研究用甲酸作为调制剂,在微波条件下,通过溶剂热法在短时间成功合成出了不同尺寸的金属有机框架化合物Ui O-66纳米晶体,并与传统烘箱加热合成的Ui O-66晶体进行了对比。XRD和SEM表征结果表明:甲酸的调制使晶体的结晶度和颗粒尺寸都增大。N_2物理吸附研究表明,通过不同加热条件合成的Ui O-66晶体具有相近的微孔体积,但是孔径分布有明显的区别。结果表明,微波合成样品的孔径主要集中在0.82和1.10 nm,而传统烘箱加热合成的样品孔径则集中在0.82,1.10和1.63 nm处。由于微波合成的样品具有更小的孔径分布,因而使其在77 K和1×10~5Pa下具有更高的氢气吸附量,样品MW-50(甲酸与Zr Cl_4摩尔比为50∶1)和MW-100的储氢量分别达到1.83%和1.85%(质量分数),而CE-50和CE-100仅为1.57%和1.58%(质量分数)。
The synthesis of UIO-66 was reported by using formic acid as the template under both microwave (MW) irradiation heating and conventional electric (CE) heating. XRD and SEM analysis show the enhancement of crystaUinity and particle sizes with the addition of formic acid. Obvious differences of pore size distribution from DFT method were observed for the synthesized UIO-66. For the similar micro pore volumes (pore width 〈2 nm), in terms of the pore size distribution from the DFT method, the materials prepared by MW heating show two major peaks at 0.82 and 1.10 nm, while the materials using CE heating appear three major peaks at 0.82, 1.10 and 1.63 nm. This leads to higher H2 storage capacities of 1.83% and 1.85% for the MW-50 (mole ratio of formic acid and ZrCI4 is 50 : 1) and MW-100 (mole ratio of formic acid and 7JCI4 is 100 : 1) than those of 1.57% and 1.58% for CE-50 and CE-100 at 1 bar and 77 K, respectively.