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Characteristic and Formation of Hydroxyapatite Synthesized from Heat Treatment of Cuttlefish Bone Kridsada Faksaw Department of Physics, Faculty of King Mongkut’s University of Technolo Outlines Introduction bone Results & Discussion 2 Objective s Experime nt Conclusio n Introduction 3 Ref: http://eng.thesaurus.rusnano.com 0 Dimensi on 1 Dimensi on 2 Dimens ion 3 Dimensi on Ref: http://commonsensecanadian.c om Nano scale 1 to 100 nanometers Shape and Size Effect Increasing of specific 3 Introduction 4 Enhanced resorbability Bone Improved densification sinter ability Hydroxyapa tite Improved cell proliferation Improved cellular activity related to bone growth Ref: http://oncoinfo.ru Ref: http://i.vimeocdn Introduction Osteon Spongy bone Compac t bone Mineralized fibrils Osteoni c canal Microsc opic view Lamella e Collagen fiber 5 Collage n triple helix Hydroxyapa tite Ca5(PO4)3 OH Hexagon al Bio ceramics Inorganic mineral IntroductionHow do you synthesized hydroxyapatite? Natural material 90-95% of Ca Ca source PO4 source Chemical material K2HPO Ca2P2O 4 7 Trace of Na2HP O4 (NH4)2H PO4 Found β - Trace of Na Odor 6 IntroductionHow to synthesis of hydroxyapatite Solid state H2O/E tOH Ball milling Sol gel 7 gelati on Precipitat ion Microw ave irradiati Ca2+ solution PO437 solution Objectives To study phase transformation of cuttlefish bone by various sintering temperature. To study characteristics of hydroxyapatite synthesized from various heated cuttlefish bone by ball milling method. To study crystal structure, functional group and morphology of synthesized hydroxyapatite by 8 Experim ent Part 2.bone Hydroxyapatite synthesis Part 1. Temperature effect on cuttlefish 9 • room tempera ture 200 to 1300 ˚C 500 °C 900 °C Ball milling method Vary precursor Experim ent: Cuttlefish bone Temperature effect on cuttlefish bone groun d 10 Temperature effect on cuttlefish bone 1300 °C 200 °C 500 °C 1100 °C 900 °C Hydroxyapatite synthesis Part 1 11 Temperature effect on cuttlef bone Orthorho CaO (lime) Results & Discussion: Intensity (a.u.) T 900 °C CaCO3 (calcite) T 500 °C CaCO3 (aragonite) Before heated room tempera ture 500 °C 900 °C mbic a≠b≠c α = β = γ = 90 Rhombohedral a=b=c α ≠ β ≠ γ ≠ 90 Cub ica = b = c α = β = γ = 90 Thermal decomposition of CaCO3 2theta (degree) Heate CaCO 3 Fig 1 XRD pattern of temperature effect on cuttlefish bone d at various temperature CO2900 °C 20 30 40 50 60 70 80 + CaO Experim Ball Milling 5CaO + 3(NH ) HPO Vary calcium sources ent: 4 2 CaO (lime phase) (for example) CaO )2HPO4 DI CaCO(NH (aragonite 4 3 5M water 3M phase) CaCO3 at 500 °C tainless(calcite steel phase) container steel ball 4 12 + H2O Ca5(PO4)3(OH) + 5H2O + 6NH3 Experim ent: Ball Milling 13 00 dried for 48 h Ground until powder Hydroxyapa tite Characterization sample X-ray diffractometer: XRD Fourier transform infrared spectro Scanning electron microscopy: SE Results & hydroxyapatite Discussion: Part 2 14 Hydroxyapatite synthesis by bal CaCO3 (aragonite) Ball milled 120 min Intensity (a.u.) 5CaCO3 + 3(NH4)2HPO4 + H2O Ball milled 60 min HAp Ca = 5(PO4)3OH + 4H2O + 5 Ball milled 30 min Ball milled 5 min JCPDS file NO. 09-0432 CaCO3 (aragonite) 20 30 40 50 60 2theta (degree) a) Aragonite phase precursor Pure hydroxyapatite phase at milling According to JCPDS file NO. 09-0432 Hydroxyapatite phase Hexagonal Fig 2 XRD pattern of synthesized hydroxyapatite from cuttlefish bone at different Results & hydroxyapatite Discussion: Part 2 15 Hydroxyapatite synthesis by ba CaCO3 Ball(calcite) milled 120 min Intensity (a.u.) 5CaCO3 + 3(NH4)2HPO4 + H2O Ball milled 60 min HAp Ca = 5(PO4)3OH + 4H2O + 5 Ball milled 30 min Hydroxyapatite and CaCO3 phase appeared at milling time 5 to120 min Ball milled 5 min JCPDS file NO. 09-0432 CaCO3 (calcite) 20 30 40 50 60 2theta (degree) b) Calcite precursor According to JCPDS file NO. 09-0432 Hydroxyapatite phase Hexagonal Fig 2 XRD pattern of synthesized hydroxyapatite from cuttlefish bone at different Results & hydroxyapatite CaO Discussion: (lime) Part 2 16 Hydroxyapatite synthesis by bal Ball milled 120 min Intensity (a.u.) 5CaO + 3(NH4)2HPO4 + H2O Ball milled 60 min HAp Ca = 5(PO4)3(OH) + 5H2O Ball milled 30 min Pure hydroxyapatite phase at milling Ball milled 5 min JCPDS file NO. 09-0432 CaO (lime) 20 30 40 50 60 2theta (degree) c) Lime phase precursor According to JCPDS file NO. 09-0432 Hydroxyapatite phase Hexagonal Fig 2 XRD pattern of synthesized hydroxyapatite from cuttlefish bone at different Ball milled 120 min Ball milled 60 min 1476 565 872 1100 Ball milled 30 min 872 1476 1100 1024 Ball milled 5 min 603 565 2- CO3 group 1794 process Ball milled 120 min Ball milled 120 min 1794 1476 1100 872 1794 1476 1100 872 603 1024 Ball milled 30 min 1794 1476 1100 Ball milled 5 min 1476 1100 872 710 603 565 1024 603 1024 Ball milled 60 min 603 565 1024 1794 4000 3800 3800 3600 3600 4000 603 1024 1794 Hydroxyapatite synthesis by bal Synthesis 872 1476 1100 %Transmittance %Transmittance 1794 17 872 603 872 1476 1100 565 565 565 1024 1794 1794 1476 %Transmittance Results & Discussion: Part 2 1024 603 Ball milled 60 min b) Calcite precursor 603 565 1024 1794 1476 872 1100 Ball milled 30 min 603 565 1024 1794 1476 872 1100 Ball milled 5 min 1794 565 1476 1100 872 1024 603 565 1024 3800 3600 2500 2000 2000 1500 1000 1000 500 4000 4000 3800 3600 2500 2000 1 1500 1500 1000 500 4000 4000 3800 3800 3600 3600 2500 2500 500 500 2000 1500 1000 Wavenumber (cm ) Wavenumber (-cm 1) Wavenumber (cm-1) Wavenumber (cm-1) a) Aragonite phase precursor 872 1100 603 565 2000 1000 500 2500 2000 1500 1000 500 1500 2500 1 Wavenumber (-cm ) Wavenumber (cm-1) c) Lime phase precursor Fig 3 FTIR spectra of synthesized hydroxyapatite from cuttlefish bone at various different Part 2 Results & Ball milling Discussion: time 18 Hydroxyapatite synthesis by bal a) Aragonite phase precursor b) Calcite precursor c) Lime phase precu 120 min 500 nm 500 nm Average particle size 6070 nm 500 nm Fig. 4 SEM image of synthesized hydroxyapatite from cuttlefish bone at various different Conclusions 19 From results of temperature effect on cuttlefish Aragonite phase change to calcite phase completely and calcite phase transform to lime phase completely at temperature 500 °C and 900 °C respectively. From results of hydroxyapatite synthesis Hydroxyapatite phase appear at milling 5 minutes • Hydroxyapatite phase appear completely at 60 minutes in CaCO3 (aragonite phase) precursor. • Hydroxyapatite phase appear completely at more than 120 minutes in CaCO3 (calcite phase) precursor • Hydroxyapatite phase appear completely at 5 minutes in CaO (lime) precursor References 20 Amin, S., Bekhit, A.E., Azam, A. and Zhifa, S., 2015, “Synthesis of Nano- Hydroxyapatite (nHA) from Waste Mussel Shells Using a Rapid Microwave Method”, Materials Chemistry andM.T., Physics, 149-150, pp. 607Mehdi, S.S., Khorasani, Ehsan,Vol. D.K. and Ahmad, J., 616. 2013,“Synthesis Methods for Nanosized Hydroxyapatite Indiverse Structures ”, Acta Biomaterialia, Vol. 4, pp. 281312. J., Li ,K., Wang, H., Zhu, M. and Yan, H., 2014, “Rapid Liu, Formation of Hydroxyapatite Nanostructures by Microwave Irradiation”, Chemical Physical, Vol. 396, pp.
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