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研究生:黃士瑋
研究生(外文):Shih-Wei Huang
論文名稱:Chitosan/磷酸鈣鹽複合材料微球之製備與特性分析
論文名稱(外文):Preparation and characterization of chitosan/calcium phosphate composite microspheres
指導教授:顏秀崗顏秀崗引用關係
指導教授(外文):Shiow-Kang Yen
學位類別:碩士
校院名稱:國立中興大學
系所名稱:材料科學與工程學系所
學門:工程學門
學類:綜合工程學類
論文種類:學術論文
畢業學年度:97
語文別:英文
論文頁數:36
中文關鍵詞:甲殼素氫氧基磷灰石磷酸鈣鹽微球
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.
CONCENTS
ABSTRACT ii
CONCENTS iii
TABLE CONTNETS iv
FIGUE CONTNETS v
1. INTRODUCTION 1
2. MATERIALS AND METHODS 4
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. RESULTS AND DISCUSSION 8
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
4. CONCLUSIONS 33
REFERENCES 34

TABLE CONTNETS
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

FIGUE CONTNETS
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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