revealed that the TiO2phase was formed in the bulk of the prepared membrane. Thermo Gravimetric Analysis (TG) showed that hydrothermal modification had almost no effect on the thermal property of the hybrid membrane. The Nafion/TiO2hybrid membrane had a dramatic reduction in crossover of vanadium ions compared with the Nafion membrane (6.72×10-6vs.2.26×10-5cm2·min-1). The columbic efficiency (CE) and energy efficiency EE of the VRB with the hybrid membrane were88.8%and71.5%at60mA·cm-2, respectively, while those of the VRB with Nafion membrane were86.3%and69.7%at the same current density.
Sulfonated poly(phthalazinone ether sulfone)(SPPES) suitable for ionic exchange membrane fabrication was prepared by sulfonating PPES with fuming sulfuric acid at40℃for4-6h. By testing the sulfonation degree (SD), intrinsic viscosity and solubility of SPPES, the results showed that sulfonated polymers had higher intrinsic viscosities and excellent solubility in most polar solvents. IR analysis revealed that the-SO3H group was successfully attached to SPPES backbone. DSC and TG results showed that SPPES exhibited higher Tg than that of PPES, and Td at the first weight loss of SPPES was about300℃. The SPPES membrane (SP-02) showed a dramatic reduction in crossover of vanadium ions across the membrane compared with that of the Nafion membrane (1.24×10-7vs.22.63×10-7cm2·min-1). Cell tests identified that VRB with the SPPES membrane exhibited a lower self-discharge rate, higher CE (92.82%) and EE (67.58%) compared with the Nafion system. Furthermore, cycling tests indicated the single cell with SPPES membrane exhibited a stable performance during100cycles.
A SPPEK/WO3membrane was fabricated by a hydrothermal method to improve its performance in VRFB. SEM of the composite membrane revealed that WO3phase was well formed in the bulk of the SPPEK membrane. Compared with Nafion membrane, the hybrid membrane showed a dramatic reduction in crossover of vanadium ions across the membrane and a higher selectivity (5.81×104vs.0.22x104minScm-3). Cell tests identified that the VRB with the SPPEK/WO3hybrid membrane presented a higher coulombic efficiency (98.07%vs.92.81%) and energy efficiency (78.60%vs.76.19%) compared with the Nafion system. Cycling and chemical stability tests indicated that the hybrid membrane had enough stability to be applied in VRB system.
A SPPEK/TPA composite membrane was prepared by blending SPPEK and tungstophosphoric acid (TPA). SEM and XRD showed that TPA had excellent compatibility with SPPEK in the homogeneous membrane. With TPA content increasing, the composite membrane exhibited lower IEC, greater water uptake, lower swelling ratio, unchangeable tensile strength, higher ionic conductivity, lower selectivity, and lower permeability of vanadium ions which was still superior to Nafion membrane. In terms of vanadium ion valence, from quintavalent to trivalence, the permeability of the vanadium ion for all membrane samples increased correspondingly, especially for Nafion membrane. The static and flow cell tests showed SPPEK-TPA-17membrane exhibited a lower self-discharge rate, and higher CE and EE. Cycling and chemical stability tests indicated that the SPPEK/TPA composite membrane had enough stability to be applied in VRB system.
利用交流阻抗测试了几种商用膜的面电阻,结果发现,Nafion的面电阻最小,国产膜中,异相膜的面电阻值明显大于均相膜面电阻值,阳离子交换膜的面电阻值小于阴离子交换膜。VO2+渗透率和水迁移测试表明阴离子膜由于Donnan效应更利于阻钒离子,相应地,水迁移也小。电池测试表明,Nafion膜的充放电性能好,容量大；国产膜中,小电流密度下,阴离子膜具有更好的充放电性能和更高的容量；大电流密度下,阳离子交换膜体现出更好的充放电性能。化学稳定性测试表明,聚苯醚类阴膜DF-a化学稳定性较其它国产膜高。综合评价,Nafion膜和DF-a膜更适用于钒电池中。
采用水热法以Ti(SO4)2和尿素为前体对Nafion膜改性,制备了Nafion/TiO2杂化膜。与Nafion膜相比,杂化膜的含水率降低,而离子交换容量(IEC)、厚度、面电阻基本不变。SEM-EDS和XRD表明杂化膜中Ti02粒子分布均匀,TG测试发现水热改性没有显著降低Nafion膜的热稳定性。Nafion/TiO2膜中的钒离子V02+渗透率由改性前的2.26×10-5cm2·min-1下降到6.72×10-6cm2·min-1。Nafion/TiO2膜组装的单电池具有更小的自放电率(37h vs.14h),更高库仑效率(88.8%vs.86.3%),和更高的能量效率(71.5%vs.69.6%)。
利用后磺化法对PPES聚合物进行了磺化,以特性粘度和磺化度为评价指标,发现在40℃下磺化4-6h得到的SPPES较好地满足离子交换膜的要求,磺化后的聚合物特性粘度变大,能溶于大多数非质极性溶剂。IR, TG和DSC证实了磺化产物的主链上成功引入了-SO3H,导致了聚合物的热性能降低(Td=300℃)和玻璃化温度提高。与Nafion膜相比,SPPES膜具有更高的IEC；而具有较低的含水率、电解质的吸附率和质子传导率；SPPES膜具有显著低钒离子渗透率(1.24×10-7vs.22.63×10-7cm2·min-1); SPPES膜组装的钒电池具有更高的库仑效率和能量效率和良好的稳定性。
利用水热法以NaWO3作为前体对SPPEK膜改性制备SPPEK/WO3杂化膜。SEM-EDS表明W03微粒均匀分布于杂化膜内。与SPPEK膜相比,杂化膜的钒离子的渗透率基本不变。与Nafion膜相比,杂化膜的选择性更高(5.81×104vs.0.22×104min·S·cm-3)。电池测试表明,SPPEK/WO3组成VRB的CE和EE(98.07%和78.60%)高于Nafion膜(92.81%和76.19%)。电池循环测试和化学稳定性测试表明SPPEK/WO3杂化膜具有较好的化学稳定性。
利用共混法制备了SPPEK/TPA(磷钨酸)复合膜。SEM和XRD表明复合膜中的TPA与SPPEK具有良好的相容性,膜呈均相状态。基本性能测试表明复合膜中TPA含量增加时,复合膜离子交换容量降低,含水率增大,溶胀率降低,拉伸强度变化不大。钒离子对膜的渗透实验表明,TPA含量增大时,离子传输率变大,选择性降低,而阻钒性仍高于Nafion膜二个数量级；钒离子从五价依次降低到三价,钒离子渗透率依次增大,Nafion膜的增幅最大。静态电池和动态电池测试表明,与Nafion膜相比,SPPEK-TPA-17复合膜具有更低的自放电率和容量衰减,更高的库仑效率和能量效率。充放电循环和化学稳定性测试,表明SPPEK-TPA-17复合膜具有较好的稳定性。
With fossil supplies increasingly exhausted and the environment highly deteriorated by their consumption, renewable energy sources such as solar energy and wind energy have been developed. However, these energies have instability and discontinuous interrupt due to the climate change. So the energy conservation technologies have drawn great attention. Compared to the other energy conservation technologies, all vanadium redox flow battery (VRB) has been accepted as a very promising energy conversion device due to its green safety, fast response, deep charge-discharge ability, easily designed capacity, high energy efficiency, low cost, and no limit in geographical position. As a key component in VRB, the separator is vital to restrain the VRB's performance and its large-scale application. In this paper, the research work was focused on the preparation and properties of the membranes with high ionic conductivity and selectivity, long life, and low price. The main points in this research can be summarized as follows.
The area resistance (AR) for several commercial ionic exchange membranes (IEM) was determined by electrochemical impedance spectroscopy (EIS). The results showed Nafion membrane had the least AR value in all samples, in the domestic membranes AR values of heterogeneous membranes were markedly higher than homogeneous ones, and AR values of cationic exchange membranes (CEM) were lower than that of anionic exchange membranes (AEM). The AEM had a significant reduction in crossover of vanadium ions compared with the CEM due to the Donnan effect of AEM. Correspondingly, the AEM had a lower water transfer than the CEM. Cell test indicated that Nafion exhibited a superior charge-discharge performance and a higher capacity. For the domestic membranes, the VRB with the AEM showed a better charge-discharge performance and higher capacity than that of CEM at the lower current density, and at higher current density the cell with CEM exhibited a superior charge-discharge performance to that of AEM. The chemical stability tests showed the Poly(aryl ether)s AEM (DF-a) possessed more chemical stability and was more suitable for VRB than the other domestic IEM.
A Nafion/TiO2hybrid membrane was fabricated by a hydrothermal method. The primary properties of the hybrid membrane were measured and compared with the Nafion membrane. The results of Scanning Electron Microscope (SEM), Energy Dispersive X-Ray Spectroscopy (EDS) and X-Ray Diffraction (XRD) of the hybrid membrane revealed that the TiO2phase was formed in the bulk of the prepared membrane. Thermo Gravimetric Analysis (TG) showed that hydrothermal modification had almost no effect on the thermal property of the hybrid membrane. The Nafion/TiO2hybrid membrane had a dramatic reduction in crossover of vanadium ions compared with the Nafion membrane (6.72×10-6vs.2.26×10-5cm2·min-1). The columbic efficiency (CE) and energy efficiency EE of the VRB with the hybrid membrane were88.8%and71.5%at60mA·cm-2, respectively, while those of the VRB with Nafion membrane were86.3%and69.7%at the same current density.
Sulfonated poly(phthalazinone ether sulfone)(SPPES) suitable for ionic exchange membrane fabrication was prepared by sulfonating PPES with fuming sulfuric acid at40℃for4-6h. By testing the sulfonation degree (SD), intrinsic viscosity and solubility of SPPES, the results showed that sulfonated polymers had higher intrinsic viscosities and excellent solubility in most polar solvents. IR analysis revealed that the-SO3H group was successfully attached to SPPES backbone. DSC and TG results showed that SPPES exhibited higher Tg than that of PPES, and Td at the first weight loss of SPPES was about300℃. The SPPES membrane (SP-02) showed a dramatic reduction in crossover of vanadium ions across the membrane compared with that of the Nafion membrane (1.24×10-7vs.22.63×10-7cm2·min-1). Cell tests identified that VRB with the SPPES membrane exhibited a lower self-discharge rate, higher CE (92.82%) and EE (67.58%) compared with the Nafion system. Furthermore, cycling tests indicated the single cell with SPPES membrane exhibited a stable performance during100cycles.
A SPPEK/WO3membrane was fabricated by a hydrothermal method to improve its performance in VRFB. SEM of the composite membrane revealed that WO3phase was well formed in the bulk of the SPPEK membrane. Compared with Nafion membrane, the hybrid membrane showed a dramatic reduction in crossover of vanadium ions across the membrane and a higher selectivity (5.81×104vs.0.22x104minScm-3). Cell tests identified that the VRB with the SPPEK/WO3hybrid membrane presented a higher coulombic efficiency (98.07%vs.92.81%) and energy efficiency (78.60%vs.76.19%) compared with the Nafion system. Cycling and chemical stability tests indicated that the hybrid membrane had enough stability to be applied in VRB system.
A SPPEK/TPA composite membrane was prepared by blending SPPEK and tungstophosphoric acid (TPA). SEM and XRD showed that TPA had excellent compatibility with SPPEK in the homogeneous membrane. With TPA content increasing, the composite membrane exhibited lower IEC, greater water uptake, lower swelling ratio, unchangeable tensile strength, higher ionic conductivity, lower selectivity, and lower permeability of vanadium ions which was still superior to Nafion membrane. In terms of vanadium ion valence, from quintavalent to trivalence, the permeability of the vanadium ion for all membrane samples increased correspondingly, especially for Nafion membrane. The static and flow cell tests showed SPPEK-TPA-17membrane exhibited a lower self-discharge rate, and higher CE and EE. Cycling and chemical stability tests indicated that the SPPEK/TPA composite membrane had enough stability to be applied in VRB system.
引文
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