铝氢化镁基储氢材料的合成、吸放氢性能及其机理
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摘要
氢能是解决化石能源枯竭与环境污染两大问题的理想选择,但安全和高效的储氢技术是目前氢能规模化应用的主要瓶颈。Mg(AlH4)2由于其较高的储氢容量,引起了人们的广泛关注,但其较高的吸放氢温度和较差的储氢可逆性,难以满足实用化的要求。加之Mg(AlH4)2的制备困难,目前尚未有商业化的试剂供应,严重制约了Mg(AlH4)2基高容量储氢材料的发展。针对这些问题,本文系统研究了Mg(AlH4)2的可控制备以及球磨处理、催化剂掺杂、反应物复合和纳米化对其结构和吸放氢性能的影响,并揭示了相关的作用机理。
首先,发展了一种可控制备高纯度Mg(AlH4)2亚微米棒的方法,并系统研究了所制备样品的吸放氢热力学和动力学性能。所得Mg(AlH4)2亚微米棒的直径为0.5微米,纯度为96.1%。所得Mg(AlH4)2在加热时以三步放氢共放出9.0wt%的氢气。第一步放氢生成MgH2和Al,第二步放氢生成Al(Mg)固溶体和MgH2,第三步放氢生成Al3Mg2和Al(Mg)固溶体。由于第一步放氢为微放热反应,其无法在高氢压下实现可逆,仅后两步放氢可逆。动力学研究发现,所得Mg(AlH4)2的第一步放氢为扩散控制,具有较高的表观活化能,为123.0kJ mol-1,这是其起始放氢温度偏高的主要原因。
其次,系统研究了球磨处理对Mg(AlH4)2储氢性能影响及其机理。结果发现,高能球磨能够明显降低Mg(AlH4)2的放氢温度。经球磨12小时后,Mg(AlH4)2的放氢温度降低了40℃。高能球磨从宏观到微观改变了Mg(AlH4)2的颗粒尺寸、晶粒尺寸、微应力和晶格畸变,随球磨时间的延长,减小了材料的颗粒尺寸和晶粒尺寸,增大了材料的微应力与晶格畸变。颗粒尺寸和晶粒尺寸的减小会缩短Mg(AlH4)2放氢反应中物质的扩散距离,微应力和晶格畸变的增加会增强Mg(AlH4)2放氢反应中物质的扩散性,它们的协同作用改善了Mg(AlH4)2放氢的动力学性能。此外,微应力和晶格畸变的增加还会升高Mg(AlH4)2的Gibbs自由能,从而改变了Mg(AlH4)2放氢的热力学性能。
第三,研究了氟化钛掺杂对Mg(AlH4)2吸放氢性能的影响及其机理。研究发现,TiF3和TiF4掺杂都能够显著降低Mg(AlH4)2的放氢温度,其中TiF4的催化效果优于TiF3。2.5mol%的TiF4掺杂Mg(AlH4)2在40℃就开始放氢,82℃等温放氢时在100分钟内就可以放出4.0wt%的氢气,其原因是TiF4与Mg(AlH4)2在球磨过程中会发生反应,原位生成了催化活性物质Ti,并增加了Mg(AlH4)2的缺陷,从而改变了Mg(AlH4)2第一步放氢产物的形核长大模式,因此降低了Mg(AlH4)2第一步放氢的动力学势垒。但TiF4掺杂并不能改善Mg(AlH4)2的可逆性,2.5mol%的TiF4掺杂样品仍然只具有部分可逆性。
第四,研究了Mg(AlH4)2/LiBH4复合体系的吸放氢性能及其机理。对不同摩尔比的Mg(AlH4)2-xLiBH4样品(x＝2、4、6)的研究表明,随LiBH4含量的增力口,LiBH4样品第二步MgH2和Al的放氢温度降低,第三步Al3Mg2、 Al(Mg)和LiBH4的放氢温度升高。其中,MgH2和Al放氢温度降低的原因是：LiBH4对MgH2和AL的放氢有催化作用,而其含量的增加导致MgH2和Al的放氢动力学势垒降低；而Al3Mg2.Al(Mg)与LiBH4放氢温度的升高的原因是：LiBH4的增加改变了其反应路径,升高了反应焓变。此外,考察了Mg(AlH4)2制备过程中副产物NaCl或LiCl对Mg(AlH4)2-6LiBH4体系的影响。结果发现,NaCl会与LiBH4反应生成NaBH4和LiCl,改变了体系的化学组成；LiCl中的Cl-离子促进了Mg(AlH4)2-6LiBH4体系第二步MgH2与Al的放氢,同时LiCl阻碍了Mg(AlH4)2-6LiBH4体系第三步Al3Mg2、Al(Mg)和LiBH4的接触,从而抑制了其放氢。
最后,发展了一种机械力驱动物理气相沉积(MFPVD)制备Mg(AlH4)2纳米棒的方法,揭示了纳米棒形成机理,并系统研究了相关材料的吸放氢性能。研究指出,高能球磨产生的机械力将具有一维链状结构的[Mg(AlH4)2(Et2O)]n配位聚合物气化后,其会在基底上一维自组装形成[Mg(AlH4)2(Et2O)]n纳米棒,然后热处理除去配体Et20,得到了Mg(AlH4)2纳米棒。所得Mg(AlH4)2纳米棒的直径为20-40纳米,具有较Mg(AlH4)2微米棒更优的储氢性能,尤其是所得Mg(AlH4)2纳米棒在吸放氢过程中都能保持纳米棒状形貌,表现出良好的循环稳定性。此外,通过相似的过程也成功制备了宽度为10-40纳米的LiBH4纳米带,说明了MFPVD方法具有一定的普适性,可以推广至其他具有特定形貌有机配位聚合物的配位氢化物。
Hydrogen energy is an ideal choice that can solve the problems of the depletion of fossil fuels and the contamination of environment. However, the technique of safe and efficient storage of hydrogen is the key barrier that prevents hydrogen energy from widespread utilization. Mg(AlH4)2attracts a lot of attention due to its relatively high hydrogen capacity, but the relatively high hydrogenation/dehydrogenation temperatures and poor reversibility cannot fulfill the requirements of practical application. Furthermore, the synthesis of Mg(AlH4)2is so difficult that Mg(AlH4)2is not commercially available until now, which severely hinders the development of Mg(AlH4)2-based hydrogen storage materials. In this paper, aiming at these problems, the controllable synthesis, high-energy ball milling, catalyst-doping, composite and nanosizing of Mg(AlH4)2were systematically investigated and the corresponding mechanisms were also revealed.
First, a controllable synthesis method was developed to prepare high-purity Mg(AlH4)2submicron rods, and the hydrogen storage thermodynamics and kinetics of the as-prepared Mg(AlH4)2submicron rods were also systematically investigated. The diameter of the as-prepared Mg(AlH4)2submicron rods are0.5μm, and its purity is96.1%. The as-prepared Mg(AlH4)2release9.0wt%of hydrogen through a three-step reaction. MgH2and Al are formed after the first dehydrogenation step, and then Al(Mg) solid solution and MgH2are formed after the second dehydrogenation step, and finally Al3Mg2and Al(Mg) solid solution are formed after the third dehydrogenation step. The first dehydrogenation step is not reversible due to its exothermic nature, and the other two steps are reversible. Kinetic investigations indicate that the first dehydrogenation step of the as-prepared Mg(AlH4)2is a diffusion-controlled reaction with an relatively high apparent activation energy of123.0kJ mol-1, which is mainly responsible for its high on-set dehydrogenation temperature.
Second, the effect of high-energy ball milling on the hydrogen storage properties of Mg(AlH4)2and its mechanism were systematically investigated. After milling for12h, the hydrogen desorption temperatures of Mg(AlH4)2is lowered by40℃. From macro-to micro-scale, high-energy ball milling changes the particle size, grain size, microstrain and lattice distortion of Mg(AlH4)2, specifically decreases the particle size and grain size and increases the microstrain and lattice distortion with prolonging the milling time. The decreases in particle size and grain size can shorten the diffusion distance of the species involved in the dehydrogenation reaction, and the increases in the microstrain and lattice distortion can enhance the diffusivity of the species involved in the dehydrogenation reaction, therefore synergically improve the dehydrogenation kinetics of Mg(AlH4)2.Moreover, the increases in the microstrain and lattice distortion can also raise the Gibbs free energy of Mg(AlH4)2, consequently changes the dehydrogenation thermodynamics of Mg(AlH4)2.
Third, the effect of titanium fluoride on the hydrogen storage properties and its mechanism were investigated. It was found that doping with TiF3and TiF4can significantly reduce the dehydrogenation temperatures of Mg(AlH4)2, and the catalytic activity of TiF4is superior to that of TiF3.2.5mol%TiF4-doped Mg(AlH4)2starts to desorb hydrogen at40℃, and can release4.0wt%of hydrogen at82℃in100min. These is because TiF4can react with Mg(AlH4)2during milling, to in situ form the active catalyst Ti and increase defects, which change the nucleation and growth mode of the first-step dehydrogenation products of Mg(AlH4)2, and consequently lower the activation barrier of the first dehydrogenation step of Mg(AlH4)2.However, the reversibility of Mg(AlH4)2is not improved by doping with TiF4, as2.5mol%TiF4-doped Mg(AlH4)2is still partial reversible.
Fourth, the hydrogen storage properties of Mg(AlH4)2/LiBH4composites and its mechanism were investigated. The research on the Mg(AlH4)2-xLiBH4composites with different molar ratio (x=2,4,6) revealed that with increasing the content of LiBH4, the dehydrogenation temperature of the second step of the Mg(AlH4)2-xLiBH4composite (the reaction of MgH2and Al) is lowered, and the dehydrogenation temperature of the third step (the reaction of Al3Mg2, Al(Mg) and LiBH4) is raised. The reason for the decrease in the reaction temperature of MgH2and Al is:LiBH4is a catalyst for the reaction of MgH2and Al, and the increased content of LiBH4lowers its kinetic barrier; the reason for the increase in the reaction temperature of Al3Mg2, Al(Mg) and LiBH4is:the increased content of LiBH4causes the change of the reaction path and raises the enthalpy change. Furthermore, the effect of byproduct NaCl or LiCl from the synthesis of Mg(AlH4)2on Mg(AlH4)2-6LiBH4composite was then investigated. It is found that NaCl can react with LiBH4to form NaBH4and LiCl, changing the chemical composition of the composite; Cl" ion in LiCl promotes the second dehydrogenation step of Mg(AlH4)2-6LiBH4composite (the reaction of and Al), and LiCl restrains the third dehydrogenation step of Mg(AlH4)2-6LiBH4composite by hindering the contact between Al3Mg2, Al(Mg) and LiBH4
Finally, a mechanical-force-driven physical vapour deposition (MFPVD) method was developed to prepare Mg(AlH4)2nanorods; the formation mechanism was discussed; the hydrogen storage properties were also investigated systematically. It is found that the intense physical force from high-energy ball milling can vaporize the coordination polymer [Mg(AlH4)2(Et2O)]n which possesses a one-dimensional chain-like structure. Then the vaporized material can deposit onto the substrate and self-assemble one-dimensionally to form [Mg(AlH4)2(Et2O)]n nanorods. During successive heat treatment, the Et2O molecules were removed to form Mg(AlH4)2nanorods. The diameter of the as-prepared Mg(AlH4)2nanorods is20-40nm. The as-prepared Mg(AlH4)2nanorods exhibit superior hydrogen storage properties to the Mg(AlH4)2microrods, especially, the as-prepared Mg(AlH4)2nanorods can maintain their nanorod-like morphology during dehydrogenation and hydrogenation processes, consequently show excellent cycling stability. Moreover, LiBH4nanobelts with width of10-40nm were also successfully prepared by a similar process, indicating that the MFPVD method is general enough that can be extended to other complex hydrides which possess organic coordination polymers with unique morphology.
首先,发展了一种可控制备高纯度Mg(AlH4)2亚微米棒的方法,并系统研究了所制备样品的吸放氢热力学和动力学性能。所得Mg(AlH4)2亚微米棒的直径为0.5微米,纯度为96.1%。所得Mg(AlH4)2在加热时以三步放氢共放出9.0wt%的氢气。第一步放氢生成MgH2和Al,第二步放氢生成Al(Mg)固溶体和MgH2,第三步放氢生成Al3Mg2和Al(Mg)固溶体。由于第一步放氢为微放热反应,其无法在高氢压下实现可逆,仅后两步放氢可逆。动力学研究发现,所得Mg(AlH4)2的第一步放氢为扩散控制,具有较高的表观活化能,为123.0kJ mol-1,这是其起始放氢温度偏高的主要原因。
其次,系统研究了球磨处理对Mg(AlH4)2储氢性能影响及其机理。结果发现,高能球磨能够明显降低Mg(AlH4)2的放氢温度。经球磨12小时后,Mg(AlH4)2的放氢温度降低了40℃。高能球磨从宏观到微观改变了Mg(AlH4)2的颗粒尺寸、晶粒尺寸、微应力和晶格畸变,随球磨时间的延长,减小了材料的颗粒尺寸和晶粒尺寸,增大了材料的微应力与晶格畸变。颗粒尺寸和晶粒尺寸的减小会缩短Mg(AlH4)2放氢反应中物质的扩散距离,微应力和晶格畸变的增加会增强Mg(AlH4)2放氢反应中物质的扩散性,它们的协同作用改善了Mg(AlH4)2放氢的动力学性能。此外,微应力和晶格畸变的增加还会升高Mg(AlH4)2的Gibbs自由能,从而改变了Mg(AlH4)2放氢的热力学性能。
第三,研究了氟化钛掺杂对Mg(AlH4)2吸放氢性能的影响及其机理。研究发现,TiF3和TiF4掺杂都能够显著降低Mg(AlH4)2的放氢温度,其中TiF4的催化效果优于TiF3。2.5mol%的TiF4掺杂Mg(AlH4)2在40℃就开始放氢,82℃等温放氢时在100分钟内就可以放出4.0wt%的氢气,其原因是TiF4与Mg(AlH4)2在球磨过程中会发生反应,原位生成了催化活性物质Ti,并增加了Mg(AlH4)2的缺陷,从而改变了Mg(AlH4)2第一步放氢产物的形核长大模式,因此降低了Mg(AlH4)2第一步放氢的动力学势垒。但TiF4掺杂并不能改善Mg(AlH4)2的可逆性,2.5mol%的TiF4掺杂样品仍然只具有部分可逆性。
第四,研究了Mg(AlH4)2/LiBH4复合体系的吸放氢性能及其机理。对不同摩尔比的Mg(AlH4)2-xLiBH4样品(x＝2、4、6)的研究表明,随LiBH4含量的增力口,LiBH4样品第二步MgH2和Al的放氢温度降低,第三步Al3Mg2、 Al(Mg)和LiBH4的放氢温度升高。其中,MgH2和Al放氢温度降低的原因是：LiBH4对MgH2和AL的放氢有催化作用,而其含量的增加导致MgH2和Al的放氢动力学势垒降低；而Al3Mg2.Al(Mg)与LiBH4放氢温度的升高的原因是：LiBH4的增加改变了其反应路径,升高了反应焓变。此外,考察了Mg(AlH4)2制备过程中副产物NaCl或LiCl对Mg(AlH4)2-6LiBH4体系的影响。结果发现,NaCl会与LiBH4反应生成NaBH4和LiCl,改变了体系的化学组成；LiCl中的Cl-离子促进了Mg(AlH4)2-6LiBH4体系第二步MgH2与Al的放氢,同时LiCl阻碍了Mg(AlH4)2-6LiBH4体系第三步Al3Mg2、Al(Mg)和LiBH4的接触,从而抑制了其放氢。
最后,发展了一种机械力驱动物理气相沉积(MFPVD)制备Mg(AlH4)2纳米棒的方法,揭示了纳米棒形成机理,并系统研究了相关材料的吸放氢性能。研究指出,高能球磨产生的机械力将具有一维链状结构的[Mg(AlH4)2(Et2O)]n配位聚合物气化后,其会在基底上一维自组装形成[Mg(AlH4)2(Et2O)]n纳米棒,然后热处理除去配体Et20,得到了Mg(AlH4)2纳米棒。所得Mg(AlH4)2纳米棒的直径为20-40纳米,具有较Mg(AlH4)2微米棒更优的储氢性能,尤其是所得Mg(AlH4)2纳米棒在吸放氢过程中都能保持纳米棒状形貌,表现出良好的循环稳定性。此外,通过相似的过程也成功制备了宽度为10-40纳米的LiBH4纳米带,说明了MFPVD方法具有一定的普适性,可以推广至其他具有特定形貌有机配位聚合物的配位氢化物。
Hydrogen energy is an ideal choice that can solve the problems of the depletion of fossil fuels and the contamination of environment. However, the technique of safe and efficient storage of hydrogen is the key barrier that prevents hydrogen energy from widespread utilization. Mg(AlH4)2attracts a lot of attention due to its relatively high hydrogen capacity, but the relatively high hydrogenation/dehydrogenation temperatures and poor reversibility cannot fulfill the requirements of practical application. Furthermore, the synthesis of Mg(AlH4)2is so difficult that Mg(AlH4)2is not commercially available until now, which severely hinders the development of Mg(AlH4)2-based hydrogen storage materials. In this paper, aiming at these problems, the controllable synthesis, high-energy ball milling, catalyst-doping, composite and nanosizing of Mg(AlH4)2were systematically investigated and the corresponding mechanisms were also revealed.
First, a controllable synthesis method was developed to prepare high-purity Mg(AlH4)2submicron rods, and the hydrogen storage thermodynamics and kinetics of the as-prepared Mg(AlH4)2submicron rods were also systematically investigated. The diameter of the as-prepared Mg(AlH4)2submicron rods are0.5μm, and its purity is96.1%. The as-prepared Mg(AlH4)2release9.0wt%of hydrogen through a three-step reaction. MgH2and Al are formed after the first dehydrogenation step, and then Al(Mg) solid solution and MgH2are formed after the second dehydrogenation step, and finally Al3Mg2and Al(Mg) solid solution are formed after the third dehydrogenation step. The first dehydrogenation step is not reversible due to its exothermic nature, and the other two steps are reversible. Kinetic investigations indicate that the first dehydrogenation step of the as-prepared Mg(AlH4)2is a diffusion-controlled reaction with an relatively high apparent activation energy of123.0kJ mol-1, which is mainly responsible for its high on-set dehydrogenation temperature.
Second, the effect of high-energy ball milling on the hydrogen storage properties of Mg(AlH4)2and its mechanism were systematically investigated. After milling for12h, the hydrogen desorption temperatures of Mg(AlH4)2is lowered by40℃. From macro-to micro-scale, high-energy ball milling changes the particle size, grain size, microstrain and lattice distortion of Mg(AlH4)2, specifically decreases the particle size and grain size and increases the microstrain and lattice distortion with prolonging the milling time. The decreases in particle size and grain size can shorten the diffusion distance of the species involved in the dehydrogenation reaction, and the increases in the microstrain and lattice distortion can enhance the diffusivity of the species involved in the dehydrogenation reaction, therefore synergically improve the dehydrogenation kinetics of Mg(AlH4)2.Moreover, the increases in the microstrain and lattice distortion can also raise the Gibbs free energy of Mg(AlH4)2, consequently changes the dehydrogenation thermodynamics of Mg(AlH4)2.
Third, the effect of titanium fluoride on the hydrogen storage properties and its mechanism were investigated. It was found that doping with TiF3and TiF4can significantly reduce the dehydrogenation temperatures of Mg(AlH4)2, and the catalytic activity of TiF4is superior to that of TiF3.2.5mol%TiF4-doped Mg(AlH4)2starts to desorb hydrogen at40℃, and can release4.0wt%of hydrogen at82℃in100min. These is because TiF4can react with Mg(AlH4)2during milling, to in situ form the active catalyst Ti and increase defects, which change the nucleation and growth mode of the first-step dehydrogenation products of Mg(AlH4)2, and consequently lower the activation barrier of the first dehydrogenation step of Mg(AlH4)2.However, the reversibility of Mg(AlH4)2is not improved by doping with TiF4, as2.5mol%TiF4-doped Mg(AlH4)2is still partial reversible.
Fourth, the hydrogen storage properties of Mg(AlH4)2/LiBH4composites and its mechanism were investigated. The research on the Mg(AlH4)2-xLiBH4composites with different molar ratio (x=2,4,6) revealed that with increasing the content of LiBH4, the dehydrogenation temperature of the second step of the Mg(AlH4)2-xLiBH4composite (the reaction of MgH2and Al) is lowered, and the dehydrogenation temperature of the third step (the reaction of Al3Mg2, Al(Mg) and LiBH4) is raised. The reason for the decrease in the reaction temperature of MgH2and Al is:LiBH4is a catalyst for the reaction of MgH2and Al, and the increased content of LiBH4lowers its kinetic barrier; the reason for the increase in the reaction temperature of Al3Mg2, Al(Mg) and LiBH4is:the increased content of LiBH4causes the change of the reaction path and raises the enthalpy change. Furthermore, the effect of byproduct NaCl or LiCl from the synthesis of Mg(AlH4)2on Mg(AlH4)2-6LiBH4composite was then investigated. It is found that NaCl can react with LiBH4to form NaBH4and LiCl, changing the chemical composition of the composite; Cl" ion in LiCl promotes the second dehydrogenation step of Mg(AlH4)2-6LiBH4composite (the reaction of and Al), and LiCl restrains the third dehydrogenation step of Mg(AlH4)2-6LiBH4composite by hindering the contact between Al3Mg2, Al(Mg) and LiBH4
Finally, a mechanical-force-driven physical vapour deposition (MFPVD) method was developed to prepare Mg(AlH4)2nanorods; the formation mechanism was discussed; the hydrogen storage properties were also investigated systematically. It is found that the intense physical force from high-energy ball milling can vaporize the coordination polymer [Mg(AlH4)2(Et2O)]n which possesses a one-dimensional chain-like structure. Then the vaporized material can deposit onto the substrate and self-assemble one-dimensionally to form [Mg(AlH4)2(Et2O)]n nanorods. During successive heat treatment, the Et2O molecules were removed to form Mg(AlH4)2nanorods. The diameter of the as-prepared Mg(AlH4)2nanorods is20-40nm. The as-prepared Mg(AlH4)2nanorods exhibit superior hydrogen storage properties to the Mg(AlH4)2microrods, especially, the as-prepared Mg(AlH4)2nanorods can maintain their nanorod-like morphology during dehydrogenation and hydrogenation processes, consequently show excellent cycling stability. Moreover, LiBH4nanobelts with width of10-40nm were also successfully prepared by a similar process, indicating that the MFPVD method is general enough that can be extended to other complex hydrides which possess organic coordination polymers with unique morphology.
引文
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