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研究生(外文):Shih-Wei Huang
論文名稱(外文):Preparation and characterization of chitosan/calcium phosphate composite microspheres
指導教授(外文):Shiow-Kang Yen
外文關鍵詞:chitosanhydroxyapatitecalcium phosphatemicrosphere
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本研究利用水熱法成功的合成了多孔性磷酸鈣/chitosan的複合微球,chitosan會形成一個螯合劑來幫助磷酸鈣鹽成長,而多孔複合微球的結構跟化學鍵則利用掃描式電子顯微鏡、穿透式電子顯微鏡、X射線繞射儀、傅立葉轉換紅外線光譜儀、比表面與孔隙度分析儀、熱重分析儀、熱差分析儀來做分析。分析的結果指出本研究所合成出來的多孔性複合微球具有 38.16 m2/g 的比表面積,孔隙大小由4~100 nm,微孔及介孔比體積為0.24 cm3/g。因本研究所合成出來的多孔性複合微球具有著chitosan的特徵及良好的孔隙度,因此可以做來用藥劑或觸媒的載體,以及可注射骨粉等用途。
The porous calcium phosphate/chitosan composite microspheres could have been successfully synthesized in Ca(NO3)2•4H2O, NH4H2PO4, and chitosan cantained aqueous solution by using hydrothermal method. Chitosan could be a chelating agent for the nucleation of CaP. The microstructure and chemical bonding of the microspheres were characterized by using scanning electron microscopy (SEM), X-ray diffractometry (XRD), transmission electron microscopy (TEM), FT-IR spectrometer, and specific surface area/porosimetry & chemisorption analyzer. The porous microphres exhibit a specific surface area 38.16 m2/g, pore size from 4~100nm, and pore volume 0.24 cm3/g. Because this composite microsphere has chitosan character and also has great porosity. They could be considered as drugs or catalysts carriers, and injectable powders of bone graft.
2-1 Materials 4
2-2 Synthesis porous calcium phosphate microsphere 4
2-3 Characterization of powder analysis 4
2-3-1 Field emission scanning electron microscopy analysis 4
2-3-2 Fourier transform infrared spectroscopy analysis 5
2-3-3 X-ray diffration analysis 5
2-3-4 Specific surface area/porosimetry & chemisorption analysis 5
2-3-5 Transmission electron microscopy analysis 5
2-3-6 Inductive coupled plasma mass spectrometry analysis 6
2-4 Heat analysis 6
3-1 Crystal structure and phase transformation 8
3-2 Chemical bondings and composites 19
3-3 Surface morphology, specific surface area, and pore volume 23
3-4 Drug loading and release 31

Table 1 The elements of EDS analysis 21
Table 2 ICP-MS of element analysis 22
Table 3 BET analysis of surface area, pore volume, and pore size 30

Fig. 1 chitosan structure 3
Fig. 2 Experiment of flow chart 7
Fig. 3 The XRD diagrams of calcium phosphate/chitosan composite microsphere 9
Fig. 6 TEM image of the microsphere 12
Fig. 7 SADP of the composite material 12
Fig. 8 TEM image of the 500°C microsphere (a)x50k (b) dark field (c)x100k (d) SADP 13
Fig. 9 TEM image of the 700°C microsphere (a)x50k (b) dark field (c)x100k (d) SADP 14
Fig. 10 TGA/DSC diagrams of Chitosan in air 16
Fig. 11 TGA/DSC diagrams of Chitosan in N2 16
Fig. 12 TGA/DSC diagrams of CCaP in air 17
Fig. 13 TGA/DSC diagrams of CCaP in N2 17
Fig. 14 TGA/DSC diagrams of HA in air 18
Fig. 15 TGA/DSC diagrams of HA in N2 18
Fig. 16 The FTIR spectra of chitosan, HA, and our prepared calcium phosphate/chitosan composite microsphere (CCaP) 20
Fig. 18 Morphology of chitosan/calcium phosphate composite microspheres 23
Fig. 19 Morphology of 150°C chitosan/calcium phosphate composite microspheres 24
Fig. 20 Morphology of 300°C chitosan/calcium phosphate composite microspheres 25
Fig. 21 Morphology of 500°C chitosan/calcium phosphate composite microspheres 26
Fig. 22 Morphology of 700°C chitosan/calcium phosphate composite microspheres 27
Fig. 23 BET nitrogen adsorption/desorption isotherm 29
Fig. 24 Four type typical hysteresis loops 29
Fig. 25 BJH desorption pore 30
Fig. 26 The in-vitro drug release from CCaP composite microsphere 32
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