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목차

Ⅰ. 서론 6

Ⅱ. 이론적 배경 10

Ⅱ-1. 생체세라믹스 (bioceramics) 10

Ⅱ-2. 수산화아파타이트 (hydroxyapatite; HA) 13

Ⅱ-3. 인산삼칼슘 (tri-calcium phosphate; TCP) 17

Ⅱ-4. 이상인산칼슘 (biphasic calcium phosphate; BCP) 20

Ⅱ-5. 인산칼슘계 세라믹스의 분해 특성 23

Ⅱ-6. 이상인산칼슘 (BCP)의 골 대체물 이용 25

Ⅲ. 실험방법 27

Ⅲ-1. BCP 분말의 제조 28

Ⅲ-1-1. 건식법 (Mechanically Mixed)을 이용한 BCP 분말의 준비 28

Ⅲ-1-2. 침전법 (Precipitation)을 이용한 BCP 분말의 제조 30

Ⅲ-2. 분석을 위한 시편 준비 32

Ⅲ-3. 생체적합성 실험 33

Ⅲ-3-1. 유사체액 (SBF; Simulated Body Fluid) 제조 33

Ⅲ-3-2. in-vitro 실험 34

Ⅲ-4. BCP 세라믹의 특성 조사 37

Ⅲ-4-1. BCP 분말의 특성 조사 37

Ⅲ-4-2. 중량변화 37

Ⅲ-4-3. X-선 회절 분석 37

Ⅲ-4-4. 유도결합 플라즈마(ICP) 방출 분광 분석 38

Ⅲ-4-5. SEM 관찰 38

Ⅲ-5. 세포 증식 및 분화 시험 분석 39

Ⅳ. 결과 및 고찰 40

Ⅳ-1. BCP 분말의 특성 조사 40

Ⅳ-1-1. Ca/P 비율에 따른 P-BCP 분말 분석 40

Ⅳ-1-2. 적외선 흡수 분광분석 장비에 의한 M-BCP, P-BCP 분말 분석 43

Ⅳ-1-3. 열 중량ㆍ시차열 분석 에 의한 M-BCP, P-BCP 분말 분석 45

Ⅳ-1-4. X-선 회절분석 (분말 분석) 47

Ⅳ-2. X-선 회절분석 (R-SBF 침적 전ㆍ후) 50

Ⅳ-3. 중량변화 52

Ⅳ-4. SEM 분석 54

Ⅳ-5. ICP 방출 분광분석 62

Ⅳ-6. 세포 증식 및 분화 시험 분석 65

Ⅴ. 결론 66

Ⅵ. 참고문헌 68

초록 72

표목차

Table 1. Various calcium phosphates with Ca/P ratio 9

Table 2. Type of tissue attachment and present use of bioceramics 12

Table 3. Elements of apatites (M10(ZO₄)6X₂) 13

Table 4. Methods for the synthesis of HA powder and their morphology 16

Table 5. Various companies manufacturing BCP products 26

Table 6. Chemicals and Their Purities and Amounts to Prepare 1000 mL of C-SBF and R-SBF 35

Table 7. Ion Concentrations of C-SBF and R-SBF calculated from the Amounts of Dissolved Chemicals, Compared with those Human Blood Plasma 36

Table 8. Relative densities of P-BCP & M-BCP specimens measured by Archimedes method 49

Table 9. Weight gain of M-BCP and P-BCP with immersion period (data obtained from the average value of 5 samples) 53

Table 10. The list of association/dissociation reactions in SBF 56

Table 11. Calcium and phosphorus ion concentration and pH of R-SBF as a function of soaking time 63

그림목차

Fig. 1 Hydroxyapatite structure. The numbers printed on the atom symbols are the Z co-ordinates. 15

Fig. 2 α-TCP unit cell (left) projected on the (a, b) plane, (right) projected onto the (b, c) plane. Tetrahedra represent PO₄ groups, and light balls denote Ca atoms 19

Fig. 3 β-TCP unit cell projected on the (a, c) plane. Tetrahedra represent PO4 groups, small balls designate Ca atoms, and big balls are for the Ca's with half occupancy 19

Fig. 4 XRD pattern of calcium deficient apatite 21

Fig. 5 Various shapes and forms of commercialized BCP 25

Fig. 6 BCP manufactured by Osteon 25

Fig. 7 Flow chart for the preparation and characterization of specimen 27

Fig. 8 Flow chart of mechanically mixed BCP preparation procedure 29

Fig. 9. Flow chart of chemically precipitated BCP preparation procedure 31

Fig. 10 XRD patterns of P-BCP heat treated at 900℃ for 1 hour with different Ca/P ratio during precipitation 41

Fig. 11 XRD pattern of mixed commercial HA and TCP powders (before ball milling) 42

Fig. 12 XRD pattern of chemically precipitated BCP (calcined at 900℃ for 1 hour; Ca/P=1.55) 42

Fig. 13 FT-IR spectra of M-BCP powder before sintering 44

Fig. 14 FT-IR spectra of calcined P-BCP powder 44

Fig. 15 TG/DTA evolution curves for M-BCP powder before sintering 46

Fig. 16 TG/DTA evolution curves for P-BCP powder before sintering 46

Fig. 17 XRD patterns of M-BCP specimens heated at 1000, 1100, 1200 and 1300℃ for 2 hours, respectively 48

Fig. 18 XRD patterns of P-BCP specimens heated at 1000, 1100, 1200 and 1300℃ for 2 hours, respectively 48

Fig. 19 Experimental curves of relative densities for P-BCP & M-BCP specimens measured by Archimedes method 49

Fig. 20 XRD patterns of mechanically mixed BCP specimens ; unsoaked and soaked for 1, 7, 21 days, respectively 51

Fig. 21 XRD patterns of chemically precipitated BCP specimens ; unsoaked and soaked for 1, 7, 21 days, respectively 51

Fig. 22 Curves represent weight gain of M-BCP and P-BCP with immersion period 52

Fig. 23 Schematic presentations of the origin of negative charge on the HA surface and the process of bonelike apatite formation thereon in SBF 55

Fig. 24. Surface morphology of M-BCP specimens before soaking (L : 500, R : 5000) 57

Fig. 25. Surface morphology of P-BCP specimens before soaking (L : 500, R : 5000) 57

Fig. 26. Surface morphology of M-BCP specimens soaked in R-SBF for 7 days (L : 500, R : 5000) 58

Fig. 27. Surface morphology of P-BCP specimens soaked in R-SBF for 7 days (L : 500, R : 5000) 58

Fig. 28. Surface morphology of M-BCP specimens soaked in R-SBF for 21 days (L : 500, R : 5000) 59

Fig. 29. Surface morphology of P-BCP specimens soaked in R-SBF for 21 days (L : 500, R : 5000) 59

Fig. 30. Surface morphology of M-BCP specimens soaked in R-SBF during 1, 3, 6, 12, 18 and 24 hours 60

Fig. 31. Surface morphology of P-BCP specimens soaked in R-SBF during 1, 3, 6, 12, 18 and 24 hours 61

Fig. 32 Calcium ion concentration and pH of R-SBF as a function of soaking time 64

Fig. 33 Phosphorus ion concentration and pH of R-SBF as a function of soaking time 64

Fig. 34 Comparison of M-BCP, P-BCP, and control (culture plate) in terms of cell proliferation after 1 day cell culture 65

Fig. 35 ALP Staining results; left: M-BCP, right: P-BCP (200x) after 7 days. Red color showed ALP positive cells response 65