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Effect of Solution and Calcination Time on Sol-gel Synthesis of Hydroxyapatite

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Abstract

Nano-sized hydroxyapatite (HA) particles were synthesized by sol-gel through water and ethanol based mediums of phosphoric acid (H3PO4) and calcium hydroxide (Ca(OH)2) at pH = 11 for different calcination time (1 h, 2 h, 4 h). The effects of calcination time and solution on the crystallinity, morphology and impurity phases of the HA nanoparticles were examined via Fourier Transform Infrared (FTIR), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Diffraction (XRD). It was found that crystallite size and the fraction crystallinity of the synthesized samples increased with calcination time. According to solution medium, only CaO as impurity was appeared in the water-based solvent, CaO and Ca(OH)2 impurities were appeared in the ethanol-based solvent. The lowest crystallinity was 0.92 and the highest crystallinity was 1.73 respectively, depending on the process parameters. The Ca/P atomic ratio closest to the bone was found as 1.5178. As a result, the employed water-based sol-gel processes for 1 h calcination time was determined as the optimum for the formation of nano-sized HA powders using calcium hydroxide and phosphoric acid.

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References

  1. Gopi D, Kavitha L, Rajeswari D. Synthesis of pure and substituted hydroxyapatite nanoparticles by cost effective facile methods, In Aliofkhazraei M ed., Handbook of Nanoparticles, 2015, 167–190.

    Google Scholar 

  2. Cai Y R, Liu Y K, Yan W Q, Hu Q H, Tao J H, Zhang M, Shi Z L, Tang R K. Role of hydroxyapatite nanoparticle size in bone cell proliferation. Journal of Materials Chemistry, 2007, 17, 3780–3787.

    Article  Google Scholar 

  3. Dorozhkin S V. Nanosized and nanocrystalline calcium orthophosphates. Acta Biomaterialia, 2010, 6, 715–734.

    Article  Google Scholar 

  4. Dong Z H, Li Y B, Zou Q. Degradation and biocompatibility of porous nano-hydroxyapatite/polyurethane composite scaffold for bone tissue engineering. Applied Surface Science, 2009, 255, 6087–6091.

    Article  Google Scholar 

  5. Wang Y Y, Liu L, Guo S R. Characterization of biodegradable and cytocompatible nano-hydroxyapatite/polycaprolactone porous scaffolds in degradation in vitro. Polymer Degradation and Stability, 2010, 95, 207–213.

    Article  Google Scholar 

  6. Sadat-Shojai M, Khorasani M T, Dinpanah-Khoshdargi E, Jamshidi A. Synthesis methods for nanosized hydroxyapatite with diverse structures, Acta Biomaterialia, 2013, 9, 7591–7621.

    Article  Google Scholar 

  7. Vallet-Regí M, González-Calbet J M. Calcium phosphates as substitution of bone tissues. Progress in Solid State Chemistry, 2004, 32, 1–31.

    Article  Google Scholar 

  8. Liu D M, Troczynski T, Tseng W J. Water-based sol-gel synthesis of hydroxyapatite: Process development. Scanning Electron Microscopy, 2001, 22, 1721–1730.

    Google Scholar 

  9. Liou S C, Chen S Y, Lee H Y, Bow J S. Structural characterization of nano-sized calcium deficient apatite powders. Biomaterials, 2004, 25, 189–196.

    Article  Google Scholar 

  10. Türk S, Altınsoy İ, ÇelebiEfe G, Ipek M, Özacar M, Bindal C. Microwave-assisted biomimetic synthesis of hydroxyapatite using different sources of calcium. Materials Science and Engineering: C, 2017, 76, 528–535.

    Article  Google Scholar 

  11. Bose S, Saha S. Synthesis of hydroxyapatite nanopowders via sucrose-templated sol-gel method. Journal of the American Ceramic Society, 2003, 86, 1055–1057.

    Article  Google Scholar 

  12. Eshtiagh-Hosseini H, Housaindokht M R, Chahkandi M. Effects of parameters of sol-gel process on the phase evolution of sol-gel-derived hydroxyapatite. Materials Chemistry and Physics, 2007, 106, 310–316.

    Article  Google Scholar 

  13. Hsieh M F, Perng L H, Chin T S, Perng H G. Phase purity of sol-gel-derived hydroxyapatite ceramic. Biomaterials, 2001, 22, 2601–2607.

    Article  Google Scholar 

  14. Fathi M H, Hanifi A, Mortazavi V. Preparation and bioactivity evaluation of bone-like hydroxyapatite nanopowder. Journal of Materials Processing Technology, 2008, 202, 536–542.

    Article  Google Scholar 

  15. Michael F M, Khalid M, Ratnam C T, Chee C Y, Rashmi W, Hoque M E. Sono-synthesis of nanohydroxyapatite: Effects of process parameters. Ceramics International, 2015, 42, 6263–6272.

    Article  Google Scholar 

  16. Waheed S, Sultan M, Jamil T, Hussain T. Comparative analysis of hydroxyapatite synthesized by sol-gel, ultrasonication and microwave assisted technique. Materials Today: Proceedings, 2015, 2, 5477–5484.

    Google Scholar 

  17. Bakan F, Laçin O, Sarac H. A novel low temperature sol-gel synthesis process for thermally stable nano crystalline hydroxyapatite. Powder Technology, 2013, 233, 295–302.

    Article  Google Scholar 

  18. Huang Z, Zhou Q, Wang X F, Liu Z C. A biomimetic synthesis process for Sr2+, HPO4 2-, and CO3 2- substituted nanohydroxyapatite. Materials and Manufacturing Processes, 2016, 31, 217–222.

    Article  Google Scholar 

  19. Degirmenbasi N, Kalyon D M, Birinci E. Biocomposites of nanohydroxyapatite with collagen and poly(vinyl alcohol). Colloids Surfaces B: Biointerfaces, 2006, 48, 42–49.

    Article  Google Scholar 

  20. Fan W, Sun Z, Wang J, Zhou J, Wu K, Cheng Y. Evaluation of Sm0.95Ba0.05Fe0.95Ru0.05O3 as a potential cathode material for solid oxide fuel cells. RSC Advances, 2016, 6, 34564–34573.

    Article  Google Scholar 

  21. Sanosh K P, Chu M C, Balakrishnan A, Lee Y J, Kim T N, Cho S J. Synthesis of nano hydroxyapatite powder that simulate teeth particle morphology and composition. Current Applied Physics, 2009, 9, 1459–1462.

    Article  Google Scholar 

  22. Currey J. Sacrificial bonds heal bone. Nature, 2001, 414, 699.

    Article  Google Scholar 

  23. Pang Y X, Bao X. Influence of temperature, ripening time and calcination on the morphology and crystallinity of hydroxyapatite nanoparticles. Journal of the European Ceramic Society, 2003, 23, 1697–1704.

    Article  Google Scholar 

  24. Chen L, Tang C Y, Ku H S, Tsui C P, Chen X. Microwave sintering and characterization of polypropylene/multi-walled carbon nanotube/hydroxyapatite composites. Composites Part B: Engineering, 2014, 56, 504–511.

    Article  Google Scholar 

  25. Paz A, Guadarrama D, López M, González J E, Brizuela N, Aragón J. A comparative study of hydroxyapatite nanoparticles synthesized by different routes. Química Nova, 2012, 35, 1724–1727.

    Article  Google Scholar 

  26. Varma H K, Babu S S. Synthesis of calcium phosphate bioceramics by citrate gel pyrolysis method. Ceramics International, 2005, 31, 109–114.

    Article  Google Scholar 

  27. Mujahid M, Sarfraz S, Amin S, Road J. On the formation of hydroxyapatite nano crystals prepared using cationic surfactant. Materials Research-Ibero-American Journal of Materials, 2015, 18, 468–472.

    Google Scholar 

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Authors and Affiliations

  1. Biomedical, Magnetic and Semi Conductive Materials Research Center (BIMAS-RC), Sakarya University, Esentepe Campus, Sakarya, 54187, Turkey

    Serbülent Türk, Mahmut Özacar & Cuma Bindal

  2. Faculty of Engineering, Department of Metallurgy and Materials Engineering, Sakarya University, Esentepe Campus, Sakarya, 54187, Turkey

    İbrahim Altınsoy, Gözde Çelebi Efe, Mediha Ipek & Cuma Bindal

  3. Science & Arts Faculty, Department of Chemistry, Sakarya University, Sakarya, 54187, Turkey

    Mahmut Özacar

Authors
  1. Serbülent Türk
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  2. İbrahim Altınsoy
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  3. Gözde Çelebi Efe
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  4. Mediha Ipek
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  5. Mahmut Özacar
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  6. Cuma Bindal
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Correspondence to Cuma Bindal.

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Türk, S., Altınsoy, İ., Çelebi Efe, G. et al. Effect of Solution and Calcination Time on Sol-gel Synthesis of Hydroxyapatite. J Bionic Eng 16, 311–318 (2019). https://doi.org/10.1007/s42235-019-0026-3

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