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Journal of Advanced Ceramics 2013, 2(3): 274-284 https://doi.org/10.1007/s40145-013-0072-y
Research Article | Open Access | Issue | Published: 07 September 2013

Sintering effects on chemical and physical properties of bioactive ceramics

Show Author's Information Lukasz WITEKa,b,*( ),  James SMAYa,  Nelson R. F. A. SILVAc,  Teja GUDAd,  Joo L. ONGd,  Paulo G. COELHOb,e
School of Chemical Engineering, Oklahoma State University, 423 Engineering North, Stillwater, OK, USA
Department of Operative Dentistry, Universidade Federal de Minas Gerais, Pampulha, Belo Horizonte, MG, Brazil
Department of Biomedical Engineering, University of Texas San Antonio, One UTSA Circle, San Antonio, TX, USA
Department of Biomaterials and Biomimetics, New York University, 345 East 24th Street, 804S New York, NY, USA
Department of Periodontology and Implant Dentistry, College of Dentistry, New York University, 345 East 24th Street, New York, NY, USA
Keywords:
sintering, bone graft material, chemical/physical characterization, bi-phasic calcium phosphate (BCP)
Cite this article:
WITEK L, SMAY J, SILVA NRFA, et al. Sintering effects on chemical and physical properties of bioactive ceramics. Journal of Advanced Ceramics, 2013, 2(3): 274-284. https://doi.org/10.1007/s40145-013-0072-y
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Abstract Full text About this article

The objective of this study was to characterize the chemical and physical properties of bioactive ceramics prepared from an aqueous paste containing hydroxyapatite (HA) and beta tri-calcium phosphate (β-TCP). Prior to formulating the paste, HA and β-TCP were calcined at 800 ℃ and 975 ℃ (11 h), milled, and blended into 15%/85% HA/β-TCP volume-mixed paste. Fabricated cylindrical rods were subsequently sintered to 900 ℃, 1100 ℃ or 1250 ℃. The sintered specimens were characterized by helium pycnometry, X-ray diffraction (XRD), Fourier transform-infrared (FT-IR), and inductively coupled plasma (ICP) spectroscopy for evaluation of porosity, crystalline phase, functional-groups, and Ca:P ratio, respectively. Mechanical properties were assessed via 3-point bending and diametral compression. Qualitative microstructural evaluation using scanning electron microscopy (SEM) showed larger pores and a broader pore size distribution (PSD) for materials sintered at 900 ℃ and 1100 ℃, whereas the 1250 ℃ samples showed more uniform PSD. Porosity quantification showed significantly higher porosity for materials sintered to 900 ℃ and 1250 ℃ (p < 0.05). XRD indicated substantial deviations from the 15%/85% HA/β-TCP formulation following sintering where lower amounts of HA were observed when sintering temperature was increased. Mechanical testing demonstrated significant differences between calcination temperatures and different sintering regimes (p < 0.05). Variation in chemical composition and mechanical properties of bioactive ceramics were direct consequences of calcination and sintering.


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About this article

Sintering effects on chemical and physical properties of bioactive ceramics

Show Author's information Lukasz WITEKa,b,*( ), James SMAYa, Nelson R. F. A. SILVAc, Teja GUDAd, Joo L. ONGd, Paulo G. COELHOb,e
School of Chemical Engineering, Oklahoma State University, 423 Engineering North, Stillwater, OK, USA
Department of Operative Dentistry, Universidade Federal de Minas Gerais, Pampulha, Belo Horizonte, MG, Brazil
Department of Biomedical Engineering, University of Texas San Antonio, One UTSA Circle, San Antonio, TX, USA
Department of Biomaterials and Biomimetics, New York University, 345 East 24th Street, 804S New York, NY, USA
Department of Periodontology and Implant Dentistry, College of Dentistry, New York University, 345 East 24th Street, New York, NY, USA

Abstract

The objective of this study was to characterize the chemical and physical properties of bioactive ceramics prepared from an aqueous paste containing hydroxyapatite (HA) and beta tri-calcium phosphate (β-TCP). Prior to formulating the paste, HA and β-TCP were calcined at 800 ℃ and 975 ℃ (11 h), milled, and blended into 15%/85% HA/β-TCP volume-mixed paste. Fabricated cylindrical rods were subsequently sintered to 900 ℃, 1100 ℃ or 1250 ℃. The sintered specimens were characterized by helium pycnometry, X-ray diffraction (XRD), Fourier transform-infrared (FT-IR), and inductively coupled plasma (ICP) spectroscopy for evaluation of porosity, crystalline phase, functional-groups, and Ca:P ratio, respectively. Mechanical properties were assessed via 3-point bending and diametral compression. Qualitative microstructural evaluation using scanning electron microscopy (SEM) showed larger pores and a broader pore size distribution (PSD) for materials sintered at 900 ℃ and 1100 ℃, whereas the 1250 ℃ samples showed more uniform PSD. Porosity quantification showed significantly higher porosity for materials sintered to 900 ℃ and 1250 ℃ (p < 0.05). XRD indicated substantial deviations from the 15%/85% HA/β-TCP formulation following sintering where lower amounts of HA were observed when sintering temperature was increased. Mechanical testing demonstrated significant differences between calcination temperatures and different sintering regimes (p < 0.05). Variation in chemical composition and mechanical properties of bioactive ceramics were direct consequences of calcination and sintering.

Keywords: sintering, bone graft material, chemical/physical characterization, bi-phasic calcium phosphate (BCP)

References(27)

[1]
Stoll C, Mengsteab S, Stoll D, et al. Analysis of polymorphic TGFB1 codons 10, 25, and 263 in a German patient group with non-syndromic cleft lip, alveolus, and palate compared with healthy adults. BMC Med Genet 2004, 5: 15.
DOI Google Scholar
[2]
Seitz H, Rieder W, Irsen S, et al. Three-dimensional printing of porous ceramic scaffolds for bone tissue engineering. J Biomed Mater Res B: Appl Biomater 2005, 74B: 782-788.
DOI Google Scholar
[3]
Moore WR, Graves SE, Bain GI. Synthetic bone graft substitutes. ANZ J Surg 2001, 71: 354-361.
DOI Google Scholar
[4]
Kivrak N, Taş AC. Synthesis of calcium hydroxyapatite–tricalcium phosphate (HA–TCP) composite bioceramic powders and their sintering behavior. J Am Ceram Soc 1998, 81: 2245-2252.
DOI Google Scholar
[5]
Daculsi G, LeGeros RZ. Tricalcium phosphate/hydroxyapatite biphasic ceramics. In Bioceramics and Their Clinical Applications. Kokubo T, Ed. Cambridge, UK: Woodhead Publishing, 2008: 395-423.
DOI
[6]
LeGeros RZ, LeGeros JP. Hydroxyapatite. In Bioceramics and Their Clinical Applications. Kokubo T, Ed. Cambridge, UK: Woodhead Publishing, 2008: 367-394.
DOI
[7]
Smay J. Dissolution of CaS filled, HA:beta-TCP scaffolds with hierarchical pore network. IADR, Miami, FL, USA, 2009: 1-16.
[8]
Rey C, Combes C, Drouet C. Tricalcium phosphate-based ceramics. In Bioceramics and Their Clinical Applications. Kokubo T, Ed. Cambridge, UK: Woodhead Publishing, 2008: 326-366.
DOI
[9]
Pines M, Witek L, Clark E, et al. Flexural strength of degradable 3-D scaffolds for critical bone repair. IADR, Barcelona, Spain, 2010. Available at https://iadr.confex.com/iadr/2010barce/preliminaryprogram/abstract_133134.htm.
[10]
Moore JR, Phillips TW, Weiland AJ, et al. Allogenic transplants of bone revascularized by microvascular anastomoses: A preliminary study. J Orthop Res 1983, 1: 352-360.
DOI Google Scholar
[11]
Cretiu-Vasiliu CE. Assembly of hydroxyl apatite: β-tricalcium phosphate: Calcium sulfate bone eingineering scaffolds. Master Thesis. Stillwater, OK, USA: Oklahoma State University, 2008.
[12]
Smay JE, Cesarano J III, Lewis JA. Colloidal inks for directed assembly of 3-D periodic structures. Langmuir 2002, 18: 5429-5437.
DOI Google Scholar
[13]
Guda T, Walker JA, Singleton BM, et al. Guided bone regeneration in long-bone defects with a structural hydroxyapatite graft and collagen membrane. Tissue Eng Part A 2012, .
DOI Google Scholar
[14]
Mijares DQ. Synthetic bone mineral (SBM): Prevention of bone loss induced by estrogen deficiency in a rat model. Master Thesis. New York, NY, USA: New York University, 2009.
[15]
Young RA. The Rietveld Method. Oxford, UK: Oxford University Press, 1995.
[16]
Taylor JC. Rietveld Made Easy: A Practical Guide to the Understanding of the Method and Successful Phase Quantifications. Sietronics Pty Limited, 2003.
[17]
Coelho PG, Coimbra ME, Ribeiro C, et al. Physico/chemical characterization and preliminary human histology assessment of a β-TCP particulate material for bone augmentation. Mat Sci Eng C 2009, 29: 2085-2091.
DOI Google Scholar
[18]
Fell JT, Newton JM. Determination of tablet strength by the diametral-compression test. J Pharm Sci 1970, 59: 688-691.
DOI Google Scholar
[19]
Miranda P, Saiz E, Gryn K, et al. Sintering and robocasting of β-tricalcium phosphate scaffolds for orthopaedic applications. Acta Biomater 2006, 2: 457-466.
DOI Google Scholar
[20]
Kong Y-M, Kim H-E, Kim H-W. Phase conversion of tricalcium phosphate into Ca-deficient apatite during sintering of hydroxyapatite–tricalcium phosphate biphasic ceramics. J Biomed Mater Res B: Appl Biomater 2008, 84B: 334-339.
DOI Google Scholar
[21]
Hench LL, Wilson J. An Introduction to Bioceramics. Singapore: World Scientific, 1993.
DOI
[22]
Greiner-Wronowa E, Paluszkiewicz C, Stoch L. Applying FTIR spectroscopy in the study of archeometric sensor glasses. J Mol Struct 1999, 511–512: 199-204.
DOI Google Scholar
[23]
LeGeros RZ. Properties of osteoconductive biomaterials: Calcium phosphates. Clin Orthop Relat Res 2002, 395: 81-98.
DOI Google Scholar
[24]
LeGeros RZ, Lin S, Rohanizadeh R, et al. Biphasic calcium phosphate bioceramics: Preparation, properties and applications. J Mater Sci: Mater M 2003, 14: 201-209.
Google Scholar
[25]
Raynaud S, Champion E, Bernache-Assollant D, et al. Calcium phosphate apatites with variable Ca/P atomic ratio I. Synthesis, characterisation and thermal stability of powders. Biomaterials 2002, 23: 1065-1072.
DOI Google Scholar
[26]
Lewis KN, Thomas MV, Puleo DA. Mechanical and degradation behavior of polymer-calcium sulfate composites. J Mater Sci: Mater M 2006, 17: 531-537.
DOI Google Scholar
[27]
Martin RI, Brown PW. Mechanical properties of hydroxyapatite formed at physiological temperature. J Mater Sci: Mater M 1995, 6: 138-143.
DOI Google Scholar
Publication history
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Acknowledgements
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Publication history

Received: 01 March 2013
Revised: 16 May 2013
Accepted: 13 June 2013
Published: 07 September 2013
Issue date: September 2013

Copyright

© The author(s) 2013

Acknowledgements

Professor Van Thompson from King's College London Dental Institute (https://kclpure.kcl.ac.uk/portal/van. thompson.html) is gratefully acknowledged for his guidance as well as for putting this group of authors together to complete this work and manuscript.

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Open Access: This article is distributed under the terms of the Creative Commons Attribution Noncommercial License which permits any noncommercial use, distribution, and reproduction in any medium, provided the original author(s) and source are credited.

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