孔性材料负载的NaAlH_4的储氢特性
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摘要
随着全球经济的高速发展,人类面临着化石燃料资源日渐匿乏和生态环境恶化的双重压力,因此开发清洁、可再生能源意义重大。氢由于清洁无污染,储量丰富,被认为是最有希望替代化石能源的能源载体。但氢气的高效储存与传输技术成为实用化瓶颈。为达到美国能源部(DOE)车载储氢技术的要求,必须开发出高体积能量密度与高质量能量密度的轻质储氢材料。本文在综述了储氢材料研究进展的基础上,以NaAlH4为主要研究对象,针对其存在的脱/加氢温度高、动力学性能差,循环寿命低等问题,利用有序介孔氧化硅和有序介孔碳等材料建立了空间约束的储氢体系,以期改善NaAlH4的储氢性能。通过X射线衍射(XRD)、傅立叶变换红外光谱(FTIR)、氮气吸附/脱附测试、扫描电子显微镜(SEM)、高分辨率透射电子显微镜(HRTEM)等测试手段观察了该体系下材料的形貌、结构和元素分布。利用热重(TG)-差示扫描量热(DSC)技术、压力-组分-温度(p-c-T)脱/加氢等温线以及循环测试等对材料的脱氢热力学特性、脱/加氢动力学性能、循环稳定性与循环寿命等进行了具体分析。
首先通过水热法制备了有序介孔氧化硅SBA-15,并利用湿法浸渍技术将NaAlH4填装入有序介孔氧化硅孔道中。研究发现,合成的有序介孔氧化硅表面含有大量硅羟基,易与NaAlH4发生反应,严重降低了NaAlH4的实际储氢容量。利用硅烷偶联剂等对有序介孔氧化硅表面进行修饰后,介孔氧化硅表面的硅羟基数量明显减少,有效减弱了表面硅羟基的影响。之后对表面修饰后的介孔氧化硅负载的NaAlH4体系的一系列测试结果表明,空间约束法制备的样品中,NaAlH4均匀地分布于介孔氧化硅的孔道,其分解产物等也被限制于氧化硅的孔道中。该体系的初始脱氢温度由纯NaAlH4的185℃降低到150℃,并且在较低温度下有更快的脱氢动力学性能。另外,在没有掺杂催化剂的条件下,这种空间约束体系也可在较低温度和氢压下(125-150℃/3.5-5.5 MPa)实现脱氢后的样品再氢化过程。由于在介孔氧化硅孔道的限制下,NaAlH4以及Na3AlH6、NaH、Al等脱氢产物在脱/加氢循环中颗粒尺寸始终保持在纳米量级,具有较大的比表面积和反应活性,避免了Al元素的偏析团聚,有利于再氢化过程的进行,改善了介孔氧化硅约束的NaAlH4体系的热力学和动力学性能。
之后利用有序介孔氧化硅SBA-15为模板、蔗糖为碳源制备了有序介孔碳CMK-3。通过熔融浸渍技术将NaAlH4填装进有序介孔碳的孔道,得到介孔碳约束下的NaAlH4储氢体系。实验数据显示,NaAlH4均匀分布于介孔碳的孔道中,表现出优异的储氢性能。体系的储氢脱氢温度也由纯NaAlH4的185℃降低到150℃,根据等温脱氢数据计算得到,体系的脱氢激活能由纯NaAlH4的120kJ/mol降低到46 kJ/mol。在180℃时,样品90 min的脱氢量达到5wt.%,且15次脱/加氢循环后的可逆储氢容量仍保有80%。由于介孔碳的空间限制作用,样品在脱/加氢循环中颗粒尺寸得到有效控制,避免了元素的偏析团聚,显著改善了脱/加氢循环稳定性。另外,通过与石墨混合的NaAlH4样品的比较实验可知,介孔碳不仅仅具有空间约束作用,而且自身对NaAlH4也显示出良好的催化效果,是尺寸约束与催化的协同作用,为今后改善NaAlH4等络合氢化物储氢性能提供了新的思路。
With the fast development of the global economy, the deficiency of fossil fuel re-sources and the deterioration of ecological environment present a tremendous challenge to long-term development of human society. The research and development of a clean and reproducible energy source are of great significance. Hydrogen is believed to be the most promising candidate as an energy carrier to replace the conventional fossil fuel because of its abundance, convenience, and non-polluting nature while the storage and transportation of hydrogen is one of stumbling block to its practical applications. In or-der to meet the requirements of US Department of Energy (DOE) for on-board fuel cell vehicle, it is essential to develop new technologies and materials with high volumetric and gravimetric energy densities. Based on the review of the progress in hydrogen stor-age materials, the NaAlH4 was selected as the major object owning to its high hydrogen contents. However, there still remains problems such as high de-/re-hydrogenation tem-perature, poor kinetics and short cycling life in the pristine NaAlH4 system. To over-come the obstacle mentioned above, a novel space-confined system where NaAlH4 is confined into the ordered mesoporous silica (OMS) or the ordered mesoporous carbon (OMC) was developed. The morphologies, microstructures and element distribution of the samples were systematically investigated by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Nitrogen adsorption/desorption iso-therms, Scanning electron microscopy (SEM), High-resolution transmission electron microscopy (HR-TEM). The de-hydrogenation thermodynamics, de-/re-hydrogenation kinetics, cycling stability and retention of materials were characterized by Thermogravi-metry (TG)-Differential scanning calorimetry (DSC) technique and Pressure-compo-sition-temperature (p-c-T) de-/re-hydrogenation isotherms and cycling test.
Firstly, the ordered mesoporous silica SBA-15 was synthesized through the hydro-thermal method. Then the NaAlH4 was loaded into the pore of the SBA-15 by the means of wet-impregnation technique. It was found that as-synthesized SBA-15 possesses a large numbers of reactive silanol groups at the surfaces which can react with the NaAlH4 to produce water and hydrogen, leading to the reduction of the actual hydrogen capac-ity of NaAlH4. After the surface modification of SBA-15 with suitable silane coupling agent, the silanol groups at the surface was decreased markedly, depressing the influences on the NaAlH4. The space confined NaAlH4 in the modified SBA-15 shows fine distri- bution of NaAlH4 particle and the de-hydrogenation product in pore of SBA-15,lower de-hydrogenation temperature of 150℃from the pristine NaAlH4 of 185℃and faster de-hydrogenation kinetics under lower temperature. Moreover, without any catalysts, the re-hydrogenation in a de-hydrogenated space-confined NaAlH4 system was achieved even under the temperatures of 125-150℃and the hydrogen pressures of 3.5-5.5 MPa. By the physical limitation of the pores of SBA-15, the NaAlH4 particles, as well as the re-sulting Na3AlH6, Al and NaH phases, were maintained within nanoscale, and have larger surface area and higher reactivity, preventing the phase segregation and agglomeration of Al element during de-/re-hydrogenation cycles. This is responsible for the improvement of thermodynamics and kinetics of the NaAlH4 space-confined in SBA-15.
Secondly, the ordered mesoporous carbon CMK-3 was synthesized using orderd mesoporous silica SBA-15 as the template and sucrose as the carbon source. Then the space-confined system was conducted by loading the NaAlH4 into the pore of CMK-3. The de-hydrogenation temperature of this system was decreased from 180℃to 150℃, and the activation energy of the system also reduced from 120 kJ/mol to 46 kJ/mol compared with pristine NaAlH4. At 180℃the space-confined NaAlH4/CMK-3 sam-ple evolved about 5.0 wt.% hydrogen in 90 min, and had the capacity retention of>80% after fifteen de-/re-hydrogenation cycles. These remarkable improvements on de-/re-hydrogenation cycling stability were mainly attributed to the nano-confinement by the CMK-3 which controled the particle size within nanoscale and prevented the phase seg-regation and agglomeration of elements. Furthermore, the catalysis of carbon itself was also the key factor for the improved performance by comparison with NaAlH4/graphite sample. Therefore, the synergistic effects of both nano-confinement and catalysis of porous materials provided a new avenue for improvement of the hydrogen storage prop-erties of complex hydrides.
首先通过水热法制备了有序介孔氧化硅SBA-15,并利用湿法浸渍技术将NaAlH4填装入有序介孔氧化硅孔道中。研究发现,合成的有序介孔氧化硅表面含有大量硅羟基,易与NaAlH4发生反应,严重降低了NaAlH4的实际储氢容量。利用硅烷偶联剂等对有序介孔氧化硅表面进行修饰后,介孔氧化硅表面的硅羟基数量明显减少,有效减弱了表面硅羟基的影响。之后对表面修饰后的介孔氧化硅负载的NaAlH4体系的一系列测试结果表明,空间约束法制备的样品中,NaAlH4均匀地分布于介孔氧化硅的孔道,其分解产物等也被限制于氧化硅的孔道中。该体系的初始脱氢温度由纯NaAlH4的185℃降低到150℃,并且在较低温度下有更快的脱氢动力学性能。另外,在没有掺杂催化剂的条件下,这种空间约束体系也可在较低温度和氢压下(125-150℃/3.5-5.5 MPa)实现脱氢后的样品再氢化过程。由于在介孔氧化硅孔道的限制下,NaAlH4以及Na3AlH6、NaH、Al等脱氢产物在脱/加氢循环中颗粒尺寸始终保持在纳米量级,具有较大的比表面积和反应活性,避免了Al元素的偏析团聚,有利于再氢化过程的进行,改善了介孔氧化硅约束的NaAlH4体系的热力学和动力学性能。
之后利用有序介孔氧化硅SBA-15为模板、蔗糖为碳源制备了有序介孔碳CMK-3。通过熔融浸渍技术将NaAlH4填装进有序介孔碳的孔道,得到介孔碳约束下的NaAlH4储氢体系。实验数据显示,NaAlH4均匀分布于介孔碳的孔道中,表现出优异的储氢性能。体系的储氢脱氢温度也由纯NaAlH4的185℃降低到150℃,根据等温脱氢数据计算得到,体系的脱氢激活能由纯NaAlH4的120kJ/mol降低到46 kJ/mol。在180℃时,样品90 min的脱氢量达到5wt.%,且15次脱/加氢循环后的可逆储氢容量仍保有80%。由于介孔碳的空间限制作用,样品在脱/加氢循环中颗粒尺寸得到有效控制,避免了元素的偏析团聚,显著改善了脱/加氢循环稳定性。另外,通过与石墨混合的NaAlH4样品的比较实验可知,介孔碳不仅仅具有空间约束作用,而且自身对NaAlH4也显示出良好的催化效果,是尺寸约束与催化的协同作用,为今后改善NaAlH4等络合氢化物储氢性能提供了新的思路。
With the fast development of the global economy, the deficiency of fossil fuel re-sources and the deterioration of ecological environment present a tremendous challenge to long-term development of human society. The research and development of a clean and reproducible energy source are of great significance. Hydrogen is believed to be the most promising candidate as an energy carrier to replace the conventional fossil fuel because of its abundance, convenience, and non-polluting nature while the storage and transportation of hydrogen is one of stumbling block to its practical applications. In or-der to meet the requirements of US Department of Energy (DOE) for on-board fuel cell vehicle, it is essential to develop new technologies and materials with high volumetric and gravimetric energy densities. Based on the review of the progress in hydrogen stor-age materials, the NaAlH4 was selected as the major object owning to its high hydrogen contents. However, there still remains problems such as high de-/re-hydrogenation tem-perature, poor kinetics and short cycling life in the pristine NaAlH4 system. To over-come the obstacle mentioned above, a novel space-confined system where NaAlH4 is confined into the ordered mesoporous silica (OMS) or the ordered mesoporous carbon (OMC) was developed. The morphologies, microstructures and element distribution of the samples were systematically investigated by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Nitrogen adsorption/desorption iso-therms, Scanning electron microscopy (SEM), High-resolution transmission electron microscopy (HR-TEM). The de-hydrogenation thermodynamics, de-/re-hydrogenation kinetics, cycling stability and retention of materials were characterized by Thermogravi-metry (TG)-Differential scanning calorimetry (DSC) technique and Pressure-compo-sition-temperature (p-c-T) de-/re-hydrogenation isotherms and cycling test.
Firstly, the ordered mesoporous silica SBA-15 was synthesized through the hydro-thermal method. Then the NaAlH4 was loaded into the pore of the SBA-15 by the means of wet-impregnation technique. It was found that as-synthesized SBA-15 possesses a large numbers of reactive silanol groups at the surfaces which can react with the NaAlH4 to produce water and hydrogen, leading to the reduction of the actual hydrogen capac-ity of NaAlH4. After the surface modification of SBA-15 with suitable silane coupling agent, the silanol groups at the surface was decreased markedly, depressing the influences on the NaAlH4. The space confined NaAlH4 in the modified SBA-15 shows fine distri- bution of NaAlH4 particle and the de-hydrogenation product in pore of SBA-15,lower de-hydrogenation temperature of 150℃from the pristine NaAlH4 of 185℃and faster de-hydrogenation kinetics under lower temperature. Moreover, without any catalysts, the re-hydrogenation in a de-hydrogenated space-confined NaAlH4 system was achieved even under the temperatures of 125-150℃and the hydrogen pressures of 3.5-5.5 MPa. By the physical limitation of the pores of SBA-15, the NaAlH4 particles, as well as the re-sulting Na3AlH6, Al and NaH phases, were maintained within nanoscale, and have larger surface area and higher reactivity, preventing the phase segregation and agglomeration of Al element during de-/re-hydrogenation cycles. This is responsible for the improvement of thermodynamics and kinetics of the NaAlH4 space-confined in SBA-15.
Secondly, the ordered mesoporous carbon CMK-3 was synthesized using orderd mesoporous silica SBA-15 as the template and sucrose as the carbon source. Then the space-confined system was conducted by loading the NaAlH4 into the pore of CMK-3. The de-hydrogenation temperature of this system was decreased from 180℃to 150℃, and the activation energy of the system also reduced from 120 kJ/mol to 46 kJ/mol compared with pristine NaAlH4. At 180℃the space-confined NaAlH4/CMK-3 sam-ple evolved about 5.0 wt.% hydrogen in 90 min, and had the capacity retention of>80% after fifteen de-/re-hydrogenation cycles. These remarkable improvements on de-/re-hydrogenation cycling stability were mainly attributed to the nano-confinement by the CMK-3 which controled the particle size within nanoscale and prevented the phase seg-regation and agglomeration of elements. Furthermore, the catalysis of carbon itself was also the key factor for the improved performance by comparison with NaAlH4/graphite sample. Therefore, the synergistic effects of both nano-confinement and catalysis of porous materials provided a new avenue for improvement of the hydrogen storage prop-erties of complex hydrides.
引文
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