固体透氧膜法直接制备储氢合金新工艺
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摘要
以LaNi5为代表的AB5型储氢合金具有较高的储氢容量，良好的吸放氢动力学特性，以及活化容易、平衡压力适中、吸放氢平衡压差小等优势，已成为储氢材料应用研究的重点之一。目前商用AB5型储氢合金的工业制备方法为高温熔炼法，制备工艺复杂，生产流程长、成本高、污染重，应用受到限制。因此，开发一种短流程、易操作、低能耗、少污染的新型制备方法势在必行。
本文综述了储氢合金现有的制备工艺及研究进展，分析了各种工艺特色及优缺点，在此基础上提出了采用SOM（固体透氧膜）工艺，以混合金属氧化物为原料直接电解脱氧制备储氢合金。透氧膜的采用提高了电解电压因而提高了电解速率。论文详细研究了熔盐的性质（挥发速率、电导率），透氧膜的电导率和抗腐蚀性，烧结、粒度、成型压力、电压、温度等参数对电解过程的影响，以及反应机理和反应速率，并与FFC工艺和其它工艺进行了对比。
对熔盐CaCl_2的研究表明，950℃CaCl_2及CaCl_2-NaCl熔盐挥发速率小于3.02×10~(-6)g·cm~(-2)·s，电导率高于3.3S·m~(-1)；实验室自制的透氧膜管为8%Y_2O_3稳定的ZrO_2管，结构致密，有良好的抗腐蚀性和导电性，在950℃电导率为0.131S·m~(-1)；实验采用的各种氧化物烧结片在950℃CaCl_2中的溶解度均低于0.078%。以上参数均满足实验要求。
SOM法直接制备LaNi_5合金的研究结果表明：采用SOM法从La_2O_3-NiO混合物烧结片直接制备储氢合金LaNi_5是可行的；实验最佳的电解温度为950℃，更高的电解温度下，活性金属La会部分流失；电解产物的组成及收率表明最佳的烧结温度为1000℃，烧结片的组成为La_4Ni_3O_(10)和NiO；电解机理为La_4Ni_3O_(10)在氩气氛下的预热过程中生成La_2NiO_4，烧结片浸入熔盐后La_2NiO_4与CaCl_2迅速自发地反应生成LaOCl和NiO，随后NiO电解还原出的金属Ni与LaOCl反应生成LaNi_5；电解过程的电流效率为86.7%，能耗为3.55kWh/kgLaNi_5；实验对产物的储氢性能测试表明，SOM工艺制备的LaNi_5，最高储氢容量为1.43%，达到理论容量的90%，高于FFC和其它工艺制备的LaNi_5；产物成分均匀，因而更容易活化，其第一次活化过程吸氢量即达0.85%；吸放氢平台在0.2~0.3MPa，与理论值相符；电解产物经水洗、烘干后即表现出较高的储氢容量，与传统工艺相比，无需复杂的后续处理，进一步缩短了流程。
SOM法直接制备CeNi_5的研究结果表明：用NiO-CeO_2烧结片直接电解制备合金CeNi_5的还原机理为NiO首先被还原为Ni，与随后生成的CeOCl反应生成CeNi_5；最优工艺条件为：球磨时间25h、制片压力15MPa、烧结温度850℃、电解温度1000℃、电解时间3h；电解电流效率为75.5%，能耗为4.03kW·h/kg。
实验证实了直接制备LaNi_5的A侧及B侧取代，如La_xCe_(1-x)Ni_5（x=0、0.2、0.4、0.6、0.8、1.0）、LaNi_(4.6)Si_(0.4)、LaNi_4Al的可行性。混合氧化物烧结片的成分分别为NiO-La_4Ni_3O_(10)、NiO-La_(10)(SiO_4)_6O_3-La_4Ni_3O_(10)、NiO-LaAlO_3。SOM工艺的优势在于可采用较高的电解电压来提高电解速率，因此在透氧膜管可承受的范围内电解电压应尽可能地高，本实验制备的膜管可承受的最高电压为4V。在以SiO2制Si以及NiO-La_(10)(SiO_4)_6O_3-La_4Ni_3O_(10)制备的LaNi_(4.6)Si_(0.4)的研究中发现，在较高的电解电压下（3.9V），由于存在CaSiO3的分解，产物中含有大量CaSi。而在3.5V的电压下可获得较为理想的反应产物。
根据中间产物和循环伏安曲线分析了电脱氧机理，推出了电解速率模型，影响电解速率的因素包括阴极片孔隙率、电极接触面积、电压、透氧膜电导率及厚度、熔盐电导率等，电解速率公式为：
实验对SOM工艺和FFC工艺进行了对比，结果表明：SOM工艺电解产物为疏松的海绵状结构，有较大的比表面积，更适合用作储氢材料，而FFC工艺由于电解时间较长，电解产物经过长时间烧结后颗粒互相粘连，出现一定程度的玻璃态；SOM工艺电解过程结束电流降到背景电流值，而FFC工艺由于阳极碳棒和熔盐直接接触，碳粉剥落后引起电子电导，因而电流上升降低了电流效率；SOM工艺与FFC工艺相比，电解时间缩短3倍，电流效率提高3倍，能耗降低66~75%，有更好的应用前景。
The LaNi_5-type hydrogen storage alloy is becoming one of the emphases ofresearch in hydrogen storage materials. It possesses the excellent performanceproperties: large hydrogen storage capacity, excellent dynamic characteristics andlittle difference of balance pressure between the hydrogen absorbing and releasing. Itis easy to be activated, and also the balance pressure of it is moderate and flat. Thecommonly used preparation process is the induction melting method, which involvesthe melting of the individual metals of high purity, followed by a prolongedannealing process at elevated temperatures. Such a multistep process involves highenergy consumption and high environmental impact and results in low productionefficiency. Many efforts have been made to develop novel processes with highefficiency of production and also low cost.
This paper summarized the current preparing processes and research progress ofAB5type of hydrogen storage alloy, analyzed the characteristic, advantage anddisadvantage of them. To solve the problems exist in present process, we propose theSOM process and directly prepared hydrogen storage alloy from oxide precursors. Ahigher voltage was used in SOM process to achieve high deoxidization rate. Thispaper was focused on the property of the molten salt, the stability and conductanceof solid oxide-ion membrane, the impact of electrolysis parameter such as sintering,ball-milled time, cathode preparing, electrolysis voltage, molten slat temperature onthe process. The experimental results were compared with FFC process.
The investigation of the molten CaCl_2showed that the volatility was lower than3.02×10~(-6)g·cm~(-2)·s at950oC, the conductivity of it was higher than3.3S·m~(-1). Thecomposition of solid oxygen-ion membrane was8%mol Y2O3stabilized ZrO2whichwas compact and resist-eroded. The conductivity of it was0.131S m-1at950oC.
Direct electrochemical reduction of mixed oxide precursor to LaNi_5alloy inmolten salt by SOM process was confirmed to be feasible. The optimal sintering temperature and molten salt temperature was1000and950℃respectively. La woulddissolved in molten slat if the temperature was high than1000oC or the electrolysistime was longer than3h. The composition of the sintered pellet was La4Ni3O10, itreacted with the molten CaCl_2spontaneously to form LaOCl and NiO. Theelectrodeoxidization of the sintered pellet of La2O3-NiO (actually LaOCl-NiO)consisted of two steps:(1) The NiO was reduced to metal Ni; and (2) theintermediate product LaOCl react with pre-formed Ni to form LaNi_5alloy. Thecurrent efficiency was86.7%and the energy consumption was as low as3.55kW·h/kg-LaNi_5. The test of hydrogen storage capacity of the LaNi_5product showedthat the maximum hydrogen storage capacity was1.43%under the pressure of3MPawhich was higher than the product of FFC and other process. The absorption andrelease hydrogen platform appeared in range of0.2-0.3MPa which was accordedwith theoretical value. The activation curve showed that the capacity of productreached1.35%after20activation cycles which was not far away from the maximumhydrogen storage capacity. Another one to mention was the product LaNi_5fromSOM process was only washed, milled with mortar and dried in oven, while theproduct from conventional process must be treated with a serious of follow-upprocess. So SOM process can further shorten the productive process.
The investigation of preparing of CeNi5by SOM process showed that thereduction of NiO-CeO_2may take place in two steps: first, NiO was reduced into Niand CeO2reacted with CaCl_2to form CeOCl, then Ni reacted with CeOCl leading toform CeNi5. The optimal conditions for the electrochemical reduction are:ball-milled time25h, pellet pressure load15MPa, sintering temperature850℃,molten salt temperature1000℃, electrolysis time3h.The current efficiency was75.5%and the energy consumption was as low as4.03kW·h/kg-CeNi5.
The experiment also demonstrate the feasibility of direct preparation of morecomplex rare earth based multi-element alloys such as La_xCe_(1-x)Ni_5(x=0.2,0.4,0.6,0.8), LaNi_(4.6)Si_(0.4), LaNi_4Al from the relative oxides. The composition of the sintered pellet was NiO-La_4Ni_3O_(10), NiO-La_(10)(SiO_4)_6O_3-La_4Ni_3O_(10), NiO-LaAlO_3respectively.The advantage of SOM process was higher electrolysis voltage to achieve highdeoxidization rate, so the voltage should be as high as impossible. But in the processof preparing Si and LaNi_(4.6)Si_(0.4), it was found that there was CaSi appeared if thevoltage was3.9V for the decomposition of CaSiO3.The result also showed that theperfect product which we wanted was achieved under the voltage of3.5V
The reduction mechanism was investigated by the cyclic voltammetry as well asthe phase composition of the intermediate products. The electrolysis rate wasaffected by the porosity of cathode, contact area, electrolysis voltage, conductivityand thickness of SOM, conductivity of molten salt. The equation of electrolysis ratewas calculated as the equation followed:
Comparison of the SOM and FFC process was performed, the results showed thatthe product of SOM process was better to be used as hydrogen storage materials fornormal sponginess and high porosity rate, while the product of FFC processdisplayed the conglutination of the grains and a low porosity rate, it may beattributed to the long time of sintering in molten salt. In SOM process the currentdecreased to the leakage current at the end of electrolysis, while it rose at the end ofexperiment for the electronic conductivity resulted from the carbon powderseparated from graphite rod. In comparison with FFC process, SOM process wasmore efficient and suitable for industrial application, it only needed25~33%ofenergy consumption, while it reduced3times of electrolysis time and enhanced3times of current efficiency.
本文综述了储氢合金现有的制备工艺及研究进展，分析了各种工艺特色及优缺点，在此基础上提出了采用SOM（固体透氧膜）工艺，以混合金属氧化物为原料直接电解脱氧制备储氢合金。透氧膜的采用提高了电解电压因而提高了电解速率。论文详细研究了熔盐的性质（挥发速率、电导率），透氧膜的电导率和抗腐蚀性，烧结、粒度、成型压力、电压、温度等参数对电解过程的影响，以及反应机理和反应速率，并与FFC工艺和其它工艺进行了对比。
对熔盐CaCl_2的研究表明，950℃CaCl_2及CaCl_2-NaCl熔盐挥发速率小于3.02×10~(-6)g·cm~(-2)·s，电导率高于3.3S·m~(-1)；实验室自制的透氧膜管为8%Y_2O_3稳定的ZrO_2管，结构致密，有良好的抗腐蚀性和导电性，在950℃电导率为0.131S·m~(-1)；实验采用的各种氧化物烧结片在950℃CaCl_2中的溶解度均低于0.078%。以上参数均满足实验要求。
SOM法直接制备LaNi_5合金的研究结果表明：采用SOM法从La_2O_3-NiO混合物烧结片直接制备储氢合金LaNi_5是可行的；实验最佳的电解温度为950℃，更高的电解温度下，活性金属La会部分流失；电解产物的组成及收率表明最佳的烧结温度为1000℃，烧结片的组成为La_4Ni_3O_(10)和NiO；电解机理为La_4Ni_3O_(10)在氩气氛下的预热过程中生成La_2NiO_4，烧结片浸入熔盐后La_2NiO_4与CaCl_2迅速自发地反应生成LaOCl和NiO，随后NiO电解还原出的金属Ni与LaOCl反应生成LaNi_5；电解过程的电流效率为86.7%，能耗为3.55kWh/kgLaNi_5；实验对产物的储氢性能测试表明，SOM工艺制备的LaNi_5，最高储氢容量为1.43%，达到理论容量的90%，高于FFC和其它工艺制备的LaNi_5；产物成分均匀，因而更容易活化，其第一次活化过程吸氢量即达0.85%；吸放氢平台在0.2~0.3MPa，与理论值相符；电解产物经水洗、烘干后即表现出较高的储氢容量，与传统工艺相比，无需复杂的后续处理，进一步缩短了流程。
SOM法直接制备CeNi_5的研究结果表明：用NiO-CeO_2烧结片直接电解制备合金CeNi_5的还原机理为NiO首先被还原为Ni，与随后生成的CeOCl反应生成CeNi_5；最优工艺条件为：球磨时间25h、制片压力15MPa、烧结温度850℃、电解温度1000℃、电解时间3h；电解电流效率为75.5%，能耗为4.03kW·h/kg。
实验证实了直接制备LaNi_5的A侧及B侧取代，如La_xCe_(1-x)Ni_5（x=0、0.2、0.4、0.6、0.8、1.0）、LaNi_(4.6)Si_(0.4)、LaNi_4Al的可行性。混合氧化物烧结片的成分分别为NiO-La_4Ni_3O_(10)、NiO-La_(10)(SiO_4)_6O_3-La_4Ni_3O_(10)、NiO-LaAlO_3。SOM工艺的优势在于可采用较高的电解电压来提高电解速率，因此在透氧膜管可承受的范围内电解电压应尽可能地高，本实验制备的膜管可承受的最高电压为4V。在以SiO2制Si以及NiO-La_(10)(SiO_4)_6O_3-La_4Ni_3O_(10)制备的LaNi_(4.6)Si_(0.4)的研究中发现，在较高的电解电压下（3.9V），由于存在CaSiO3的分解，产物中含有大量CaSi。而在3.5V的电压下可获得较为理想的反应产物。
根据中间产物和循环伏安曲线分析了电脱氧机理，推出了电解速率模型，影响电解速率的因素包括阴极片孔隙率、电极接触面积、电压、透氧膜电导率及厚度、熔盐电导率等，电解速率公式为：
实验对SOM工艺和FFC工艺进行了对比，结果表明：SOM工艺电解产物为疏松的海绵状结构，有较大的比表面积，更适合用作储氢材料，而FFC工艺由于电解时间较长，电解产物经过长时间烧结后颗粒互相粘连，出现一定程度的玻璃态；SOM工艺电解过程结束电流降到背景电流值，而FFC工艺由于阳极碳棒和熔盐直接接触，碳粉剥落后引起电子电导，因而电流上升降低了电流效率；SOM工艺与FFC工艺相比，电解时间缩短3倍，电流效率提高3倍，能耗降低66~75%，有更好的应用前景。
The LaNi_5-type hydrogen storage alloy is becoming one of the emphases ofresearch in hydrogen storage materials. It possesses the excellent performanceproperties: large hydrogen storage capacity, excellent dynamic characteristics andlittle difference of balance pressure between the hydrogen absorbing and releasing. Itis easy to be activated, and also the balance pressure of it is moderate and flat. Thecommonly used preparation process is the induction melting method, which involvesthe melting of the individual metals of high purity, followed by a prolongedannealing process at elevated temperatures. Such a multistep process involves highenergy consumption and high environmental impact and results in low productionefficiency. Many efforts have been made to develop novel processes with highefficiency of production and also low cost.
This paper summarized the current preparing processes and research progress ofAB5type of hydrogen storage alloy, analyzed the characteristic, advantage anddisadvantage of them. To solve the problems exist in present process, we propose theSOM process and directly prepared hydrogen storage alloy from oxide precursors. Ahigher voltage was used in SOM process to achieve high deoxidization rate. Thispaper was focused on the property of the molten salt, the stability and conductanceof solid oxide-ion membrane, the impact of electrolysis parameter such as sintering,ball-milled time, cathode preparing, electrolysis voltage, molten slat temperature onthe process. The experimental results were compared with FFC process.
The investigation of the molten CaCl_2showed that the volatility was lower than3.02×10~(-6)g·cm~(-2)·s at950oC, the conductivity of it was higher than3.3S·m~(-1). Thecomposition of solid oxygen-ion membrane was8%mol Y2O3stabilized ZrO2whichwas compact and resist-eroded. The conductivity of it was0.131S m-1at950oC.
Direct electrochemical reduction of mixed oxide precursor to LaNi_5alloy inmolten salt by SOM process was confirmed to be feasible. The optimal sintering temperature and molten salt temperature was1000and950℃respectively. La woulddissolved in molten slat if the temperature was high than1000oC or the electrolysistime was longer than3h. The composition of the sintered pellet was La4Ni3O10, itreacted with the molten CaCl_2spontaneously to form LaOCl and NiO. Theelectrodeoxidization of the sintered pellet of La2O3-NiO (actually LaOCl-NiO)consisted of two steps:(1) The NiO was reduced to metal Ni; and (2) theintermediate product LaOCl react with pre-formed Ni to form LaNi_5alloy. Thecurrent efficiency was86.7%and the energy consumption was as low as3.55kW·h/kg-LaNi_5. The test of hydrogen storage capacity of the LaNi_5product showedthat the maximum hydrogen storage capacity was1.43%under the pressure of3MPawhich was higher than the product of FFC and other process. The absorption andrelease hydrogen platform appeared in range of0.2-0.3MPa which was accordedwith theoretical value. The activation curve showed that the capacity of productreached1.35%after20activation cycles which was not far away from the maximumhydrogen storage capacity. Another one to mention was the product LaNi_5fromSOM process was only washed, milled with mortar and dried in oven, while theproduct from conventional process must be treated with a serious of follow-upprocess. So SOM process can further shorten the productive process.
The investigation of preparing of CeNi5by SOM process showed that thereduction of NiO-CeO_2may take place in two steps: first, NiO was reduced into Niand CeO2reacted with CaCl_2to form CeOCl, then Ni reacted with CeOCl leading toform CeNi5. The optimal conditions for the electrochemical reduction are:ball-milled time25h, pellet pressure load15MPa, sintering temperature850℃,molten salt temperature1000℃, electrolysis time3h.The current efficiency was75.5%and the energy consumption was as low as4.03kW·h/kg-CeNi5.
The experiment also demonstrate the feasibility of direct preparation of morecomplex rare earth based multi-element alloys such as La_xCe_(1-x)Ni_5(x=0.2,0.4,0.6,0.8), LaNi_(4.6)Si_(0.4), LaNi_4Al from the relative oxides. The composition of the sintered pellet was NiO-La_4Ni_3O_(10), NiO-La_(10)(SiO_4)_6O_3-La_4Ni_3O_(10), NiO-LaAlO_3respectively.The advantage of SOM process was higher electrolysis voltage to achieve highdeoxidization rate, so the voltage should be as high as impossible. But in the processof preparing Si and LaNi_(4.6)Si_(0.4), it was found that there was CaSi appeared if thevoltage was3.9V for the decomposition of CaSiO3.The result also showed that theperfect product which we wanted was achieved under the voltage of3.5V
The reduction mechanism was investigated by the cyclic voltammetry as well asthe phase composition of the intermediate products. The electrolysis rate wasaffected by the porosity of cathode, contact area, electrolysis voltage, conductivityand thickness of SOM, conductivity of molten salt. The equation of electrolysis ratewas calculated as the equation followed:
Comparison of the SOM and FFC process was performed, the results showed thatthe product of SOM process was better to be used as hydrogen storage materials fornormal sponginess and high porosity rate, while the product of FFC processdisplayed the conglutination of the grains and a low porosity rate, it may beattributed to the long time of sintering in molten salt. In SOM process the currentdecreased to the leakage current at the end of electrolysis, while it rose at the end ofexperiment for the electronic conductivity resulted from the carbon powderseparated from graphite rod. In comparison with FFC process, SOM process wasmore efficient and suitable for industrial application, it only needed25~33%ofenergy consumption, while it reduced3times of electrolysis time and enhanced3times of current efficiency.
引文
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