Surface Modification of Nano-Hydroxyapatite with Silane Agent
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1 ß 23 ß 1 «Ã Vol. 23, No Ç 1 Journal of Inorganic Materials Jan., 2008» : X(2008) Þ¹ Ò À Đ³ Ù Å Ð (ÎÄÅ Ç ÂÍ ËÊÌÏÁÉ È ÃÆ ) Ì É (KH-560) ¼ ³ (n-ha) ³ ËØ ÌË n-ha KH-560 Õ Ì»Þ ÒßÈ (FT-IR) Ô X È Çà (XPS) ³ É ³³ Ï Ì (Si OH) ÌÐ (HPO 2 4 ) Ù» ÝÁ Õ Si O P Üà Ïß Ì HA ³ OH ÖÝÁ ÜÃ É ËØÕ HA Ì (PC) Õ Õ Ã ÆÅËØÕ¹ ³ dz È (SEM) ³½ ÅËØÕÕ HA Ð PC Æ ± ³ ««Å Õ Ì Ã Õ ÖÊ Ü ¼ ³ Ì É Ì ³ Õ R318» A Surface Modification of Nano-Hydroxyapatite with Silane Agent LIAO Jian-Guo, WANG Xue-Jiang, ZUO Yi, ZHANG Li, WEN Ji-Qiu, LI Yu-Bao (Research Center for Nano-Biomaterials, Analytical & Testing Center, Sichuan University, Chengdu , China) Abstract: Nano-hydroxyapatite (n-ha) was modified by using silane coupling reagent (KH-560), and the interfacial interactions between n-ha and KH-560 was also studied. Fourier transform infrared spectra (FT-IR) and X-ray photoelectron spectra (XPS) analyses show that the silane coupling molecular binds strongly to n-ha surface. Chemical bonding (Si O P) is formed by the reaction between Si OH and HPO 2 4 group, and a similar interface effect exists between Si OH and the hydroxyl group of HA. Surface modification of HA particles can improve the mechanical strength of the n-ha/polycarbonate (n-ha/pc) composites dramatically. SEM observation shows that modified HA particles uniformly distribute in the PC matrix. The results indicate that the interfacial interaction between surface-modified inorganic particles and polymer matrix is crucial for the improvement of the mechanical strength of the composites. Key words: nano-hydroxyapatite; silane-agent; polycarbonate; composites; surface modification 1 Þ Ý Ê ½ (Ä É) Ý Ö - ½ º Ð Ó Ê Á ½ Đ (n-ha). Þ Ð Đ (HA, Ca 10 (PO 4 ) 6 (OH) 2 ) Í «Ö º ÄÃÅÄ ÖÞÅ Ð HA Í Á ÐÍ Å ½ Ä Ù Ö º [1]. n-ha/ Ð º Ð Ê ÎÍ ÜÐ [2 5]. ÎÍ º HA HA Ö Ð ÖÈ Ý ¹ ÄÐ Å ÄÙ Ö ºÆ HA Å Ð ¼ Ö»Ò ² º Æ HA Ð ÁÕ Æ ÎÍ Ñ Å ºÐ º º¼ Ö ÐÄ µû² µ ÚÛ² µ Ä º Ú» (2004CB720604) ¹ (1975 ), À ¹ ÍÌ ½± Û« nic7504@scu.edu.cn

2 146 «Ã 23 ºÐ Å ÄÖÁ ØÉ «Ö Ð ºÐ «Ö Å Ä [6 8]. Ð (  Â) ÚÖÊ Ð HA ¼ Õ ºÐ ƺ Ö Ð ÆDupraz Ù [9] лÒÖÎ Ê HA Å Ð ºÐ ÎÍ º µ HA ÖÎ Ê ØÖ Åʽ ³ÍÐÆ Í º KH-560 ÖÖ n-ha Å A Í ºÐ HA Å Í ºÐ ÖÖ Å Ä ÎÍÆ 2 ÔÓ PC110, Đ ¹ Á Å KH-560(γ-(2, 3- ) Î ), Â É Þ n- HA ¼ [10] É (À φ(15 20)nm h(80 120)nm). º KH-560 ± ph ÖÒÍ º n-ha ¼ 80 C ± 1h, ÉÕ 80 C µð 12h, Î ÖÐ Â º Ý Î 200 ±Å Æ ºÊ ÌÚÖÖ HA ÝÅ PC Ð 100 C µðñ 8h, ÝÖÐ È (TSSJ- 25 Ò ½ Ê È Þ ½ É Þ Î Í ) È Ã Â (K-TEC40, Ò Ferromatic Milacron) Â Æ 3 Ð Nicolet 170SX ¼ ß Ó É Ð (FT- IR, Spectrum One, ¹ ) ÍÊ Ð KRATOS, XSAM800 XPS Ð (Ú ) ÍÖÆÉÄ Ð JSM-5900L Đ È É ( Jeol) Í Ç Æ Ð Ä (AUFOGRAPH, Shimadzu) ºÐ Å Ä Õ GB/T È GB/T Ò GB/T Æ 4 ß 4.1 IRÖ¼ Õ 1 Õ È Ê ÌÚÖ n-ha cm 1 ÌÖ OH ² Å cm 1 Ì Ö PO 3 4 ² Þ 960cm 1 ÌÖ² ² cm 1 ÌÖ²ÒÞÆÌÚÖÖ n-ha cm 1 Õ cm 1 ÌÈ ² KH-560 Ö ²Æ ÌÚÖ n-ha Ö HPO 2 4 (872cm 1 ) ²¾ ± Ä KH-560 Â Ö Si(OH) 3 Å HPO 2 4 ¼ º ØÍÐ Si O P Þ Å ²¾±Æ 4.2 XPS Ö¼ ÆÌÚÖ ÈÖ ÐÄ Þ Ü ÖÌÚ ÆÕ 2 ¾ KH-560 ÌÚ n-ha Ca O P C ÆÉ C ²Á ÖÉ n-ha Ö CO 2 3 Ú Æ Ê Ö n-ha Ö Ca O P ²Öº ± C ²Ú Ò È ÅÖ Si ² KH-560 Î Ê Ñ Æ À ¹ n-ha Æ Ø n-ha ¹ Î Ê Ö Ca O P È ³ º ² ¼± Î Æ È Ù C ² Æ Si ²ÖÈ n-ha Î ÚÆ n-ha Ö ÆÉ Á È» Æ ÆÐ Æ Õ 3(a) n-ha Ö»ÒÖ Þ ÅÄ eV Ì PO 3 4 Ö ÆÉ ÐÄ eV Ì Ü OH Ö ÆÉ [11], eV ÌÖ O Ü CO 2 3 Ö C=O. ÐÄ ² (533.20eV) ÅÛ ÐIJ (531.42, eV) Ö ¼ 1.0:10.9, n-ha Ö Å Í ÖÚ (1:12) ÛÆ ÐÕ 1, ÕÛ Á n-ha À Ö CO 2 3 HPO 2 4 Ù ÖÆÕ 3(b) Ê Ö n-ha O ÆÉÖÆÐ Õ È O ÆÉÖ ÐÄ Þ Õ eV ÖÁ² Ü PO 3 4 CO 2 3 Ö O ÆÉ ÅÕ 3(a) Ö O Æɲº ÞÅ Æ eV Ì O Û Ð ÄÖÈ Ö n-ha O Æ É ÅĐÈ Đ¾ Û C P ÖÆ É ÈÚÔ O C O P Ö C P(Si O Si ²). ÐÄ eV ÌÖ² Ü OH Ö O, ÅÕ 3(a) º ÞÅ Æ eV Ö ² ÖÞÅ Si O P Ö ² (Ï Ý P H ÖĐ¾ ºÒ P ĐÈ P O È Si O H Ö Õ ÄÈ ÖÛÄ ²), O Æ ÉÖÆ Ð Ä (533.03; eV) ² ÅÆÛ ÐÄ (530.57; eV) ² Ö 1.0:2.3, 1.0:10.9,

3 1 Ï Ì É ¼ ³³ ÕÌË 147 Ä n-ha Ö ÚÅÊ È ºØÍÐ ¹ÆÐ²Ö ³ ²Ö ÞÆ Õ 4 ¾Æ KH-560 ÌÚ Ö n-ha Ö P(2p) XPS Ä ÕÆ Õ 4(a) Õ Ð n-ha Ö P Æ ÉÕ PO 3 4» ÐÄ eV; Õ 4(b) P(2p) Ä Æ ² µ eV, Æ ² Ö 1.07eV. Ô 1 n-ha É ÕÕÒßÈ Ô Fig. 1 FTIR spectra of HA before and after modification (A) HA before modification; (B) HA modified with KH- 560 and (C) KH-560 Ô 2 n-ha ³ Å KH-560 ËØÕÕÖ XPS Ã Ô Fig. 2 XPS spectra of n-ha before and after modification (A) Before modification; (B) Modified with KH-560 Ô 3 n-ha ³ Õ O(1s) Å XPS Ã Ô Fig. 3 XPS O(1s) element fitting spectra of n-ha before and after modification (a) Before surface modification; (b) After surface modification Ô 4 n-ha ³ Å KH-560 ËØÕ P(2p) Ï Å XPS Ã Ô Fig. 4 XPS P(2p) element fitting spectra of n-ha before and after modification (a) Before surface modification; (b) After surface modification

4 148 «Ã 23 ÆµÚ P(2p)  (132.79eV) ± ² Ô P È Æµ ÔÐƾ  н Ú H È ÆØÓ P O H Ô H. Ó 3(b) ÆµÔ O Ô ± ÓЫKH-560 À ÔÔ Si OH n-ha ² Si O P, Đ Si Ôн Ú H È Si Ó H Ô P ÐÆ ¾ ³Î P(2p) ÐÆ Â¾Ú Ô È ±ÆµÔ «Ó 5 «Si(2p) XPS Â Ó Ó Æ Ä KH- 560 Ê ÔÔ n-ha Ä À Ü Si(2p)XPS Â Æ ±«KH-560 Ô Â Si È ÛÂà C Si O C, KH-560 À C Si O H C Si O Si. C Si O H n-ha ² Û Â µ C Si O P, Î Ó 5 Si(2p) Æ ±Ô «Pouling Ð ½ [12], C(2.5)>H(2.1) =P(2.1)>Si(1.8), Si ºÑÛÂßÇ Þ ÐÆ ¾ «C Si O C< C Si O H< C Si O P < C Si O Si. Ó KH-560 n-ha Û ÂËß µ Si(2p) ÐÆ Â Û Ú ¼ Ó 5 ¼«ÎÞ ÎÜ P H Ôн Ñ P ÞÐÆ Ó C Si O P µ Si ÔÞ ÐÆ ¾ C Si O H µ Si Þ ÐÆ ¾ ÓÈ Ô C Si O P µ «4.3 È KH-560 Ë À À Û Ó ÔÀ Ó n-ha ² Ô Ø Û n-ha ² Ô Å Ë ÔÞ ÀÔ Å Ø«Đ n-ha» Ô ² Æ ² À Á µ Î ² Ô ³ È Û«n-HA È Ô º  2 [11,13 15], Þ n-ha OH HPO 2 4 PO 3 4 Ø Ë Ô ¾ ÔÛµ ( Ó 6(a) ¼); Â Ë È À Ô n-ha ² Ô OH HPO 2 4 µ (Ó 6(b)). Û ÂÓÞ º«À«Ô 5 n-ha ³ Å Õ Si(2p) Ï Å XPS Ã Ô Fig. 5 XPS Si(2p) element fitting spectra of n-ha after modification Ô 6 n-ha KH-560» Õ Ì Fig. 6 Interfacial mechanism between n-ha and KH-560 (a) Chemical bond; (b) Hydrogen bond 4.4 Æ HA/PC ¾ ÔĐ  ² 1. Ó Æ Ô¾ ÔÔ ¾ Ç ÐÑ Ä KH-560 È ÔÔ ¾ ² ² È Â Ó HA Ï º Ô Đ Â Â«¾ Ô Đ ĐÚ Ï «Ï º ÓÛµ ¾ HA Ô² ÎÄ Ê È Ô Å Æ Ó Ç Æ ÔÛµ Æ Ó 1 HA/PCØ Ð Table 1 Mechanical properties of HA/PC composites Tensile Bending Compressive Sample PC/HA strength strength strength /MPa /MPa /MPa PC PC/HA 90/ PC/HA-KH /

5 1 Ï Ì É ¼ ³³ ÕÌË 149 ĐÚ Ï Ô Đ Ô ¾«HA ÔÆ Ï Ô» Ó HA PC Ô Ûµ Å ÐÑ Ç «4.5 Ð Ñ SEM Ý Ó 7 ¾ ÐÑ«ÔÔ«SEM Ë«Ó Æ ² Ô HA PC ¼º Ð ² Ø Ï «À À «««µ в ÔÑ Ã Ä² Ê Ô Ð² Ï º «² Ê ÔÔ n-ha PC ¼ Ï «À À ß «² Ä KH-560 Ê ÔÔ Ð² Ï «Ô 7 n-ha/pc(10/90) Õ SEM Ì Fig. 7 Fracture surfaces of the n-ha / PC(10/90) composites (a) Before modification; (b) After modification 5 Æ n-ha KH-560 ËßÔ µ KH-560 Ô À  n-ha ² Û ÂËß ÔÛµ È ÔÀ ¾ n-ha ² ² Ø Ï«² ÔÔ n-ha PC HA/PC ¾ ÔĐ  ² n-ha ² ÔÈ HA/ Ï ¾ ÂÔ Å««º¾ [1] Hulbert S F, Bokros J C, Hench L L, et al. Ceramics in clinical applications. past, present and future, in High Tech Ceramics, ed. by P. Vincenzini, Italy: Milan Press, [2] Verheyen CCPM, de Wijn J R, van Blitterswijk C A, et al. J. Biomed. Mater. Res., 1993, 27 (4): [3] Ylinen P. J. Mater. Sci.: Mater. in Med., 1994, 5 (9): [4] ËÞ Û«Ü Ø ¹ Ä 2004, 21 (2): [5] Ü Û«Ø (ZHANG Li, et al). Ä (Journal of Inorganic Materials), 2006, 21 (5): [6] Liu Q, de Wijn J R, Bakker D, et al. J. Mater. Sci.: Mater. in Med., 1996, 7 (9): [7] Deb S, Wang M, Tanner K E, et al. J. Mater. Sci.: Mater. in Med., 1996, 7 (3): [8] Î ± ± Ø ¹ Ä 2001, 18 (2): [9] Dupraz A M P, Meer S A T V d, de Wijn J R, et al. J. Mater. Sci.: Mater. in Med., 1996, 7 (12): [10] Ľ ¹ Û«Ø ÐÆ 2000, 10 (11): [11] Wang X J, Li Y B, Wei J, et al. Biomaterials, 2002, 23 (24): [12] Ù Ä ÝÄ Í ÝÄ «Á Ø Ç [13] Ù ² Ø Í 2004, 18 (3): [14] Î ÊÀ Ä Ã 2006, 26 (1): [15] Ï Ø (YAO Cao, et al). Ä (Journal of Inorganic Materials), 2006, 21 (2):

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