摘要
Mg(AlH4)2是一种理想的储氢材料,理论储氢容量高达7.5%(质量分数)。然而较高的起始放氢温度在很大程度上制约了Mg(AlH4)2的应用。正交试验设计方法能够在较少的试验次数中掌握可靠的实验数据以及各因素之间的内在联系从而确定最优的实验方案,特别适用与多因素多水平的实验条件研究。利用高能球磨法成功地制备了Mg(AlH4)2,并将NaAlH4和TiF3引入到该体系中。利用傅里叶红外转换测试仪(FTIR)对产物的结构进行表征,程序控温脱附(TPD)对产物的放氢温度和放氢量进行测定。此外,采用三因素三水平的L9(33)正交试验法,以Mg(AlH4)2的起始放氢温度为指标,以NaAlH4的添加量、TiF3的添加量和球磨间隔时间为因素,同时考察以上3项重要因素对降低Mg(AlH4)2起始放氢温度的影响。通过对正交试验的系统分析发现,NaAlH4的添加量对降低Mg(AlH4)2的起始放氢温度影响最显著,其次为TiF3的添加量,最后为球磨间隔时间。得到最佳试验条件,在最佳条件下Mg(AlH4)2的起始放氢温度仅为72℃,与未添加的相比放氢温度降低了67℃,放氢性能明显提高。
Mg( AlH4 )2 was a kind of ideal hydrogen storage material, and it had a high hydrogen storage capacity of 7.5% (mass fraction). However, its application was blocked by its tough dehydrogenation temperature. Mg( AlH4 )2 was successfully prepared by high energy ball-milling, and further doped with NaAlH4 and TiF3. The Fourier infrared spectrometer (FTIR) and temperature-pro- grammed desorption system (TPD) were used to determine the structure and the onset dehydrogenation temperature of the product, re- spectively. In addition, the L9 (33) orthogonal experimental method was used to determine the optimum conditions to decrease the de- sorption temperature of Mg ( AlH4 ) 2, with the onset dehydrogenation temperature as the indictor, as well as the additive amount of NaAlH4, the additive amount of TiF3 , and the pause time during the ball-milling as the factors. The orthogonal experimental results were systematically investigated. The additive amount of NaAlH4 was found to be the key factor, the next was the additive amount of TiF3, the final ore was the pause time during ball-milling. And the optimal preparation condition was determined. For the Mg ( AlH4 ) 2, prepared under the optimum conditions, the onset desorption temperature reduced to 72 ℃, which was about 67 ℃ lower than the pure Mg(AlH4 )2. The hydrogen storage properties were improved.
出处
《稀有金属》
EI
CAS
CSCD
北大核心
2014年第1期55-59,共5页
Chinese Journal of Rare Metals
基金
国家高技术研究发展计划(2012AA051901)
国家自然科学基金(51071087,51171083,21103124)
天津市应用基础及前沿技术研究项目(11JCYBJC077000)
高等学校学科创新引智基地(111计划)(B12015)资助
关键词
正交试验
因素水平
Mg(AlH4)2
放氢温度
复合催化
orthogonal experimental
factors and levels
Mg( AlH4 ) 2
dehydrogenation temperature
co-catalyst