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Biomimetic apatite-based composite materials obtained by spark plasma sintering (SPS): physicochemical and mechanical characterizations

  • Biomaterials Synthesis and Characterization
  • Original Research
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Abstract

Nanocrystalline calcium phosphate apatites are biomimetic compounds analogous to bone mineral and are at the origin of the bioactivity of most biomaterials used as bone substitutes. Their unique surface reactivity originates from the presence of a hydrated layer containing labile ions (mostly divalent ones). So the setup of 3D biocompatible apatite-based bioceramics exhibiting a high reactivity requests the development of «low» temperature consolidation processes such as spark plasma sintering (SPS), in order to preserve the characteristics of the hydrated nanocrystals. However, mechanical performances may still need to be improved for such nanocrystalline apatite bioceramics, especially in view of load-bearing applications. The reinforcement by association with biopolymers represents an appealing approach, while preserving the advantageous biological properties of biomimetic apatites. Herein, we report the preparation of composites based on biomimetic apatite associated with various quantities of microcrystalline cellulose (MCC, 1–20 wt%), a natural fibrous polymer. The SPS-consolidated composites were analyzed from both physicochemical (X-ray diffraction, Fourier transform infrared, solid state NMR) and mechanical (Brazilian test) viewpoints. The preservation of the physicochemical characteristics of apatite and cellulose in the final material was observed. Mechanical properties of the composite materials were found to be directly related to the polymer/apatite ratios and a maximum crushing strength was reached for 10 wt% of MCC.

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References

  1. Billotte WG. Ceramic biomaterials. In: Park JB, Bronzino JD, editors. Biomaterials principles and applications. Boca Raton: CRC Press; 2003. p. 21–54.

    Google Scholar 

  2. Heness G, Ben-Nissan B. Innovative bioceramics. Mater Forum. 2004;27:104–14.

    Google Scholar 

  3. Eichert D. Etude de la réactivité de surface d’apatites de synthèse nanocristallines. PhD thesis, INP Toulouse, 2001.

  4. Cazalbou S, Eichert D, Ranz X, Drouet C, Combes C, Harmand MF, Rey C. Ion exchanges in apatites for biomedical application. J Mater Sci. 2005;16:405–9.

    Google Scholar 

  5. Grossin D, Rollin-Martinet S, Estournes C, Rossignol F, Champion E, Combes C, Rey C, Chevallier G, Drouet C. Biomimetic apatite sintered at very low temperature by spark plasma sintering: physico-chemistry and microstructure aspects. Acta Biomater. 2010;6:577–85.

    Article  Google Scholar 

  6. Drouet C, Bosc F, Banu M, Largeot C, Combes C, Dechambre G, Estournes C, Raimbeaux G, Rey C. Nanocrystalline apatites: from powders to biomaterials. Powder Technol. 2009;190:118–22.

    Article  Google Scholar 

  7. Mano JF, Sousa RA, Boesel LF, Neves NM, Reis RL. Bioinert, biodegradable and injectable polymeric matrix composites for hard tissue replacement: state of the art and recent developments. Compos Sci Technol. 2004;64:789–817.

    Article  Google Scholar 

  8. Tobyn M, McCarthy GP, Staniforth JN, Edge S. Physicochemical comparison between microcrystalline cellulose and silicified microcrystalline cellulose. Int J Pharm. 1998;169:183–94.

    Article  Google Scholar 

  9. Kiziltas A, Gardner DJ, Han Y, Yang H-S. Dynamic mechanical behavior and thermal properties of microcrystalline cellulose (MCC)-filled nylon 6 composites. Thermochim Acta. 2011;519:38–43.

    Article  Google Scholar 

  10. Adel AM, El-Wahab ZHA, Ibrahim AA, Al-Shemy MT. Characterization of microcrystalline cellulose prepared from lignocellulosic materials. Part II: physicochemical properties. Carbohydr Polym. 2011;83:676–87.

    Article  Google Scholar 

  11. Vandecandelaere N, Rey C, Drouet C. Biomimetic apatite-based biomaterials: on the critical impact of synthesis and post-synthesis parameters. J Mater Sci. 2012;23:2593–606.

    Google Scholar 

  12. Elliott C. Structure and chemistry of the apatites and other calcium orthophosphates, studies in inorganic chemistry, vol. 18. Amsterdam: Elsevier; 1994. p. 288.

    Google Scholar 

  13. Kolodziejski W. Solid-state NMR studies of bones. Top Curr Chem. 2004;246:235–70.

    Article  Google Scholar 

  14. Eichert D, Drouet C, Sfihi H, Rey C, Combes C. Nanocrystalline apatite-based biomaterials: synthesis, processing and characterization. In: Kendall JB, editor. Biomaterials research advances. New York: Nova Science Publishers; 2007. p. 93–143.

    Google Scholar 

  15. Bradley JV, Bridgland LN, Colyer DE, Duer MJ, Friscic T, Gallagher JR, Reid DG, Skepper JN, Trasler CM. NMR of biopolymer-apatite composites: developing a model of the molecular structure of the mineral-matrix interface in calcium phosphate biomaterials. Chem Mater. 2010;22:6109–16.

    Article  Google Scholar 

  16. Rojas J, Lopez A, Guisao S, Ortiz C. Evaluation of several microcrystalline celluloses obtained from agricultural by-products. J Adv Pharm Technol Res. 2011;2:144–50.

    Article  Google Scholar 

  17. Atalla RH, Gast JC, Sindorf DW, Bartuska JC, Maciel GE. Carbon-13 NMR spectra of cellulose polymorphs. J Am Chem Soc. 1980;102:3249–51.

    Article  Google Scholar 

  18. Park S, Johnson DK, Ishikawa CI, Parilla PA, Davis MF. Measuring the crystallinity index of cellulose by solid state 13C nuclear magnetic resonance. Cellulose. 2009;16:641–7.

    Article  Google Scholar 

  19. Isogai A, Usuda M, Kato T, Uryu T, Atalla RH. Solid-state CP/MAS carbon-13 NMR study of cellulose polymorphs. Macromolecules. 1989;22:3168–72.

    Article  Google Scholar 

  20. Idstrom A, Brelid H, Nydén M, Nordstierna L. CP/MAS 13C NMR study of pulp hornification using nanocrystalline cellulose as a model system. Carbohydr Polym. 2013;92:881–4.

    Article  Google Scholar 

  21. Jaeger C, Groom NS, Bowe EA, Horner A, Davies ME, Murray RC, Duer MJ. Investigation of the nature of the protein-mineral interface in bone by solid-state NMR. Chem Mater. 2005;17:3059–61.

    Article  Google Scholar 

  22. Nikel O, Laurencin D, Bonhomme C, Sroga GE, Besdo S, Lorenz A, Vashishth D. Solid state NMR investigation of intact human bone quality: balancing issues and insight into the structure at the organic-mineral interface. J Phys Chem C. 2012;116:6320–31.

    Article  Google Scholar 

  23. Nikel O, Laurencin D, McCallum SA, Gundberg CM, Vashishth D. NMR investigation of the role of osteocalcin and osteopontin at the organic–inorganic interface in bone. Langmuir. 2013;29:13873–82.

    Article  Google Scholar 

  24. Bonhomme C, Gervais C, Laurencin D. Recent NMR developments applied to organic–inorganic materials. Prog Nucl Magn Reson Spectrosc. 2014;77:1–48.

    Article  Google Scholar 

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Acknowledgments

This research was partly funded by the French National Research Agency (ANR) through the NanoBioCer Project (ANR-07-BLAN-0373). We are grateful to Makram EL-BACHAWATI for the preliminary studies of this work.

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Authors and Affiliations

  1. CIRIMAT Carnot Institute, UMR CNRS/INPT/UPS 5085, Université de Toulouse, Faculté de Pharmacie 35 chemin des maraichers, 31062, Toulouse Cedex 4, France

    Fabien Brouillet

  2. Institut Charles Gerhardt de Montpellier, UMR5253, CNRS/UM/ENSCM, CC1701, Place Eugène Bataillon, 34095, Montpellier Cedex 05, France

    Danielle Laurencin

  3. CIRIMAT Carnot Institute, UMR CNRS/INPT/UPS 5085, Université de Toulouse, ENSIACET 4 allée Emile Monso, 31030, Toulouse, France

    David Grossin, Christophe Drouet & Christian Rey

  4. CIRIMAT Carnot Institute, UMR CNRS/INPT/UPS 5085, Université de Toulouse, LCMIE 118 route de Narbonne, 31062, Toulouse, France

    Claude Estournes & Geoffroy Chevallier

  5. PNF2, CNRS, UPS, MHT, 118 Route de Narbonne, 31062, Toulouse, France

    Claude Estournes & Geoffroy Chevallier

Authors
  1. Fabien Brouillet
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  2. Danielle Laurencin
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  3. David Grossin
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  4. Christophe Drouet
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  5. Claude Estournes
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  6. Geoffroy Chevallier
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  7. Christian Rey
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Corresponding author

Correspondence to Fabien Brouillet.

Electronic supplementary material

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10856_2015_5553_MOESM1_ESM.pdf

Supplementary material 1 (PDF 86 kb). Supplementary Materials in Online Ressource. Additional analyses of 1H → 31P CPMAS solid state NMR spectra (Figure S1)

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Brouillet, F., Laurencin, D., Grossin, D. et al. Biomimetic apatite-based composite materials obtained by spark plasma sintering (SPS): physicochemical and mechanical characterizations. J Mater Sci: Mater Med 26, 223 (2015). https://doi.org/10.1007/s10856-015-5553-9

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  • DOI: https://doi.org/10.1007/s10856-015-5553-9

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