Hierarchically ordered networks comprising crystalline ZrO2 tubes through sol–gel mineralization of eggshell membranes

Hierarchically ordered networks comprising crystalline ZrO2 tubes through sol–gel mineralization of eggshell membranes
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DOI:
10.1039/b301077e
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发表时间:
2003-04
影响因子:
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通讯作者:
Dong Yang;L. Qi;Jiming Ma
Dong Yang;L. Qi;Jiming Ma
中科院分区:
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文献类型:
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作者:
Dong Yang;L. Qi;Jiming Ma

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一种简单的溶胶-凝胶涂层方法成功地应用于蛋壳膜(ESM)的ZrO2涂层,得到了由结晶ZrO2管组成的大孔网状结构的分层有序薄膜。通过ESM模板的溶胶-凝胶矿化和随后的600℃煅烧得到这种分层材料,并通过XRD, SEM, TEM, HRTEM和氮吸附测量对其进行了表征。结果表明,该ZrO2材料的宏观形貌为厚度约为15µm的薄膜;膜的微观结构为直径小于1.0µm的ZrO2微管交织形成的大孔网络;管壁由四边形ZrO2纳米晶体组成,平均晶粒尺寸约为6 nm。它的比表面积为55 m2 g−1,BET平均孔径为7.0 nm,这主要是由于ZrO2纳米晶体构成了管壁。研究还表明,在700℃下煅烧初始ESM/锆前驱体杂化后,邻近的ZrO2管之间发生了明显的融合,同时氧化锆发生了四方向单斜的相变。
A facile sol–gel coating procedure has been successfully applied for the ZrO2 coating of eggshell membranes (ESM), resulting in hierarchically ordered thin films with a macroporous network structure comprising crystalline ZrO2 tubes. This hierarchical material, which was obtained through sol–gel mineralization of the ESM template and subsequent calcination at 600 °C, was characterized by XRD, SEM, TEM, HRTEM, and nitrogen sorption measurements. It has been shown that this ZrO2 material exhibits a macroscopic morphology of a film with a thickness about 15 µm; the film has a microstructure of macroporous networks composed of interwoven ZrO2 microtubes with diameters less than 1.0 µm; the tube walls consist of tetragonal ZrO2 nanocrystals with an average crystallite size about 6 nm. It shows a specific surface area of 55 m2 g−1 and a BET average pore size of 7.0 nm, which is mostly due to the ZrO2 nanocrystals constituting the tube walls. It has also been shown that calcination of the initial ESM/zirconium precursor hybrid at 700 °C resulted in significant fusion between neighboring ZrO2 tubes accompanying a tetragonal-to-monoclinic phase transformation of zirconia.