镁、锡基金属间化合物纳米颗粒的制备及储能特性的研究
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摘要
随着化石能源的日益短缺和温室效应的加剧，未来能源经济的结构重整是不可避免的。能量储存作为能源经济产业链中的重要一环正越来越受到世界各国政府的重视。氢气储存由于与未来的能源经济相关而成为研究热点之一。为了使氢气在诸如汽车推进系统等方面得到实际应用，现存的以气瓶为主的储氢技术必须得到拓展。由于高的重量比容量、体积比容量和低的操作压力，金属氢化物粉末提供了一条解决氢气储存的有效途径。此外，由于在各种化学电源中的优异表现，锂离子电池作为便携式电源在电子消费品市场得到广泛应用。然而，目前主要采用的电极材料(正极为LiCoO_2，负极为碳基材料)由于多年改进已接近其理论能量密度，满足更高能量密度的要求的唯一出路就是寻找新的电极材料。
本文采用一种物理气相沉积方法(直流电弧放电法)系列化制备了镁基和锡基金属间化合物纳米粒子。制备的主要特点在于以金属微米粉压制的复合块体靶材为原料，在活性气体(氢或甲烷)和惰性气体(Ar)混合气氛中蒸发块体靶材，经冷凝和钝化过程获得合金纳米颗粒。这种制备方法克服了镁基、锡基合金由于其体系中组元间熔点差异大，采用传统的熔炼方法不易合金化的困难。另外，通过此种制备方法可以实现金属间化合物纳米颗粒的原位合成，降低了制造成本，提高了材料的实用性。针对纳米粒子腐蚀性能难于表征的问题，采用间接的比较分析方法，即以Sn微米颗粒作为粘结剂与不同核／壳类型的Mg纳米粒子混合压制成Sn／Mg纳米复合物试样，通过其电化学腐蚀性能的对比，间接考察了Mg纳米粒子的抗腐蚀特性。
以Miedema半经验模型和比热随温度变化的经验公式为基础，结合基本热力学关系式，对Sn-Fe、Sn-Ni、Mg-Ni和Mg-Cu纳米粒子体系的有效形成热及其随温度的变化进行了计算，对这些体系中的金属间化合物相的形成规律进行了解释。研究结果表明，根据此热力学模型得到的对生成相的预测与实验结果吻合较好。
在惰性气氛下制备的镁基纳米粒子呈六边形晶体惯态，粒度分布范围50-400 nm；在CH_4气氛下制备的镁基纳米粒子外层为非晶碳层，粒度分布范围为20-100 nm。所有样品的氧化过程分两步进行，分别对应于纳米粒子外层和内核的氧化。动电位极化结果表明，在CH_4气氛下制备的Mg／C纳米复合粒子由于碳的介入具有相对较好的抗腐蚀性能。对于镁基储氢体系，制备了Mg-Ni、Mg-Cu和Mg-Ni-Sn三个体系的纳米粒子，采用传统的测量体积法考察了其气态储氢性能。对Mg-Ni体系而言，Mg_2Ni和MgNi_2两种金属间化合物与Mg、Ni、和MgO共存于纳米粒子中；在一次吸放氢循环后(活化过程)，Mg-Ni纳米粒子呈现出优异的吸氢动力学性能；在氢化处理过程后，由于存在相的转变过程，Mg_2Ni相成为主相；在吸放氢循环后，纳米颗粒粒度进一步减小，这与吸放氢循环过程中的体积膨胀／收缩造成的纳米粒子的碎裂有关；在523，573和623 K的温度下，Mg-Ni纳米粒子的最大吸氢量分别为1．75，2．21，和2．77 wt．％。对于Mg-Cu纳米粒子体系，由Mg_2Cu，MgCu_2，Mg和MgO等四个相组成；在经过几次吸放氢循环后，纳米粒子的粒度减小；在573，598和623 K的温度下Mg-Cu纳米粒子的最大吸氢容量分别为1．92，1．98和2．05 wt．％。为了考察Sn组元的影响，采用同样的方法制备了Mg_(2-x)Sn_xNi(x=0，0．1，0．2)纳米粒子，制备的纳米粒子呈现出复杂的多相结构；在首次氢化过程中，Sn的掺杂明显改善了纳米粒子的吸氢动力学性能；随着Sn组元含量的增加，由P-C-I曲线吸氢平衡压力计算得到的焓值下降，表明Sn的掺杂可以使氢化物的稳定性降低。
制备了Sn-Fe、Sn-Ni，Sn-Mg及碳包覆Sn-Fe等四个体系纳米粒子，并制成模拟电池考察了其电化学性能。对于碳包覆Sn-Fe纳米粒子，TEM结果显示Sn-Fe纳米粒子分散在由纳米碳组成的导电基体中；电极的电化学性能测试表明，由不含碳的纳米粒子制备的电极的初始电容量为562．1 mAh／g，而用碳包覆纳米粒子制备的电极的初始电容量为385．3 mAh／g；得益于适宜的活性／惰性组元微结构，碳包覆纳米粒子电极呈现出较好的电化学循环性能；30次循环后，不含碳的Sn-Fe纳米粒子电极中的FeSn_2相分解为Fe和Sn，而碳包覆Sn-Fe纳米粒子电极中未发现相分解现象。Sn-Ni纳米粒子电极的初始电容量(186．6 mAh／g)比Sn-Fe纳米粒子电极的低，但其循环性能优于后者；30次循环后，Sn-Ni纳米粒子电极未发现相分解现象。Sn-Mg纳米粒子中存在Mg_2Sn相和少量的单质Mg和Sn相；Sn-Mg纳米粒子电极的初始电容量达到430 mAh／g；在放、充电曲线上，在0．2-0．3 V和0．5-0．75 V的电压范围内分别观察到两个明显的电压平台，分别对应着Li和Mg_2Sn的合金化和去合金化过程。
With the growing shortage of fossil fuels and acceleration of global warming, energy economy has to be restructured in the future. Energy storage, an important role in the whole chain, deserves more and more attention from worldwide governments. Hydrogen storage has been one of hot research topics chiefly because of its relevance to the energy economy of the future. For utility applications, such as vehicle propulsion, existing hydrogen storage technology (gas cylinders) will have to be expanded. It is currently thought that metal hydride alloys in the powder form will provide a solution to this problem because of their gravimetric and volumetric storage capacities and safe operating pressures. In addition, Li-ion batteries are currently used as portable power sources in the consumer electronic market for its excellent performances among the chemical power sources. However, the materials (LiCoO_2 for the anode and carbon-based materials for the cathode) is claimed to have already achieved an energy density close to the theoretical limit. The only way to meet demand for even more power is to find a new electrode material.
Mg-based and Sn-based compound nanoparticles were fabricated by a physical vapor condensation method (DC arc discharge). The compressed targets based micrometer powders were used as materials, then the targets were evaporated in a mixture of active gases (H_2 or CH_4) and inert gas (Ar). After condensation and passivation process, compound nanoparticles were obtained. It partly overcomed the difficulties in melting master alloys because of the large difference between Mg/Sn and the other element. Additionally, compound nanoparticles can be prepared in situ by this method, which may be accompanied by a reduction of cost and the improvement of practicality. In view of the difficulties in evaluating the corrosion properties of Mg nanoparticles, a indirect method was adopted in the present work, ie the binding material (pure conductive tin powders) was used to form various Mg/Sn composites and the corrosion properties of nanoparticles were evaluated indirectly by comparing those composite samples each other.
Based on Miedema semi-empirical model and an empirical specific heat equation, the effective heat of formation and its temperature dependence were calculated to explain phase formation in binary Sn-Fe, Sn-Ni, Mg-Ni and Ni-Cu nanoparticles systems. It is shown that predictions of primary phase based on the thermodynamic model have good agreements with the experimental observations.
Various Mg-based nanoparticles were prepared by evaporating bulk magnesium. It is shown that the Mg-based nanoparticles produced in inert atmospheres have hexangular crystal habits with particles' sizes ranging from 50 to 400 nm, while the nanoparticles produced in CH_4 atmosphere have amorphous carbon out layers with particles' sizes among 20-100 nm. Two-steps oxidation process can be confirmed for all samples, which may be attributed to the oxidations of out layer and core of nanoparticle. Potentiodynamic polarization results indicate that Mg/C nanoparticles prepared in CH_4 atmosphere exhibit better corrosion resistance properties due to its peculiar carbon doping. For Mg-based hydrogen storage, Mg-Ni, Mg-Cu, and Mg-Sn-Ni nanoparticles were synthesized by arc discharge in a mixture of argon and hydrogen atmosphere and gas hydrogen properties were explored by by a volumetric method. The intermetallic compounds of Mg_2Ni and MgNi_2 formed with existence of Mg, Ni, and MgO in Mg-Ni nanoparticles. After one cycle of hydrogen absorption/desorption process (activation treatment), Mg-Ni nanoparticles exhibited excellent hydrogen absorption kinetic properties. Mg_2Ni phase became the main phase by a phase transformation during the hydrogen treatments. The phenomenon of refinement of grain size in the nanoparticle was also observed after the hydrogen absorption/desorption processes, which was attributed the break of nanoparticles caused by volume expansion/shrinkage during cycling. Maximum hydrogen absorption contents are 1.75, 2.21 and 2.77 wt. % at 523, 573 and 623 K, respectively. As to Mg-Cu system, four phases (Mg_2Cu, MgCu_2, Mg and MgO) were detected in the as-prepared Mg-Cu nanoparticles. It was found that the sizes of nanoparticles were diminished after several cycles of hydrogen absorption-desorption. Measured Pressure-Composition-Isotherms (P-C-I) curves demonstrated that the hydrogen absorption contents were 1.92, 1.98 and 2.05 wt. % at 573, 598 and 623 K, respectively. In order to explore the effect of Sn-doping, Mg_(2-x)Sn_xNi (x =0, 0.1, 0.2) nanoparticles were synthesized by the same method. It is found that the as-prepared nanoparticles exhibit multiphase complex structure. In the first hydriding process, the kinetics properties were improved with the increase of Sn content. After one hydriding/dehydriding cycle, the samples display fast hydrogen absorption kinetics. Based on measured pressure-composition isotherms (P-C-I) curves, the formation enthalpy of hydrides obtained from the equilibrium plateau pressures decreases with increasing Sn content, implying Sn-doping can weaken the stability of hydrides.
Four system nanoparticles, i.e. Sn-Fe, Sn-Ni, Sn-Mg and C-coated Sn-Fe nanoparticles, were synthesized by the same method and lithium storage properties were studied by model cell. As to Sn-Fe system, the electrochemical properties of electrodes based on Sn-Fe nanoparticles and its corresponding carbon-coated nanoparticles were studied. For carbon-coated nanoparticles, it is found that Sn-Fe nanoparticles (the "active" phase) dispersed in an electrically conductive matrix of nanometer-sized carbon with poor crystallization (the "inactive" phase). The electrochemical testing of the electrodes suggests that the initial capacity is 562.1 mAh/g of electrode based on Sn-Fe nanoparticles, while it is 385.3 mAh/g for its corresponding carbon-coated nanoparticles. The electrode based carbon-coated nanoparticles exhibits better cycling stability compared to its corresponding carbon-free sample, which is tightly associated with the appropriate active/inactive microstructure. According to XRD analysis, FeSn_2 decomposes to Fe and Sn completely for carbon-free sample after 30 cycling, and it is adverse in the carbon-coated sample. Compared with Fe-Sn carbon-free electrode, Sn-Ni electrode displays low initial capacity (186.6 mAh/g), but better cycling stability is obtained. After 30 cycles, there is no clear evidence to support the decomposition of Ni_3Sn_4 in Sn-Ni electrode. Compound Mg_2Sn was generated and coexisted with residual phases of Mg and Sn in nanoparticles. The initial capacity of Mg_2Sn electrode reaches 430 mAh/g. Two visible plateaus at 0.2-0.3 and 0.5-0.75 V were observed in the discharge/charge curves, which can be attributed to alloying/dealloying reactions between Li and Mg_2Sn, respectively.
本文采用一种物理气相沉积方法(直流电弧放电法)系列化制备了镁基和锡基金属间化合物纳米粒子。制备的主要特点在于以金属微米粉压制的复合块体靶材为原料，在活性气体(氢或甲烷)和惰性气体(Ar)混合气氛中蒸发块体靶材，经冷凝和钝化过程获得合金纳米颗粒。这种制备方法克服了镁基、锡基合金由于其体系中组元间熔点差异大，采用传统的熔炼方法不易合金化的困难。另外，通过此种制备方法可以实现金属间化合物纳米颗粒的原位合成，降低了制造成本，提高了材料的实用性。针对纳米粒子腐蚀性能难于表征的问题，采用间接的比较分析方法，即以Sn微米颗粒作为粘结剂与不同核／壳类型的Mg纳米粒子混合压制成Sn／Mg纳米复合物试样，通过其电化学腐蚀性能的对比，间接考察了Mg纳米粒子的抗腐蚀特性。
以Miedema半经验模型和比热随温度变化的经验公式为基础，结合基本热力学关系式，对Sn-Fe、Sn-Ni、Mg-Ni和Mg-Cu纳米粒子体系的有效形成热及其随温度的变化进行了计算，对这些体系中的金属间化合物相的形成规律进行了解释。研究结果表明，根据此热力学模型得到的对生成相的预测与实验结果吻合较好。
在惰性气氛下制备的镁基纳米粒子呈六边形晶体惯态，粒度分布范围50-400 nm；在CH_4气氛下制备的镁基纳米粒子外层为非晶碳层，粒度分布范围为20-100 nm。所有样品的氧化过程分两步进行，分别对应于纳米粒子外层和内核的氧化。动电位极化结果表明，在CH_4气氛下制备的Mg／C纳米复合粒子由于碳的介入具有相对较好的抗腐蚀性能。对于镁基储氢体系，制备了Mg-Ni、Mg-Cu和Mg-Ni-Sn三个体系的纳米粒子，采用传统的测量体积法考察了其气态储氢性能。对Mg-Ni体系而言，Mg_2Ni和MgNi_2两种金属间化合物与Mg、Ni、和MgO共存于纳米粒子中；在一次吸放氢循环后(活化过程)，Mg-Ni纳米粒子呈现出优异的吸氢动力学性能；在氢化处理过程后，由于存在相的转变过程，Mg_2Ni相成为主相；在吸放氢循环后，纳米颗粒粒度进一步减小，这与吸放氢循环过程中的体积膨胀／收缩造成的纳米粒子的碎裂有关；在523，573和623 K的温度下，Mg-Ni纳米粒子的最大吸氢量分别为1．75，2．21，和2．77 wt．％。对于Mg-Cu纳米粒子体系，由Mg_2Cu，MgCu_2，Mg和MgO等四个相组成；在经过几次吸放氢循环后，纳米粒子的粒度减小；在573，598和623 K的温度下Mg-Cu纳米粒子的最大吸氢容量分别为1．92，1．98和2．05 wt．％。为了考察Sn组元的影响，采用同样的方法制备了Mg_(2-x)Sn_xNi(x=0，0．1，0．2)纳米粒子，制备的纳米粒子呈现出复杂的多相结构；在首次氢化过程中，Sn的掺杂明显改善了纳米粒子的吸氢动力学性能；随着Sn组元含量的增加，由P-C-I曲线吸氢平衡压力计算得到的焓值下降，表明Sn的掺杂可以使氢化物的稳定性降低。
制备了Sn-Fe、Sn-Ni，Sn-Mg及碳包覆Sn-Fe等四个体系纳米粒子，并制成模拟电池考察了其电化学性能。对于碳包覆Sn-Fe纳米粒子，TEM结果显示Sn-Fe纳米粒子分散在由纳米碳组成的导电基体中；电极的电化学性能测试表明，由不含碳的纳米粒子制备的电极的初始电容量为562．1 mAh／g，而用碳包覆纳米粒子制备的电极的初始电容量为385．3 mAh／g；得益于适宜的活性／惰性组元微结构，碳包覆纳米粒子电极呈现出较好的电化学循环性能；30次循环后，不含碳的Sn-Fe纳米粒子电极中的FeSn_2相分解为Fe和Sn，而碳包覆Sn-Fe纳米粒子电极中未发现相分解现象。Sn-Ni纳米粒子电极的初始电容量(186．6 mAh／g)比Sn-Fe纳米粒子电极的低，但其循环性能优于后者；30次循环后，Sn-Ni纳米粒子电极未发现相分解现象。Sn-Mg纳米粒子中存在Mg_2Sn相和少量的单质Mg和Sn相；Sn-Mg纳米粒子电极的初始电容量达到430 mAh／g；在放、充电曲线上，在0．2-0．3 V和0．5-0．75 V的电压范围内分别观察到两个明显的电压平台，分别对应着Li和Mg_2Sn的合金化和去合金化过程。
With the growing shortage of fossil fuels and acceleration of global warming, energy economy has to be restructured in the future. Energy storage, an important role in the whole chain, deserves more and more attention from worldwide governments. Hydrogen storage has been one of hot research topics chiefly because of its relevance to the energy economy of the future. For utility applications, such as vehicle propulsion, existing hydrogen storage technology (gas cylinders) will have to be expanded. It is currently thought that metal hydride alloys in the powder form will provide a solution to this problem because of their gravimetric and volumetric storage capacities and safe operating pressures. In addition, Li-ion batteries are currently used as portable power sources in the consumer electronic market for its excellent performances among the chemical power sources. However, the materials (LiCoO_2 for the anode and carbon-based materials for the cathode) is claimed to have already achieved an energy density close to the theoretical limit. The only way to meet demand for even more power is to find a new electrode material.
Mg-based and Sn-based compound nanoparticles were fabricated by a physical vapor condensation method (DC arc discharge). The compressed targets based micrometer powders were used as materials, then the targets were evaporated in a mixture of active gases (H_2 or CH_4) and inert gas (Ar). After condensation and passivation process, compound nanoparticles were obtained. It partly overcomed the difficulties in melting master alloys because of the large difference between Mg/Sn and the other element. Additionally, compound nanoparticles can be prepared in situ by this method, which may be accompanied by a reduction of cost and the improvement of practicality. In view of the difficulties in evaluating the corrosion properties of Mg nanoparticles, a indirect method was adopted in the present work, ie the binding material (pure conductive tin powders) was used to form various Mg/Sn composites and the corrosion properties of nanoparticles were evaluated indirectly by comparing those composite samples each other.
Based on Miedema semi-empirical model and an empirical specific heat equation, the effective heat of formation and its temperature dependence were calculated to explain phase formation in binary Sn-Fe, Sn-Ni, Mg-Ni and Ni-Cu nanoparticles systems. It is shown that predictions of primary phase based on the thermodynamic model have good agreements with the experimental observations.
Various Mg-based nanoparticles were prepared by evaporating bulk magnesium. It is shown that the Mg-based nanoparticles produced in inert atmospheres have hexangular crystal habits with particles' sizes ranging from 50 to 400 nm, while the nanoparticles produced in CH_4 atmosphere have amorphous carbon out layers with particles' sizes among 20-100 nm. Two-steps oxidation process can be confirmed for all samples, which may be attributed to the oxidations of out layer and core of nanoparticle. Potentiodynamic polarization results indicate that Mg/C nanoparticles prepared in CH_4 atmosphere exhibit better corrosion resistance properties due to its peculiar carbon doping. For Mg-based hydrogen storage, Mg-Ni, Mg-Cu, and Mg-Sn-Ni nanoparticles were synthesized by arc discharge in a mixture of argon and hydrogen atmosphere and gas hydrogen properties were explored by by a volumetric method. The intermetallic compounds of Mg_2Ni and MgNi_2 formed with existence of Mg, Ni, and MgO in Mg-Ni nanoparticles. After one cycle of hydrogen absorption/desorption process (activation treatment), Mg-Ni nanoparticles exhibited excellent hydrogen absorption kinetic properties. Mg_2Ni phase became the main phase by a phase transformation during the hydrogen treatments. The phenomenon of refinement of grain size in the nanoparticle was also observed after the hydrogen absorption/desorption processes, which was attributed the break of nanoparticles caused by volume expansion/shrinkage during cycling. Maximum hydrogen absorption contents are 1.75, 2.21 and 2.77 wt. % at 523, 573 and 623 K, respectively. As to Mg-Cu system, four phases (Mg_2Cu, MgCu_2, Mg and MgO) were detected in the as-prepared Mg-Cu nanoparticles. It was found that the sizes of nanoparticles were diminished after several cycles of hydrogen absorption-desorption. Measured Pressure-Composition-Isotherms (P-C-I) curves demonstrated that the hydrogen absorption contents were 1.92, 1.98 and 2.05 wt. % at 573, 598 and 623 K, respectively. In order to explore the effect of Sn-doping, Mg_(2-x)Sn_xNi (x =0, 0.1, 0.2) nanoparticles were synthesized by the same method. It is found that the as-prepared nanoparticles exhibit multiphase complex structure. In the first hydriding process, the kinetics properties were improved with the increase of Sn content. After one hydriding/dehydriding cycle, the samples display fast hydrogen absorption kinetics. Based on measured pressure-composition isotherms (P-C-I) curves, the formation enthalpy of hydrides obtained from the equilibrium plateau pressures decreases with increasing Sn content, implying Sn-doping can weaken the stability of hydrides.
Four system nanoparticles, i.e. Sn-Fe, Sn-Ni, Sn-Mg and C-coated Sn-Fe nanoparticles, were synthesized by the same method and lithium storage properties were studied by model cell. As to Sn-Fe system, the electrochemical properties of electrodes based on Sn-Fe nanoparticles and its corresponding carbon-coated nanoparticles were studied. For carbon-coated nanoparticles, it is found that Sn-Fe nanoparticles (the "active" phase) dispersed in an electrically conductive matrix of nanometer-sized carbon with poor crystallization (the "inactive" phase). The electrochemical testing of the electrodes suggests that the initial capacity is 562.1 mAh/g of electrode based on Sn-Fe nanoparticles, while it is 385.3 mAh/g for its corresponding carbon-coated nanoparticles. The electrode based carbon-coated nanoparticles exhibits better cycling stability compared to its corresponding carbon-free sample, which is tightly associated with the appropriate active/inactive microstructure. According to XRD analysis, FeSn_2 decomposes to Fe and Sn completely for carbon-free sample after 30 cycling, and it is adverse in the carbon-coated sample. Compared with Fe-Sn carbon-free electrode, Sn-Ni electrode displays low initial capacity (186.6 mAh/g), but better cycling stability is obtained. After 30 cycles, there is no clear evidence to support the decomposition of Ni_3Sn_4 in Sn-Ni electrode. Compound Mg_2Sn was generated and coexisted with residual phases of Mg and Sn in nanoparticles. The initial capacity of Mg_2Sn electrode reaches 430 mAh/g. Two visible plateaus at 0.2-0.3 and 0.5-0.75 V were observed in the discharge/charge curves, which can be attributed to alloying/dealloying reactions between Li and Mg_2Sn, respectively.
引文
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