Fabrication and characterization of dense zirconia and zirconia-silica ceramic nanofibers.

Fabrication and characterization of dense zirconia and zirconia-silica ceramic nanofibers.
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DOI:
10.1166/jnn.2010.2441
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发表时间:
2010-09
影响因子:
--
通讯作者:
Fan Y
Fan Y
中科院分区:
工程技术4区
文献类型:
--
作者:
Xu X;Guo G;Fan Y

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本研究的目的是制备致密的氧化锆-氧化钇(ZY),氧化锆-二氧化硅(ZS)和氧化锆-氧化钇-二氧化硅(ZYS)纳米纤维作为牙科复合材料的增强元素。丙醇锆(IV)、六水合硝酸钇和正硅酸四乙酯(TEOS)被用作制备氧化锆、氧化钇和二氧化硅溶胶的前体。少量(1- 1.5wt%)的聚环氧乙烷(PEO)用作载体聚合物。在静电纺丝之前将溶胶在70 °C下预热,并且在不同加热时间下用粘度计测量它们的粘度。用粘度-时间(η-t)曲线测定凝胶点。采用特殊的反应静电纺丝装置,在凝胶点附近的条件下制备了ZY、ZS和ZYS凝胶纳米纤维。所制备的凝胶纳米纤维的直径在200和400 nm之间。通过在不同温度下的煅烧,获得了直径为100-300 nm的氧化锆-氧化钇(96/4)、氧化锆-二氧化硅(80/20)和氧化锆-氧化钇-二氧化硅(76.8/3.2/20)的致密(无孔)陶瓷纳米纤维。采用扫描电子显微镜(SEM)、高分辨场发射扫描电子显微镜(FE-SEM)、热重分析仪(TGA)、差示扫描量热仪(DSC)、傅里叶变换红外光谱仪(FT-IR)和X射线衍射仪(XRD)对凝胶和陶瓷纳米纤维进行了表征。SEM显微照片显示陶瓷ZY纳米纤维具有颗粒状结构,而陶瓷ZS和ZYS纳米纤维具有光滑的表面,在FE-SEM下均未显示出可见的孔隙。通过TGA/DSC和FT-IR证实了聚合物PEO的完全去除,通过XRD证实了氧化锆和无定形二氧化硅的四方相的形成。总之,致密的氧化锆基陶瓷纳米纤维可以使用新的反应溶胶-凝胶静电纺丝技术与最低的有机聚合物添加剂。
The objective of this study was to prepare dense zirconia-yttria (ZY), zirconia-silica (ZS) and zirconia-yttria-silica (ZYS) nanofibers as reinforcing elements for dental composites. Zirconium (IV) propoxide, yttrium nitrate hexahydrate, and tetraethyl orthosilicate (TEOS) were used as precursors for the preparation of zirconia, yttria, and silica sols. A small amount (1–1.5 wt%) of polyethylene oxide (PEO) was used as a carry polymer. The sols were preheated at 70 °C before electrospinning and their viscosity was measured with a viscometer at different heating time. The gel point was determined by viscosity–time (η–t) curve. The ZY, ZS and ZYS gel nanofibers were prepared using a special reactive electrospinning device under the conditions near the gel point. The as-prepared gel nanofibers had diameters between 200 and 400 nm. Dense (nonporous) ceramic nanofibers of zirconia-yttria (96/4), zirconia-silica (80/20) and zirconia-yttria-silica (76.8/3.2/20) with diameter of 100–300 nm were obtained by subsequent calcinations at different temperatures. The gel and ceramic nanofibers obtained were characterized by scanning electron microscope (SEM), high-resolution field-emission scanning electron microscope (FE-SEM), thermogravimetric analyzer (TGA), differential scanning calorimeter (DSC), Fourier transform infrared spectrometer (FT-IR), and X-ray diffraction (XRD). SEM micrograph revealed that ceramic ZY nanofibers had grained structure, while ceramic ZS and ZYS nanofibers had smooth surfaces, both showing no visible porosity under FE-SEM. Complete removal of the polymer PEO was confirmed by TGA/DSC and FT-IR. The formation of tetragonal phase of zirconia and amorphous silica was proved by XRD. In conclusion, dense zirconia-based ceramic nanofibers can be fabricated using the new reactive sol–gel electrospinning technology with minimum organic polymer additives.
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