溶胶-凝胶法制备纳米锑掺杂氧化锡的团聚消除

Agglomeration eliminating nano-sized antimony doped tin oxide prepared by sol-gel method

采用溶胶-凝胶法制备纳米锑掺杂氧化锡(antimony doped tin oxide,ATO)前驱体,然后通过烘干、微波、真空以及超临界流体干燥(supercritical fluid drying,SCFD)等方式干燥醇凝胶,并在600℃下进行热处理,考察干燥方式对最终产物纳米ATO团聚情况的影响。利用XRD、SEM、TEM、马尔文粒度仪等对前驱体以及纳米ATO的结构、形貌等进行表征,结果表明:采用4种方式对前驱体醇凝胶进行干燥,以SCFD处理得到的前驱体结构最为疏松,ATO颗粒呈不规则球形、粒度较为均匀,平均粒径约25nm。通过对常规干燥过程导致团聚以及SCFD消除前驱体粒子团聚的机理分析,揭示了采用超临界流体干燥醇凝胶能够使前驱体粒子保持松散的结构,并最终获得粒径小、分散性好的纳米ATO粉体,是消除纳米ATO粉体的团聚的有效途径。

After antimony doped tin oxide（ATO）precursors were prepared by the sol-gel method,oven drying,microwave drying,vacuuming drying and supercritical fluid drying（SCFD）were used to treat the alcogels of ATO precursors.Weakly agglomerated nano-sized ATO particles with tetragonal phase structure were obtained after dry precursors were annealed at 600℃ under atmosphere.The nanoparticles were characterized by X-ray diffraction（XRD）,field emission scanning electron microscopy（FESEM）,transmission electron microscopy（TEM）and Malvern Zen1600 Zeta sizer.The results showed that ATO particles with tetragonal phase structure were all well crystallized from four drying processes.However,only the ATO powder prepared by SCFD consisted of primary particles weakly attached to each other,and the average size was around 25 nm.The mechanism was that the particles of precursors could keep loose morphology after treatment by SCFD,which was the key to preparing weekly agglomerated nano-sized ATO particles.In conclusion,it was an effective way to avoid the nano-sized ATO agglomeration by SCFD process in the sol-gel method.