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1 Jurnal f the Krean Ceramic Sciety Vl. 7, N., pp. 17~11, 010. DOI:10.191/KCERS Bimimetic Apatite Precipitated n the Surface f Titanium Pwder Jng Hee Kim,G Yung Uk Sim, Tae Yung Yang, Seg Yung Yn, and Hng Chae Park Schl f Materials Science and Engineering, Pusan Natinal University, Pusan , Krea (Received Octber 19, 009; Revised December 18, 009; Accepted January 11, 009) pk t qk p ½ Á Á k Á Á y w œw ( ; ; ) ABSTRACT Bimimetic whisker-like apatite was frmed n thermally and NaOH-treated titanium pwder in a simulated bdy fluid (SBF). In the early prcess f the SBF immersin, the surface structure f the titanium pwder was lsened, pssibly due t the disslutin f Na ins n the surface f the titanium pwder int SBF. When immersed fr 7 days in SBF, fine precipitates appeared n the titanium surfaces; the cating layer (<00 nm in thickness) cnsisted f nanstructured, amrphus whisker-like and particulate phase, bserved by TEM. With the extensin f the immersin time t 16 days, the chrysanthemum flwer type mrphlgy f carbnated hydrxyapatite with a nancrystallinity was develped n the surface f the titanium pwder. Key wrds : Bimimetic apatite catings, Titanium pwder, Simulated bdy fluid, Whisker-like nanstructured crystals 1. kk w (Ti6AlV) w», ey, ü w w ww v p. ù 1,) w y ü w w., qk p y w (stecnductivity) ùk üù» ƒ w. pk w,) w y gq qk p w». pk w w w j» w plasma spraying 9,10) 5,6), sl-gel 7,8), electrphresis, electrchemical depsitin sww ƒ y gq». plasma spraying» pk»q y qk p(hydrxyapatite, HA) gq w š. ù» š œ w gq HA w vw š, 5) Crrespnding authr : Hng-Chae Park hcpark1@pusan.ac.kr Tel : Fax : »q g q d w w w w x v p ³ w gq ww w. 11) wr, (simulated bdy fluid, SBF) w gqœ pk»q q k p(bne-like apatite) t d j» w jš. 1-15) SBF ü yw pk t qk p w š Ca P w wš, ³ w gq d w. qk p w, pk x t, SBF, SBF ü e œ w. ¾ ww š pk qk p gq w q xk(flat-shaped)»q wš. pk w qk p gq wš g q e SBF ü e w mw pk w p w jš w. w y qk p gq pk e,, œ œ w w». 17

2 김종희 심영욱 양태영 윤석영 박홍채 18. 실험순서 순도 99.75%, 응집입자의 크기 1.6 µm (<50%)을 갖 는 상용 티타늄분말(Sigma-Aldrich)을 출발물질로 사용하 였다. 티타늄분말을 에탄올과 탈이온 증류수를 사용하여 초음파세척, 50 C에서 건조한 후 공기 중에서 600 C, 시 간 가열하였다. 이어서 하소분말을 5M NaOH 수용액 (60 C) 내에서 시간 반응, 여과, 증류수로 수세, 100 C에서 건 조하였다. NaOH 수용액으로 처리한 티타늄분말을 1.0 Na, 5.0 K, 1.5 Mg,.5 Ca, 18.8 Cl,. HCO, 1.0 HPO, 0.5 SO 의 이온농도 (mm)를 갖는 SBF (6.5 C) 중에서 1-16일 동안 침적시켰다. NaCl, NaHCO, KCl, K HPO H O, MgCl 6H O, CaCl, Na SO 시약을 증류수에 용해 시킨 후, 최종적으로 tris-hydrxymethyl aminmethane (TRIS) 와 HCl을 이용하여 6.5 C에서 ph=7.를 갖는 SBF 용액 을 제조하였다. 코칭 층의 표면성상을 관찰하기 위하여 주사전자현미경 (SEM, Hitachi S-00, Hitachi) 및 투과전자현미경 (TEM, JEM-010, Jel)을 이용하여 하였다. 화학 및 결정상의 조 성을 조사하기 위하여 X-선회절분석기 (XRD, D/MAX00, Rigaku) 및 적외선분광분석장치 (FTIR, Bruker IFS-66, Bruker)를 이용하였다. 코팅물질의 원소 및 표면화학을 조 사하기 위하여 에너지 분산 X-선미세분석기 (EDX) 및 X선광전분광기 (XPS, ESCALAB50, VG Scientific)를 이용 하였다. XPS에서 측정된 결합에너지는 8.6 ev의 탄화 수소 C1s에 의하여 보정되었다 Fig. 1.. 결과 및 고찰 출발물질로 사용한 티타늄분말 및 NaOH 수용액으로 처리한 시료의 X-선 회절패턴을 Fig. 1에 나타내었다. 시 료분말에서 금속 티타늄의 공기 중 가열에 의한 부분적 인 표면산화로 인하여 생성된 rutile (TiO ) (JCPDS Card #0-051)의 약한 회절피크가 출현하였다. 이러한 비정질 또는 미결정의 산화피막은 NaOH 수용액에서 Na O-TiO 표면층의 생성을 가속화시키고 따라서 SBF중에서 Ti-OH grup의 유도를 보다 용이하게 함으로써 아파타이트의 생 성을 향상시킬 수 있을 것이다(Fig. ). Fig. 은 SBF내에서 일정시간 침적시킨 시료분말의 SEM 사진을 보여준다. 5일까지 침적할 동안 티타늄분말의 표 면구조는 SBF중의 H O 이온과의 상호교환에 따른 분말 의 표면으로부터 Na 이온의 용해로 인하여 현저히 이완 되었으며, 석출물의 생성흔적을 거의 관찰할 수 없었다. 그러나 침적시간을 7일까지 연장함에 따라서 이완되어진 분말의 표면위에서 미세한 석출물의 생성이 확인되었다. TEM 관찰 및 micrbeam diffractin patterns의 분석으로부 - 한국세라믹학회지 Fig.. XRD patterns f as-received titanium pwder (a), and titanium pwder saked in NaOH aqueus slutin fr h withut (b) and with (c) preliminarily heating at 600C fr 1 h in air. SEM micrgraphs f titanium pwder after saking in SBF fr 16 days: (a) thermally and NaOH-treated sample, and (b) nly NaOH-treated. 터 비정질 나노구조를 갖는 휘스커와 입자상으로 구성된 코팅 층 (<00 nm)의 생성을 확인할 수 있었다 (Fig. ). 16 일간 침적 시, 반응생성물의 존재가 시료표면의 거의 전 영역에 걸쳐서 관찰되었으며, 이는 chrysanthemum flwer type mrphlgy와 ellipsidal particle shaped precipitates (lng rice-like grains)로 구성되어져 있었다. 이러한 미세 구조의 발달은 티타늄 판상기판의 표면위에서 SBF와의 초기반응에서 생성되는 전형적인 islated spherical cap의 mrphlgy 와 확연히 구별된다. 티타늄분말에서의 이러 한 미세구조의 발달은 첫째, 굴곡을 갖는 티타늄분말의 비교적 큰 표면적은 판상과 비교하여 SBF내에서 아파타 이트의 생성을 위한 풍부한 핵생성자리를 공급할 수 있 으며, 둘째, 티타늄입자에서의 핵생성 시 핵과 기물사이의 접촉면적은 충분히 작기 때문에 우선 배향성성장이 가능 하며, 셋째, 아파타이트의 결정구조는 육방정단위정 (a=0.91 nm, c=0.689 nm)을 가지므로 다른 결정축에 비하 여 c-축에 평형한 결정학적 방향을 따라서 결정성장이 보 다 용이하다는 것 등에 기인하는 것으로 생각된다. 이러한 16)

3 티타늄분말의 표면에 석출된 생체모방 아파타이트 Fig.. Fig.. 19 SEM micrgraphs f the surfaces f the titanium pwder after saking in SBF fr (a) 1, (b), (c) 5, (d) 7, and (e, f) 16 days. (a) TEM micrgraph f the surface f the titanium pwder after saking in SBF fr 7 days and (b) SAD patterns n the cating layer. 미세구조는 α-tricalcium phsphate의 가수분해에 의한 whisker-like HA 생성의 중간과정에서 흔히 나타난다. 또한, SEM 사진 (Fig. )에서 볼 수 있는 바와 같이 시료 표면위의 핵생성이 보다 용이한 자리에서 다핵이 생성되 어 서로 인접하면서 성장하는 것을 알 수 있다. SBF내에서 7일 및 16일 침적한 후 생성된 석출물에 대 한 EDX 분석 (Fig. 5)은 시료표면에서 Ti 이외에 C, O, Na, P, Ca의 존재를 보여주었다. NaOH 수용액처리 후 증 류수를 이용한 수세에도 불구하고 소량의 Na 이온이 잔 존하는 것으로 생각된다. Ca/P atmic rati는 CHA의 양 론조성 (.)과 비슷한.7와.96을 각각 나타내었다. 이 경우 침적시간이 16일로 증가할 때 다소간의 Ca 이온이 티타늄분말의 표면에 존재하는 것으로 생각된다. SBF에 16일간 침적한 시료의 FTIR spectrum은 주로 17,18) Fig. 5. EDX spectra f the surfaces f the titanium pwder saked in SBF fr (a) 7 and (b) 16 days. Full scale: (a) 7 and (b) 996 cts. adsrptin band와 공존하는 H O, PO 를 나타내었 으며(Fig. 6), 이는 문헌 에 보고된 carbnated HA (CHA) 의 그것과 기본적으로 유사하였다. 5 cm 에서의 강한 adsrptin band와 161 cm 에서의 stretching band는 SBF에서 처리된 시료표면에 존재하는 H O에 기인한다. CO ) 1 1 제 7 권 제 호(010)

4 10 ½ Á Á k Á Á y Fig. 6. XPS spectra f (a) XPS survey, (b) Tip, (c) Cap, and (d) Pp f the surface f the titanium pwder saked in SBF fr 16 days. Fig. 7. FTIR spectrum f the titanium pwder after saking in SBF fr 16 days cm e stretching mde w 760, 69, 60, 59, 7 cm 1 - PO bands y w. 0,1) - w, FTIR spectrum CHAü ƒ CO adsrptin bandsƒ 100~1550 cm ~950 cm - xw. qk p CO grup w OH grups ey w cm 1 OH - stretch band y. SBF 16 e w XPS spectra Fig. 7 ùkü. gq d t C, Ca, O, P Ti ƒ. Tip / Tip 1/ w (binding energy)ƒ ƒƒ ev ùkû, ƒ y k (quardrivalent xidatin state), Ti w w. Cap spectrum Ca w w Cap / (.9 ev) Cap 1/ (6. ev). Pp spectrum 5 P ùkü 10.1 ev vj ùkü. w Cap Pp w š19,) CHA w.. w, yw pk t ù { f x w wz

5 qk p gq. SBFü e gq,, w. 7 e, ù w gq d ( Ì <00 nm). 16 ¾ e ƒ» t y x mrphlgy ùkü., pk t t w t w w œ, w w» w w, qk p w p ( ) w w w w w whisker-like phase j. XPS, FTIR, carbnated hydrxyapatite. EDX w 7, 16 e z Ca/P mlar rati ƒƒ Acknwledgment w w ( ) w REFERENCES 1. M. Lng and H. J. Rack, Titanium Ally in Ttal Jint Replacement-A Materials Science Perspective, Bimaterials, (1998).. X. Y. Liu, K. C. Paul, and C. X. Ding, Surface Mdificatin f Titanium, Titanium Allys, and Related Materials fr Bimedical Applicatins, Mater. Sci. Eng. R, (00).. M. Wang, Develping Biactive Cmpsite Materials fr Tissue Replacement, Bimaterials, 1-51 (00).. M. G. V. Jse, S. Eduard, P. T. Antni, O. Take, S. Katsuaki, W. M. Graysn, and J. M. Sally, Nvel Biactive Functinally Graded Catings n Ti6AlV, Adv. Mater., (000). 5. C. F. Feng, K. A. Khr, E. I. Liu, and P. Cheang, Phase Transfrmatins in Plasma Sprayed Hydrxyapatite Catings, Scripta. Mater., 10-9 (000). 6. X. B. Zheng, M. H. Huang, and C. X. Ding, Bnd Strength f Plasma-sprayed Hydrxyapatite/Ti Cmpsite Catings, Bimaterials, (000). 7. M. F. Hsieh, L. H. Perng, and T. S. Chin, Hydrxyapatite Cating n Ti6AlV Ally Using a Sl-gel Derived Precursr, Mater. Chem. Phys., (00). 8. E. Milella, F. Csentin, A. Licciulli, and C. Massar, Preparatin and Characterisatin f Titania/Hydrxyapatite pk t qk p 11 Cmpsite Catings Obtained by Sl-gel Prcess, Bimaterials, 15-1 (001). 9. X. L. Cheng, M. Filiagg, and S. G. Rsce, Electrchemically Assisted C-precipitatin f Prtein with Calcium Phsphate Catings n Titanium Ally, Bimaterials, (00). 10. M. Shirkhanzadeh, Calcium Phsphate Catings Prepared by Electrcrystallizatin frm Aqueus Electrilytes, J. Mater. Sci. Mater. Med., (1995). 11. K. de Grt, H. B. Wen, Y. Liu, P. Layrlle, and F. Barrere, Bimimetic Catings n Orthpedic Implants: a Review ; pp in Mineralizatin in natural and synthetic bimaterials. Ed. by P. Li, P. Calvert, T. Kkub, R. Levy and C. Scheid and P. A. Warrendalc, Materials Research Sciety, Warrendale, T. Kkub, H. Kushitani, S. Sakka, T. Kitsugi, and T. Yamamur, Slutins Able t Reptduce in Viv Surface-structure Changes in Biactive Glass-ceramics A-W, J. Bimed. Mater. Res., 71- (1990). 1. H. Takadama, H. M. Kim, T. Kkub, and T. Nakamura, TEM-EDX Study f Mechanism f Bne-like Apatite Frmatin n Biactive Titanium Metal in Simulated Bdy Fluid, J. Bimed. Mater. Res., (001). 1. T. Kkub, F. Miyaji, and H. M. Kim, Spntaneus Frmatin f Bnelike Apatite Layer n Chemically Treated Titanium Metals, J. Am. Ceram. Sc., (1996). 15. T. Kkub, Frmatin f Bilgically Active Bne-like Apatite n Metals and Plymers by a Bimimetic Prcess, Thermchim. Acta., 80/ (1996). 16. H. M. Kim, Biactive Ceramics: Challenges and Perspectives, J. Ceram. Sc. Jap., 109 S9-57 (001). 17. S. Y. Yn, Y. M. Park, S. S. Park, R. Stevens, and H. C. Park, Synthesis f Hydrxyapatite Whiskers by Hydrlysis f Alpha Tricalcium Phsphate Using Micrwave Heating, Mater. Chem. Phys., (005). 18. Y. M. Park, S. C. Ryu, S. Y. Yn, R. Stevens, and H. C. Park, Preparatin f Whisker-shaped Hydrxyapatite/Beta Tricalcium Phsphate Cmpsite, Mater. Chem. Chem., (008). 19. D. Wei, Y. Zhu, D. Jia, and Y. Wang, Bimimetic Apatite Depsited n Micrarc Oxidized Anatase-based Ceramic Cating, Ceram. Inter., 119- (008). 0. S. Kutspuls, Synthesis and Charcaterizatin f Hydrxyapatite Crystals: A Review Study n the Analytical Methds, J. Bimed. Mater. Res., (00). 1. M. Lenka and A. M. Frank, Preparatin f SBF with different HCO- cntent and its Influence n the Cmpsitin f Bimimetic Apatites, Acta. Bimater., (006).. W. H. Sng, Y. K. Jun, Y. Han, and S. H. Hng, Bimimetic Apatite Catings n Micr-arc Oxidized Titania, Bimaterials, (00). 7«y(010)

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