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1 Bimaterials Research (2005) 9(3) : Bimaterials Research 7 The Krean Sciety fr Bimaterials» w Hydrxyapatite (HA) gq w A Study f Hydrxyapatite (HA) Cating by Electrstatic Spray Depsitin 1 Áùx 2 Á½z 2 Á 2 Áy 1 Á 2 * Chang-Sup Byun 1, Nak-Hyun Oh 2, Yung-Hn Kim 2, Yen-Wk Chen 2, Sang-H Lee 1, and Wnhee Lee 2 * 1 ŠŠ Š gš, 2 iš Š gš 1 Department f Materials Engineering, Hanbat University, Taejn , Krea 2 Department f Advanced Materials Engineering, Sejng University, Seul , Krea (Received August 8, 2005/Accepted August 16, 2005) Catings f hydrxyapatite (HA) n titanium substrate have been cnducted by electrstatic spray depsitin (EDS). Electrstatic spray depsited HA films n Ti were heat-treated (400~900) and their physical characteristics were investigated by Scanning Electrnic Micrscpy (SEM), X-ray Diffractmeter (XRD), and X-ray Phtelectrnic Spectrscpy (XPS). The precursr f slutin fr the HA cating by ESD was prepared by mixing f nan-sized HA pwder with ethyl alchl. As-depsited HA films were cnsisted f HA particles which were distributed unifrmly n the Ti substrate, shwing a prus structure. By heat treatment (400~900 C), less prus and crystalline HA films were frmed n Ti substrate. Majr surface elements n the heat treated HA samples were Ca and P in the frm f HA. It is cncluded that EDS can be applied t the frmatin f unifrm and crystalline HA films n Ti substrate. Key wrds: Electrstatic-spray-depsitin, Hydrxyapatite, Ti, Implant d Œ fš f tf f tš h f ŽŠ f Š j tf g Š Œ lš f. 1,2) tfd g Ti Ti Š, lz f tœ gf f. f g 3) fd Œ ~fƒ t e f tœ g tf g fd f. fj 4) gf Ti Ti Šf h ƒf dš } Šjf g j t xœf g dš x hœd d f gf. Ti 5-8) Ti Šf txœf dš tœ g h f erf fl f ŒŠh Š fš Œf h hf ešl Šf xef h f h f. Ti 9,10) Ti Šf tœf f eš s ŠdŠ fhf f d f hydrxyapatite (HA) z f. 11) HA fx ŒŠ(Ca 10 (PO 4 ) 6 (OH) 2 ) f xf jdf tœf h ff~ *sfhf: whlee@sejng.ac.kr lh ŠŠ f h f f g Š f lš f. HA 12,13) il Šf dš ff Š } Šjf l Š hf lf. fš 14] hf ŠŠ eš tœ gf h } Ti Ti Š tœ gf HA z Š h tœf f f f l Šjf. 15,16) HA Ti Ti Š z Š j g h f f plasma spray, radi frequency(rf) magnetrn sputtering f f. 17) Plasma spray f l fdš HAf dfz fg, z Š f. ff f ŒŠ g hf ff HA Œ f t Šf dš g r HA z wf Ti dš f ii Š f g f hhf hf lh f. Š 18) RF magnetrn sputteringf hf h l hf f ff i d 19,20) fš z hf step cverage il f fš lrf Œ~ d hh f h f. 157
2 변창섭 오낙현 김영훈 천연욱 이상호 이원희 158 이에 본 연구에서는 비교적 공정제어가 쉽고, 단순하며, 설 치비가 저렴하고, 우수한 step cverage를 얻을 수 있는 정전 기분사 증착 (Electrstatic spray depsitin (ESD)) 장비를 사용하여 Ti 기판에 HA를 코팅한 후 각기 다른 열처리 조건 을 통해 코팅표면의 미세구조와 HA의 결정성 변화, 그리고 표 면과 계면의 화학적 결합을 관찰하였다. 21) 재료 및 방법 HA 증착용 기판은 cp Ti로 지름이 7 mm이고 두께가 0.6 mm인 디스크 형태로 표면을 매끄럽게 하기 위해 #400, #800, #1000, #1500 순으로 SiC 연마지를 이용하여 연마 하고 연마 후에는 오염물과 표면의 거칠기를 조절하기 위해 에 칭용액(100 ml 증류수, 3 ml 불산, 6 ml 질산)에 10초간 에칭 하고 증류수에서 5분간 초음파 세척 후 건조하였다. 증착용 선 구물질인 HA(0.3 g) 분말을 ethyl alchl(100 ml)에 교반하고 준비된 기판과 용액을 ESD장치에 설치하고 20분간 정전기분 사 증착(ESD)을 실시하였다. Figure 1은 ESD장치의 개략도를 보여주며, Table 1에 본 실험실에서 사용된 ESD장비의 공정변 수를 나타내었다. ESD 장치는 노즐에 높은 전압을 가하고 기 판은 접지시켜 노즐과 기판에 가해지는 강한 자기장을 이용하 여 pump에서 밀어주는 용액을 분사시켜 용매가 증발되면서 기판위에 코팅층을 형성하게 한다. 코팅된 시편들은 남아 있 을지도 모르는 용매를 증발시키기 위하여 건조기에서 약 2시 간 건조시킨 후 열처리 조건(400~900 C)에 맞추어 고진공로 (high vacuum furnace system)를 이용하여 5 10 trr의 진 공에서 열처리를 실시하였다. 열처리된 시편들은 SEM을 이용 하여 형성된 HA 코팅층 표면의 미세구조 및 코팅 패턴을 관 찰하였으며, XRD로 코팅층의 결정상을 조사하였다. 또한 XPS 를 이용하여 코팅층 표면의 구성원소 및 화학적 결합상태를 관 찰하였다. 14) -5 Figure 1. Schematic diagram f ESD. Table 1. ESD experimental cnditins Pwer 8 KV Bimaterials Research 2005 Nzzle/substrate distance 30 mm 결과 및 고찰 Figure 2는 정전기분사 증착 후 열처리 전의 HA 코팅층 표 면형상을 보여주고 있다. 그림에서 보는 바와 같이 약 30~50 nm 크기의 HA 분말들이 Ti 기판에 전체적으로 고르게 분사된 것을 볼 수 있다. 아울러 증착된 HA 코팅층 내에 다수의 기 공이 보이고 있고, 표면은 비교적 거칠고 다공성임을 짐작할 수 있다. Figure 3은 열처리 조건에 따른 HA 코팅층의 표면조직 변화 를 보여주고 있다. 일반적으로 열처리를 실시한 HA 코팅층 형 상은 Figure 2와 달리 기공도가 크게 감소한 미세구조를 나타내 고 있으며 아울러 HA 입자들이 서로 합체되어 커지는 것을 볼 수 있다. 800 C까지 열처리한 시편들의 경우 증착된 HA 입자 들이 서로 합체되어 커지는 양상은 동일하나 900 C의 열처리 에 의해 합체된 입자들은 서로 용융되어 기공이 거의 없는 매 우 치밀한 막으로 전환되었다. 또한 900 C의 열처리는 cp Ti의 상변태 온도(882)를 넘겨 Ti의 상변화가 있어났으며, HA가 열 분해하여 TCP(Tricalcium phsphate)와 같은 이차상이 Ti내부로 침투한 것처럼 보인다. 이로써 정전기분사 증착된 HA 코팅층의 열처리는 최소 900 C 이상의 온도가 필요함을 알 수 있다. Figure 4는 증착용 선구물질인 HA 분말과 Ti 기판에 대한 기본 XRD pattern을 보여주고 있다. HA의 주 peak은 25~35 C에서 나타나고, Ti의 주 peak는 35~45 C에서 나타 났다. 열처리 조건에 따른 시편의 XRD data를 Figure 5에 나타내었다. 일반적으로 모든 열처리시편에서 HA의 주요 peak 이 관찰되었으며 ESD장비를 이용하여 HA가 Ti 기판에 코팅된 것을 알 수 있다. 그러나 400~600 C에서 열처리를 시행한 시편의 경우 HA 회절 peak의 강도가 약하고 샤프하게 나오지 않은 것을 볼 수 있었다. 이는 Figure 2에서와 같이 선구용액 을 만들어 ESD를 이용하여 분사하였을 때 작은 알갱이 형태 의 HA가 400~600 C의 열처리에서는 서로 결합하거나 핵생 성이 있어나지 않아 결정성이 미약했기 때문이라 판단된다. Figure 2. SEM micrgraphs f as-depsited HA n Ti. Flw rate 10 ml/h Depsitin time 20 min Nzzle size N. 25
3 정전기분사 증착법을 이용한 Hydrxyapatite (HA) 코팅에 관한 연구 159 Figure 3. SEM micrgraphs f HA n Ti after heat treatment at 400C (a), 500C (b), 600C (c), 700C (d), 800C (e), and 900C (f). Figure 5. XRD patterns f a HA cating n Ti substrate after heat treatment at 400C (a), 500C (b), 600C (c), 700C (d), 800C (e), and 900C (f). scan spectra를 Figure 6에 나타내었고, 이것을 토대로 표면에 존재하는 원소를 확인할 수 있었다. HA의 주요 성분인 Ca과 P 그리고 C, O가 측정되었고 Ar sputtering을 2번(100씩) 행함으로써 표면구조를 좀더 자세히 분석할 수 있었다. Figure 7은 400~600 C에서 열처리를 행한 HA 코팅층에 대한 sputtering전후의 narrw scan을 나타낸 것이며 Ca는 온도별로 400 C, 500 C에서는 350.6~347.2 ev에서 600 C에서는 표면 에서 347.6~351 ev, 2번에 걸친 sputtering후에는 346.8~ ev의 binding energy 범위에서 주요 peak이 나타났다. P는 400 C과 500 C에서 주요 peak이 ev에서 나타나 나 600 C 표면에서는 ev에서 주요 peak이 나타나는 것을 볼 수 있는데 이는 온도가 올라가면서 HA분말들이 열분 해 하여 tricalcium phsphate(tcp)와 같은 원소로 전이됨을 알 수 있다. 그리고 2번에 걸친 sputtering 후에도 Ca, P의 성분이 나타나므로 코팅층의 두께는 최소 200Å 이상인 것을 + Figure 4. XRD patterns f precursr HA pwders (a) and Ti substrate (b). 반면, 700~900 C에서 열처리를 시행한 시편의 경우 HA 코 팅층의 입자가 서로 결합하고 소결되어 결정성을 이루며 400~600 C에서 보다는 회절 peak의 강도가 높고 sharp한 pattern을 얻을 수 있었으며 CaTiO 및 TiO 와 같은 산화피 막이 동시에 형성되는 것을 알 수 있었다. 0~800 ev의 binding energy 범위에서 측정된 XPS wide 3 2 Vl. 9, N. 3
4 160 변창섭 오낙현 김영훈 천연욱 이상호 이원희 Figure 6. XPS wide scan spectra f a HA cating after heat treatment at 400C (a), 500C (b), and 600C (c). Table 2. Elemental distributin f a HA cating after heat-treatment Element C 1s O 1s P 2p Ca 2p Ti 2p surface surface surface Figure 8. SEM micrgraphs f a HA cating n prus Ti implant. Figure 7. XPS narrw scan spectra f a HA cating after heat treat- ment at 400C (a), 500C (b), and 600C (c). 알 수 있다. Table 2에 정량된 성분의 원소량을 나타내었으며 sputtering을 할수록 탄소의 양은 전체적으로 줄어들고 Ca, P 의 양은 전체적으로 늘어나는 것을 볼 수 있다. 이와 같은 현상은 대기 중에서 흡착된 탄소 원자가 sputtering을 통하여 제거 됨으로써 P와 Ca 성분이 상대적으로 표면에 더 많이 Bimaterials Research 2005 노출되었기 때문이다. Figure 8은 본 연구에서 사용된 실험조건을 이용하여 HA가 코팅된 다공성 임플란트의 표면향상을 보여주고 있다. 그림에 서 보는 바와 같이 정전기분사 증착에 의해 다공성 구조를 갖 는 Ti 기판에 HA가 기공 내부까지 균일하게 증착된 것을 알 수 있다. 이는 정전기분사 증착이 기존에 사용되는 증착법의 한계인 step cverage의 문제점을 해결해줄 수 있는 새로운 공정법이 될 수 있는 가능성을 시사해주고 있다. 본 연구를 통해 ESD 장비를 이용하여 Ti 기판에 결정성 HA의 코팅 가능성을 확인 할 수 있었으며 코팅층의 기계적 특 성 및 계면과의 반응성에 관한 추후 연구가 수행될 예정이다. 결 론 본 연구는 생체이식 재료에 있어 생체불활성 재료인 Ti 기판
5 hh lrf fdš Hydrxyapatite (HA) z Š 161 tœ lf HA z Š j g u ESDg dš z wf i hf Œ f ŒŠh Šf ršf HA z f f j f. 1. hh lr s hf HA z w Œf f f ŠeŠ ff h x ilf j. 2. s Š HA z w Œf } Š i ~ ff d HA fff Š t yl f f ff s HAf Š Š TCP f frf ~900 C s ŠŠ HA z wf ff ŠŠ hf f d CaTiO 3 TiO 2 f Œ f Œ f f. 4. Š ESD g fdš Ti h HAf z f Œf Š f. f f d jt Š yf Š fš lef f. šx 1. L. L. Hench, Effect f temperature n electr-chemical depsitin f calcium phsphate catings in a simulated bdy fluid, J. Am. Ceram. Sc., 74, (1991). 2. P. Ducheyne and L. L. Hench, The prcessing and static mechanical prperties f metal fibre reinfrced biglass, J. Mater. Sci., 17, (1982). 3. J. W. Brets, Advances in Biceramics, Advan. Ceram. Mater., 2, (1987). 4. L. L. Hench, Ceramic Implants fr Humans, Advan. Ceram. Mater., 1, (1986). 5. S. Hb, E. Ichida, and L. T. Garcia), Osseintegratin and cclusal rehabilitatin, Quintessence Int., Tky, H. Kawahara, M. Hirabayash, and T. Shikita,: Single crystal alumina fr dental implants and bne screws, J. Bimed. Mater. Res., 14, (1980). 7. B. Kasem, Bicmpatibility f titanium implants : Surface science aspects, J. Prsth. Dent., 49, (1987). 8. B. Kasem and J. Lausmaa, Brenemark, Quintessence Pub. C., Chicag, j, Œ, txœ f Š i f ƒ gf z Š h, ŠxgŠ l, 17, (1990). 10. B. H. Shearcr, Osse-integrated implants; a review f the literature, J. Int. Dent., 45, (1995). 11. S. D. Ck, K. A. Thmas, J. F. Kay, and M. Jarch, Hudrxyapatitc cated titanium fr rthpcdic implant applicatins, Clin. Orthp. Related Res., 232, (1988). 12. L. L. Hench, Biceramics: Frm cncept t clinic, J. Am. Ceram. Sc., 74, (1991). 13. W. Abdel-Fattah, W. Osiris, S. Mhamed, and M. Khalil, Recnstructin f resected mandibles using a hydrxyapatite veterinary bne graft, Bimaterials, 15, (1994). 14. J. H. Lee, J. W. Lee, and C. Y. Kim, Apatite Frmatin Behavir n Biactive Glasses with Glass Cmpsitin and Reactin Slutin, J. Kr. Ceram. Sc., 37, (2000). 15. J. A. Helsen, J. Prt, J. Schrten, G. Timmermus, E. Brauns, and J. Vandersstraeten, Glasses and Biglasses : Synthesis and Catings, J. Eur. Sc., 17, (1997). 16. C. Y. Kim, A. E. Clark, and L. L. Hench, Cmpsitinal Dependence f Calcium Phsphate Layer Frmatin in FlurideBiglasses, J. Bimed. Mater. Res., 26, (1992). 17. C. Zang, Y. Leng, and X. Zang, In vitr Stability f Plasmasprayed Hydrxyapatite Catings n Ti-6Al-4V Implant under Cyclic Lading, J. Bimed. Mater. Res., 50, (2000). 18. J. H. Chern, H. J. Lin, S. J. Ding, and C. P. Ju, Characterizatin f Immersed Hydrxyapatite-biactive Glass Cating in Hanks Slutin, Mater. Chem. Phys., 64, (2000). 19. J. Jansen, J. Wlke, S. Swann, J. van der Waerden, and K. de Grt, Applicatin f magnetrn sputtering fr prducing ceramic catings n implant materials, Clin. Oral Implants Res., 4, 28Á34 (1993). 20. K. van Dijk, H. Schaeken, J. Wlke, C. Mariee, F. Habraken, J. Verheven, and J. Jansen, Influence f discharge pwer level n the prperties n hydrxyapatite-films depsited n Ti6Al4V with RF magnetrn sputtering, J. Bimed. Mater. Res., 29, (1995). 21. S. Leeuwenburgh, J. Wlke, J. Schnman, and J. Jansen, Electrstatic Spray Depsitin (ESD) f calcium phsphate catings, J. Bimed. Mater. Res., 66A, 330Á334 (2003). Vl. 9, N. 3
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