Ti-Ni系储氢电极合金的微结构和电化学性能研究
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摘要
本文在对国内外Ti基储氢合金材料的研究进展进行全面综述的基础上,确定以抗腐蚀能力强、抗粉化性能好、合金组分数低、在实际生产中使用更为方便的Ti-Ni系合金为研究对象。本研究采用机械合金化法,以前过渡族金属和后过渡族金属Ti、Ni为基础进行机械球磨制备了TiNi、Ti_3Ni_2、Ti_2Ni三种二元非晶合金粉末,运用XRD、RDF、SEM、DSC等材料研究方法和恒电流充放电、循环伏安、电化学阻抗和阶跃等电化学测试方法对不同球磨态的Ti-Ni系合金进行了结构与电化学性能的系统研究,并从中选出具有较高放电容量且综合性能较好的球磨70h的合金样品,进一步研究了退火热处理对该Ti-Ni系合金相结构与电化学性能的影响,力求进一步提高合金的综合电化学性能。
对三种合金的XRD分析显示,在机械合金化的过程中,Ti逐渐向Ni里扩散,二者在机械力的作用下融合形成合金。球磨10h后形成了部分TiNi、Ti_2Ni、Ti_3Ni_2合金,球磨70h后形成了典型的非晶漫散射峰,合金转变为非晶相。由XRD数据进行RDF和g(r)计算表明,球磨70h后合金具有典型的长程无序、短程有序的非晶结构。采用DSC测量了不同球磨时间TiNi合金粉末放热曲线。对于球磨30h的粉末,由于在球磨过程中积累的应变能的释放,约从2000C到4000C出现了一个宽的放热平台。对于球磨70h、100h的合金粉末,基体变成了非晶态,在加热过程中非晶晶化,约在530℃其DSC曲线上有一个明显的相变点。晶化过程中应力完全释放,形成以Ti_2Ni、TiNi相为主的多晶相组织。
随着球磨时间的增加,合金非晶化程度增大,从而导致放电容量增大。三种非晶合金中,球磨70h的Ti3Ni2合金电极的放电容量最高,为173.3mAh/g。TiNi合金电极活化困难,随充放电循环进行,放电容量不断增加,而Ti_2Ni和Ti_3Ni_2合金电极初始放电容量较高,但循环稳定性不好,放电容量逐渐降低。对球磨70h的三种非晶合金样品进行退火热处理,晶化后样品的放电容量均明显增加,其中Ti_2Ni合金电极容量高达289.2mAh/g,但循环稳定性不好,除TiNi外放电容量都急剧下降。电化学性能测试表明,合金电极的动力学性能较好,氢的氧化还原反应控制着电极反应。退火热处理及延长球磨时间可使合金电极表现出相对较好的反应活性和放电容量,所有合金电极中,Ti3Ni2的综合电化学性能较好。
In this thesis, the Ti-Ni based hydrogen storage electrode alloys were selected as the subject on the basis of precious research works on Ti based hydrogen storage alloys which have been extensively reviewed and due to its excellent resistance of corrosion,strong resistance to pulverization, low component number and can be easily used in practical application .In this research,TiNi,Ti_2Ni and Ti_3Ni_2 binary amorphous alloys were prepared by mechanical alloying with Ti and Ni. The microstructure and electrochemical properties of different as-milled Ti-Ni based hydrogen alloys were investigated systemically by means of XRD、RDF、SEM、DSC analysis and the electrochemical test methods, from which the Ti-Ni based alloys milled for 70h with the highest discharge capacity and a better overall electrode properties were selected for further study. Then the effect of annealing treatment on the phase structures and electrochemical properties of Ti-Ni based hydrogen storage alloy’s electrodes were investigated in order to improve the overall electrochemical properties of the alloys.
The results of the study of XRD analysis indicate that Ti diffuse into Ni ,as a result, alloys formed under mechanical force during the process of mechanical alloying. After milling 10h, part alloys of TiNi,Ti_2Ni and Ti_3Ni_2 were formed,and amorphisation occured for longer milling time, after milling for 70h amorphous were formed with representative broad amorphous peak.Applied XRD data to calculate RDF and g(r) indicated that the samples after milling 70h had long-range ordering and disorder in shorter distance charceteristic.The exothermal curves of TiNi alloys powder with different milling time were measured by DSC.For powder milling 30h, there exists a wide exothermal platue from about 2000C to 4000C which cause by the relaxation of strain energy accumulated during milling. The sharp exothermal peaks appear for the powder milling for 70h and 100h which caused by crystallization of amorphous phase.The stress released completely during crystallization process and formed polycrystal phase structure with mostly TiNi and Ti_2Ni phase.
With the ball-milling time postponement the amorphorization degree increased, thus leading to the increment of discharge capacity. The Ti3Ni2 alloy electrode for milling 70h had the maximum discharge capacity (173.3mAh/g) among three kinds of amorphous alloys. Alloy electrodes of TiNi was difficult to be activated ,which discharge capacity increased gradually during the charge-discharge cycles. Alloy electrodes of Ti_2Ni and Ti_3Ni_2 had high initial discharge capacity, but the cycling stability and discharge capacity decreased with the increase of cycle number. The crystallizations of three kinds of amorphous alloys by annealing heattreated improved their discharge capacity,and Ti2Ni alloy electrode had the maximum discharge capacity(289.2mAh/g) among those,but the cyclic capability deteriorated quickly except TiNi alloy eledtrode.The electrochemical performance tests indicated that dynamic performances of alloy electrodes were relatively preferable and the oxidation and deoxidization of hydrogen dominated electrode reaction. Annealing heattreatment and prolong ball-milling time can improve the reactive ability of alloy electrodes and among those electrodes Ti_3Ni_2 alloy electride had the best integrated electrochemical properties.
对三种合金的XRD分析显示,在机械合金化的过程中,Ti逐渐向Ni里扩散,二者在机械力的作用下融合形成合金。球磨10h后形成了部分TiNi、Ti_2Ni、Ti_3Ni_2合金,球磨70h后形成了典型的非晶漫散射峰,合金转变为非晶相。由XRD数据进行RDF和g(r)计算表明,球磨70h后合金具有典型的长程无序、短程有序的非晶结构。采用DSC测量了不同球磨时间TiNi合金粉末放热曲线。对于球磨30h的粉末,由于在球磨过程中积累的应变能的释放,约从2000C到4000C出现了一个宽的放热平台。对于球磨70h、100h的合金粉末,基体变成了非晶态,在加热过程中非晶晶化,约在530℃其DSC曲线上有一个明显的相变点。晶化过程中应力完全释放,形成以Ti_2Ni、TiNi相为主的多晶相组织。
随着球磨时间的增加,合金非晶化程度增大,从而导致放电容量增大。三种非晶合金中,球磨70h的Ti3Ni2合金电极的放电容量最高,为173.3mAh/g。TiNi合金电极活化困难,随充放电循环进行,放电容量不断增加,而Ti_2Ni和Ti_3Ni_2合金电极初始放电容量较高,但循环稳定性不好,放电容量逐渐降低。对球磨70h的三种非晶合金样品进行退火热处理,晶化后样品的放电容量均明显增加,其中Ti_2Ni合金电极容量高达289.2mAh/g,但循环稳定性不好,除TiNi外放电容量都急剧下降。电化学性能测试表明,合金电极的动力学性能较好,氢的氧化还原反应控制着电极反应。退火热处理及延长球磨时间可使合金电极表现出相对较好的反应活性和放电容量,所有合金电极中,Ti3Ni2的综合电化学性能较好。
In this thesis, the Ti-Ni based hydrogen storage electrode alloys were selected as the subject on the basis of precious research works on Ti based hydrogen storage alloys which have been extensively reviewed and due to its excellent resistance of corrosion,strong resistance to pulverization, low component number and can be easily used in practical application .In this research,TiNi,Ti_2Ni and Ti_3Ni_2 binary amorphous alloys were prepared by mechanical alloying with Ti and Ni. The microstructure and electrochemical properties of different as-milled Ti-Ni based hydrogen alloys were investigated systemically by means of XRD、RDF、SEM、DSC analysis and the electrochemical test methods, from which the Ti-Ni based alloys milled for 70h with the highest discharge capacity and a better overall electrode properties were selected for further study. Then the effect of annealing treatment on the phase structures and electrochemical properties of Ti-Ni based hydrogen storage alloy’s electrodes were investigated in order to improve the overall electrochemical properties of the alloys.
The results of the study of XRD analysis indicate that Ti diffuse into Ni ,as a result, alloys formed under mechanical force during the process of mechanical alloying. After milling 10h, part alloys of TiNi,Ti_2Ni and Ti_3Ni_2 were formed,and amorphisation occured for longer milling time, after milling for 70h amorphous were formed with representative broad amorphous peak.Applied XRD data to calculate RDF and g(r) indicated that the samples after milling 70h had long-range ordering and disorder in shorter distance charceteristic.The exothermal curves of TiNi alloys powder with different milling time were measured by DSC.For powder milling 30h, there exists a wide exothermal platue from about 2000C to 4000C which cause by the relaxation of strain energy accumulated during milling. The sharp exothermal peaks appear for the powder milling for 70h and 100h which caused by crystallization of amorphous phase.The stress released completely during crystallization process and formed polycrystal phase structure with mostly TiNi and Ti_2Ni phase.
With the ball-milling time postponement the amorphorization degree increased, thus leading to the increment of discharge capacity. The Ti3Ni2 alloy electrode for milling 70h had the maximum discharge capacity (173.3mAh/g) among three kinds of amorphous alloys. Alloy electrodes of TiNi was difficult to be activated ,which discharge capacity increased gradually during the charge-discharge cycles. Alloy electrodes of Ti_2Ni and Ti_3Ni_2 had high initial discharge capacity, but the cycling stability and discharge capacity decreased with the increase of cycle number. The crystallizations of three kinds of amorphous alloys by annealing heattreated improved their discharge capacity,and Ti2Ni alloy electrode had the maximum discharge capacity(289.2mAh/g) among those,but the cyclic capability deteriorated quickly except TiNi alloy eledtrode.The electrochemical performance tests indicated that dynamic performances of alloy electrodes were relatively preferable and the oxidation and deoxidization of hydrogen dominated electrode reaction. Annealing heattreatment and prolong ball-milling time can improve the reactive ability of alloy electrodes and among those electrodes Ti_3Ni_2 alloy electride had the best integrated electrochemical properties.
引文
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