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1 Jurnal f the Krean Ceramic Sciety Vl. 47, N., pp. 244~248, DOI: /KCERS Fabricatin f Prus Calcium Phsphate by Using a Pre-Frm f Nature Material Sang-Jin Lee and Hn-Chel Lee Department f Advanced Materials Science and Engineering, Mkp Natinal University, Muan , Krea (Received March 19, 2010; Revised May 9, 2010; Accepted May 10, 2010) y w œ e Á z s w œw ( ; ; ) ABSTRACT Prus calcium phsphates were successfully fabricated by using a cuttlefish bne. The cuttlefish bne, which is cmpsed f CaCO, shwed a special prus micrstructure cntaining unifrm-sized vids. In this study, the pre-frms infiltrated distilled phsphric acid were sintered at 1200 C in an air atmsphere. The prus micrstructure f the pre-frms was kept their riginal pattern after sintering with a synthesis f calcium phsphate. The btained prus calcium phsphate, sintered at 1200 C fr h at 17% cncentratin f phsphric acid, shwed unifrm pen pres f 150 µm in size and β-tcp phase in the XRD patterns. Abve 16% cncentratin, CaO phase, derived frm the decmpsitin f CaCO, decreased gradually in the sintered samples, and the measured Ca/P ratis f the samples prepared frm 16% and 18% cncentratin were 1.67 and 1.4, which are clse t stichimetric HA (1.66) and β-tcp (1.50). Key wrds : Cuttlefish bne, Calcium phsphate, Phsphric acid, Prus micrstructure 1. w k wš, w, ey w, ww w» w ƒ y w š. 1-5) w tricalcium phsphate (Ca (PO 4 ) 2, w TCP w) hydrxyapatite (Ca 10 (PO 4 ) 6 (OH) 2, w HP w) ù ey w w š. 6-9) β-tcp HP e w š š j w, ù CaO 2 ù w w ) w w œ yw w e w j»»œ sww œ x, w»œj» mw wš. 1-15) Crrespnding authr : Sang-Jin Lee lee@mkp.ac.kr Tel : Fax : Ë ù ŠË w e w œ w ƒ w š, 17-19) ey ƒ g y xƒš. w k e w e y š, w wù w e w w ƒ w. 20) x w p w w, ey e œ œ w w. e œ w w œ x œ, p w œ y w w œ w w. w œ w œ en g xw, mw yw, œ w œ p š w. 2. x 2.1. œ w e, f l ü 244

2 자연물의 미세구조를 활용한 다공성 인산칼슘 제조 245 준비된 인산 (HPO4, reagent grade, Duksan Pure Chemical C., Ltd. Ansan, Krea)과 이소프로필 알코올의 혼합액에 담근 후, 데시케이터를 약 10분간 진공상태로 유지하였다. 이 때 인산과 이소프로필 알코올의 혼합비는 예비실험 결 과에 의하여, 인산칼슘이 합성되며 다공체 조직이 크게 변형되지 않는 범위로서, 인산의 농도를 12%~20%까지 변화시켰다. 다공성의 갑오징어 뼈 내부로 희석된 인산용 액이 침투되어 들어가고, 이 후 용액 내에 가라 앉은 갑 오징어 뼈를 건조기에서 24시간 동안 건조시켰다. 건조된 갑오징어 뼈는 공기분위기에서 분당 4 C/min의 승온속도 로 1200 C까지 열처리 하였다. 비교실험을 위하여 건조된 갑오징어 뼈를 온도 별로 공기 중에서 하소하여, 상변화 거동을 살펴보았다. 특성분석 농도 별로 인산을 침투시킨 갑오징어 뼈의 열처리에 따 른 결정상 분석을 위하여 X-ray diffractmeter (Rigaku D/ MAX 2200, Japan)를 사용하였으며, CuKα 특성 X선 파장 을 이용하여 40 kv, 0 ma의 조건하에서 분석을 실시하였 다. 갑오징어 뼈의 하소 전 후의 미세구조와 합성된 인산 칼슘 다공체의 미세구조 분석은 주사 전자 현미경(S-500N, Hitachi, Japan)을 사용하여 Au-Pd sputter로 코팅한 후 관찰 하였다. 열처리 된 다공체의 각 인산농도에 따른 Ca/P rati 는 ICP AES (spectrflame EOF, spectr analysis Inc., USA)를 이용하여 화학분석에 의해 측정하였다 결과 및 고찰 Fig. 1. SEM micrgraphs f (a) verall raw cuttlefish bne and (b) surface f a pillar. 갑오징어 뼈의 미세구조를 하소 전과 후로 나누어 Figs. 1과 2에 나타내었다. 하소 전의 갑오징어 뼈 (Fig. 1)는 매 우 특이한 다공성의 미세구조를 보였다. 규칙적인 층상구 조에 직각방향으로 수 많은 기둥들이 나열되어 있는 비 교적 규칙적인 다공성 구조로 높이 200 µm, 폭 50 µm의 반복되는 기공이 층을 이루며 형성되어 있는 구조를 보 였다. 작은 기둥의 확대 사진 (Fig. 1(b))에서는 줄무늬의 형태가 반복되는 매우 치밀한 미세구조를 관찰할 수 있 었다. 그러나 800 C에서 하소 된 갑 오징어 뼈의 경우는 (Fig. 2) 특이한 다공성의 미세구조가 무너지고, 부드러운 분말의 응집체 형태를 나타내었다. 갑오징어 뼈의 하소에 의한 결정상의 변화를 Fig. 에 나타내었다. 하소 전의 갑오징어 뼈의 경우는 CaCO 의 피크가 관찰되었다. CaCO 결정상은 하소 시, 700 C까지 관찰되었으며, 800 C 이후로는 CaO 피크만이 관찰되었고, 그 이상의 온도에서도 CaO 피크만이 관찰됨을 확인하였 다. 즉 갑오징어 뼈는 인산칼슘 합성에 주요한 칼슘 성분 을 보유하고 있으면서 고유의 특이한 다공성 구조를 보 이고 있어, 재료의 미세구조를 그대로 활용하여 인산칼슘 Fig. 2. SEM micrgraph f cuttlefish bne calcined at 800C fr 1 h. 다공체의 제조에 활용 가능한 자연 재료임을 알 수 있었 다. 하소 후 층상의 다공성 구조가 파괴되는 것은, CaCO 의 분해에 의한 것으로 판단된다. 제 47 권 제 호(2010)

3 246 Á z Fig.. XRD patterns f calcined cuttlefish bne at (a) 600 C, (b) 700 C, (c) 800 C, (d) 900 C, and (e) 1000 C fr 1 h. Fig. 4. XRD patterns f heated (1200 C fr 1 h) prus cuttlefish bne infiltrated phsphric acid at each cncentratin. œ e w Fig. 4 ùkü. e w w, w v v g w w ü en w w. x ù e yw w, y Fig. 5. XRD patterns f prus cuttlefish bne infiltrated 17% cncentratin-phsphric acid, heated at 1200 C fr 1 h ~ h. g ƒ x w. w w w š w š j» w, CaCO w 700 C 6 w z, e w 1200 C 1 w. 18) XRD, 12% CaO HA β-tcpƒ. z ƒ ƒw CaO vj β-tcp vjƒ ƒ. 18% CaO vjƒ e, 20% β-tcp vj. ù, CaO v jƒ 20%, ƒ w œ ù œ xk x w. w k, CaOƒ w e œ w, 17% x w C, 17% w y Fig. 5 ùkü C y k, CaO w β-tcp. w r x. œ ü š w y w, w x w 1100 C 100 C¾ w ù, w œ ƒ yw 1200 C w xw., x w ƒ w, 18% 2 œ š, 16% z w w wz

4 자연물의 미세구조를 활용한 다공성 인산칼슘 제조 247 Ca/P Ratis at Each Phsphric Acid Cncentratin Cncentratin (%) Ca/P Rati Table 1. 공의 크기는 높이에는 변화가 없으나 폭이 더욱 증가되 어 약 100 µm의 크기를 나타내었다. 따라서 약 150 µm 크기의 열린 기공을 갖는 인산칼슘 다공체가 제조 되었 으며, 이것은 생체재료로 사용되는 기존의 다공성 인산칼 슘의 기공크기를 만족하는 크기라 볼 수 있다. 성형체의 용융이 발생하지 않는 샘플에서, CaO가 소량 존재하는 또 다른 열처리 및 농도 하에서의 샘플들도 이와 비슷한 미세구조가 관찰되었다. Fig. 6에서 보듯이 인산칼슘으로 합성된 다공체의 표면은 하소 전 갑오징어 뼈의 미세구 조 (Fig. 1(b))와는 달리 부분적으로 소결이 일어나 치밀 한 미세구조를 보이는 부분을 관찰할 수 있었으며, 이와 함께 소량의 기공이 혼재하는 미세구조를 보였다. 인산 농도에 따른 Ca/P rati를 Table 1에 나타내었다. 본 실험에서는 인산의 침투 후 열처리 전 다공체의 Ca/P rati와 합성 후의 Ca/P rati가 차이를 보이게 되는데, 이 것은 건조공정 시 발생하는 인산의 증발과 열처리 공정 시 CaCO 의 분해에 의한 무게변화에 기인한다고 생각된 다. 따라서 합성 후의 Ca/P rati를 화학분석을 통해 측정 하여, 인산의 농도에 따른 열처리 후 최종적으로 얻어지 는 Ca/P rati를 측정함으로써 화학양론 조성에 맞는 HA 와 β-tcp 분말의 합성여부를 고찰하였다. 인산의 농도가 12%에서 20%로 변화됨에 따라 Ca/P rati는 2.1에서 1.22로 측정되었다. 화학양론적인 HA와 β-tcp의 Ca/P rati가 각각 1.66과 1.50인 것을 감안할 때, 16%와 18% 인산농도 범위에서 인산칼슘이 합성될 가능성이 가장 높 다고 볼 수 있으며, 실제 XRD 결과 (Figs. 4 and 5)에서 도 16% 이상에서 CaO 피크가 감소되며, 인산칼슘 합성 이 증가되고 있음을 알 수 있었다. 본 연구에서 얻어진 HA와 β-tcp는 넓은 범위의 Ca/P rati에서 연속적으로 합성되었고, 16% 인산농도의 경우 Ca/P rati가 1.67을 보 여 1.66인 HA의 화학양론 조성에 가까우나, 실제 XRD 결과에서는 β-tcp가 주 피크로 관찰되는 결과를 보였다. 21) Fig. 6. SEM micrgraphs f prus cuttlefish bne infiltrated 17% cncentratin-phsphric acid, heated at 1200C fr h. CaO 피크가 관찰되었다. 17% 농도에서 시간 유지하여 제조된 인산칼슘 다공체 의 경우, 성형체의 용융현상 없이 처음의 형태을 유지하 였으며, 그 미세구조를 Fig. 6에 나타내었다. 전체적인 미 세구조를 볼 때, 하소 전 갑오징어 뼈의 미세구조 패턴을 양호하게 유지하고 있었으며, 반응에 의하여 각 층간 기 둥의 두께가 좀 더 증가되었음을 관찰 할 수 있었다. 기 4. 결 론 갑오징어 뼈의 독특한 미세구조를 활용하여 다공성의 인산칼슘을 제조하였다. 희석된 인산용액을 석회석 성분 의 갑오징어 뼈의 다공체 내로 침투시켜 열처리함으로써 제 47 권 제 호(2010)

5 248 Á z s³»œ 150 µm ³ w x e œ w, œ y. CaCO w w š w q w œ ƒ ƒ w, 17% w 1200 C, w CaOƒ w β-tcp w ƒ w. w œ Ca/P rati yw HA β-tcp w, w œ w e w ùkü. š w w œ e w ey w ú, w œ wš y w ƒ k q. w œ e ey l p mw, ü scaffld w ƒ wz w. Acknwledgment 2007w s w w ( ) w REFERENCES 1. J. B. Park and R. S. Lakes, Bimaterials An Intrductin; pp , Plenum Press, New Yrk, L. L. Hench, Biceramics, J. Am. Ceram. Sc., 81 [7] (1998).. S. R. Kim, Y. H. Kim, S. J. Jung, and D. H. Riu, Synthesis and Characterizatin f Silicn Substituted Hydrxyapatite, J. Kr. Ceram. Sc., 8 [12] (2001). 4. H. J. Kim, S. C. Chi, J. W. Sek, and R. Telle, Bne Cements in TTCP, DCPA, β-tcp and PHA System, J. Kr. Ceram. Sc., 9 [1] (2002). 5. L. H. Lee and J. S. Ha, Fabricatin and Prperties f Siactive Prus Ceramics fr Bne Substitutin, J. Kr. Ceram. Sc., 45 [10] (2008). 6. J. S. Chi, H. C. Park, and S. Y. Yn, Sr-cntaining Hydrxyapatite fr Bne Replacement, J. Kr. Ceram. Sc., 45 [10] (2008). 7. A. M. Gatti, D. Zaffe, and G. P. Pli, Behavir f Tricalcium Phsphate and Hydrxyapatite Granules in Sheep Bne Defects, Bimaterials, (1990). 8. N. O. Engin and A. C. Tas, Preparatin f Prus Ca 10 (PO 4 ) 6 (OH) 2 and β Ca (PO 4 ) 2 Biceramics, J. Am. Ceram. Sc., 8 [7] (2000). 9. H. S. Ryu, H. J. Yun, K. S. Hng, B. S. Chang, C. K. Lee, and S. S. Chung, An Imprvement in Sintering Prperty f b Tricalcium Phsphate by Additin f Calcium Pyrphsphate, Bimaterials, (2002). 10. A. Deptula, W. Lada, T. Olczak, A. Brell, C. Alvani, and A. Bartlme, Preparatin f Spherical Pwders f Hydrxyapatite by Sl-Gel Prcess, J. Nn-Cryst. Slids., (1992). 11. M. Yshimura, H. Suda, K. Okamt, and K. Iku, Hydrthermal Synthesis f Bicmpatible Whisker, J. Mater. Sci., 29 [1] (1994). 12. M. G. S. Murray, J. Wang, C. B. Pntn, and P. M. Marquis, An Imprvement in Prcessing f Hydrxyapatite Ceramics, J. Mater. Sci., 0 [12] (1995). 1. R. Famery, N. Richard, and P. Bch, Preparatin f α and β Tricalcium Phsphate Ceramics, With and Withut Magnesium Additin, Ceram. Int., (1994). 14. S. C. Liu and S. Y. Chen, Transfrmatin Mechanism f Different Chemically Precipitated Apatitic Precursrs int β-tricalcium Phsphate upn Calcinatins, Bimatcrials, (2002). 15. S. Jinawath and P. Sujaridwrakun, Fabricatin f Prus Calcium Phsphates, Mater. Sci. and Eng., C (2002). 16. D. M. Liu, Fabricatin and Characterizatin f Prus Hydrxyapatite Granules, Bimatcrials, (1996). 17. M. D. Kwn, S. H. Oh, and S. J. Lee, Snthesis f β-tricalcium Phsphate by Using an Eggshell, J. Kr. Ceram. Sc., 9 [11] (2002). 18. S. J. Lee, Y. S. Yn, M. H. Lee, and N. S. Oh, Highly Sinterable Beta-Tricalcium Phsphate Synthesized frm Eggshell, Mater. Lett., (2007). 19. S. J. Lee, Y. S. Yn, M. H. Lee, and N. S. Oh, Nansized Hydrxyapatite Pwder Synthesized frm Eggshell and Phsphric Acid, J. Nanscience and Nantechnlgy, 7 [11] (2007). 20. S. J. Lee, Y. C. Lee, and Y. S. Yn, Characteristics f Calcium Phsphate Pwders Synthesized frm Cuttlefish Bne and Phsphric Acid, J. Ceram. Prc. Res., 8 [6] (2007). 21. M. Bhner, J. Lemaitre, A. P. Legrand, and P. Belgrand Synthesis, X-ray Diffractin and Slid-State 1P Magic Angle Spinning NMR Study f β-tricalcium Orthphsphate, J. Mater. Sci: Mater. Med., 7 [7] (1996). w wz

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