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Journal Article•DOI•

Accurate characterization of pure silicon-substituted hydroxyapatite powders synthesized by a new precipitation route

David Marchat1, Maria Zymelka1, Cristina Coelho2, Laurent Gremillard3, Lucile Joly-Pottuz3, Florence Babonneau2, Claude Esnouf3, Jérôme Chevalier3, Didier Bernache-Assollant1 •
Ecole nationale supérieure des mines de Saint-Étienne1, Pierre-and-Marie-Curie University2, University of Lyon3
01 Jun 2013-Acta Biomaterialia (Acta Biomater)-Vol. 9, Iss: 6, pp 6992-7004
TL;DR: The results, particularly those from infrared spectroscopy, raise serious reservations about the phase purity of previously prepared and biologically evaluated SiHA powders, pellets and scaffolds in the literature.
About: This article is published in Acta Biomaterialia.The article was published on 2013-06-01 and is currently open access. It has received 88 citations till now. The article focuses on the topics: Infrared spectroscopy & Fourier transform infrared spectroscopy.

Summary (1 min read)

Jump to: [1. Introduction] – [2.1 Powder synthesis] – [2.2.1 X-ray powder diffraction and Rietveld refinement] – [2.2.4 Electron microscopy (HR-TEM, SAED and EDX)] and [3.2.4 Electron microscopy]

1. Introduction

  • In order to correctly describe the physical, chemical and biological properties of SiHAs and to compare them to routinely implanted HA and β-TCP, well-characterized pure SiHAs powders first need to be prepared.
  • Therefore, this work was devoted to the development of a new route to synthesize monophasic SiHA powders with controlled stoichiometry.
  • To this purpose, a solution of soluble silicate was first prepared from TEOS via a sol-gel route, and then accurate powder analysis was carried out by means of ICP/AES, Xray powder diffraction, Rietveld refinement, high resolution electron transmission microscopy (HR-TEM) with energy dispersive spectroscopy (EDS) as well as infrared (FT-IR/ATR) and solid-state NMR spectroscopy.
  • Two pH levels of precipitation were studied, as well as six Si/P molar ratios.

2.1 Powder synthesis

  • The as-synthesized powders were heated under air using an alumina crucible.
  • The heating and cooling rate was fixed at 4°C min -1 .

2.2.1 X-ray powder diffraction and Rietveld refinement

  • Crystalline phases were identified by means of a Siemens D5000 θ/2θ X-ray diffractometer.
  • The evolution of the crystallinity of the samples after calcination at 1000°C for 15 h was evaluated by means of the full width at half maximum (FWHM) of the (211) peak at 2θ=31.8°, as it had the highest intensity and minimal overlap with neighboring peaks.

2.2.4 Electron microscopy (HR-TEM, SAED and EDX)

  • Gold was then distributed as crystallized nano-domains which were used as a reference in the selected area electron diffraction (SAED) patterns to calculate as precisely as possible the lattice parameters.
  • The SAED patterns obtained from regions with or without gold on the HA part were the same.

3.2.4 Electron microscopy

  • The results are the average of about ten intervals per pattern.
  • Moreover, other experimental patterns for different zone axes (not shown here) were obtained and compared to theoretical electron diffraction patterns calculated by means of the Java Electron Microscopy Simulation (JEMS) software [87] .
  • The results indicate that the experimental and simulated patterns are perfectly superimposed for 0.734 ≥ c/a ≥ 0.729.

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Citations
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Journal Article•DOI•
Silicon: the evolution of its use in biomaterials.

[...]

James R. Henstock1, L. T. Canham, Susan I. Anderson2•
Keele University1, University of Nottingham2
01 Jan 2015-Acta Biomaterialia
TL;DR: This review discusses the current data obtained from original research in biochemistry and biomaterials science supporting the role of silicon in bone, comparing both the biological function of the element and analysing the evolution of silicon-containing biommaterials.

150 citations

Book Chapter•DOI•
Cationic and Anionic Substitutions in Hydroxyapatite

[...]

Ilaria Cacciotti1•
Sapienza University of Rome1
01 Jan 2015

100 citations

Journal Article•DOI•
Biodegradable and Biocompatible Systems Based on Hydroxyapatite Nanoparticles

[...]

Pau Turon, Luis J. del Valle, Carlos Alemán, Jordi Puiggalí
06 Jan 2017-Applied Sciences
TL;DR: The present review is mainly focused on both the capability of HAp nanoparticles to encapsulate diverse compounds as well as the preparation methods of scaffolds incorporating HAp.
Abstract: Composites of hydroxyapatite (HAp) are widely employed in biomedical applications due to their biocompatibility, bioactivity and osteoconductivity properties. In fact, the development of industrially scalable hybrids at low cost and high efficiency has a great impact, for example, on bone tissue engineering applications and even as drug delivery systems. New nanocomposites constituted by HAp nanoparticles and synthetic or natural polymers with biodegradable and biocompatible characteristics have constantly been developed and extensive works have been published concerning their applications. The present review is mainly focused on both the capability of HAp nanoparticles to encapsulate diverse compounds as well as the preparation methods of scaffolds incorporating HAp. Attention has also been paid to the recent developments on antimicrobial scaffolds, bioactive membranes, magnetic scaffolds, in vivo imaging systems, hydrogels and coatings that made use of HAp nanoparticles.

83 citations

Journal Article•DOI•
In vitro three-dimensional bone tissue models: from cells to controlled and dynamic environment.

[...]

Guenaelle Bouet1, David Marchat, Magali Cruel, Luc Malaval, Laurence Vico •
French Institute of Health and Medical Research1
01 Feb 2015-Tissue Engineering Part B-reviews
TL;DR: This review focuses on state-of-the-art and the current advances in the development of 3D culture systems for bone biology research, and details main characteristics and challenges associated with its three main components, that is, scaffold, cells, and perfusion bioreactor systems.
Abstract: Most of our knowledge of bone cell physiology is derived from experiments carried out in vitro on polystyrene substrates However, these traditional monolayer cell cultures do not reproduce the complex and dynamic 3-dimensional (3D) environment experienced by cells in vivo Thus, there is a growing interest in the use of 3D culture systems as tools for understanding bone biology These in vitro engineered systems, less complex than in vivo models, should ultimately recapitulate and control the main biophysical, biochemical and biomechanical cues that define the in vivo bone environment, while allowing their monitoring This review focuses on state of the art and the current advances in the development of 3D culture systems for bone biology research It describes more specifically advantages related to the use of such systems, and details main characteristics and challenges associated with its three main components, ie scaffold, cells and perfusion bioreactor systems Finally, future challenges for non-invasive imaging technologies are addressed

80 citations

Journal Article•DOI•
Ionic substituted hydroxyapatite for bone regeneration applications: A review

[...]

Antonia Ressler1, Andreja Žužić1, Irena Ivanišević1, Nikhil Kamboj2, Hrvoje Ivanković1 •
University of Zagreb1, Tallinn University of Technology2
01 Jun 2021
TL;DR: In this paper, a review summarises recent and relevant studies on cationic and anionic substitutions in the HAp lattice that are commonly found in the human body.
Abstract: Biological apatites are characterised by various ionic substitutions within the HAp lattice that are crucial for bone metabolism. The introduction of key role elements within synthetic calcium phosphates (CaP), mainly hydroxyapatite (HAp), can increase osteogenesis and enhance bone regeneration process. The lattice structure of HAp enables cationic and anionic substitutions leading to the enhanced biological performance of synthetic bone graft materials. This review summarises recent and relevant studies on cationic and anionic substitutions in the HAp lattice that are commonly found in the human body. Furthermore, co-substituted HAp obtained from synthetic and biological precursors, along with their influence on the bone regeneration process, has been discussed. Finally, future perspectives for the use of substituted HAp have been presented.

77 citations

References
More filters
Journal Article•DOI•
Effect of Silicon Substitution on the Sintering and Microstructure of Hydroxyapatite

[...]

Iain R. Gibson1, Serena M. Best1, William Bonfield1•
Queen Mary University of London1
20 Dec 2004-Journal of the American Ceramic Society
TL;DR: In this article, the substitution of between 0 and 1.6 wt% silicon (Si-HA) in hydroxyapatite (HA) inhibited densification at low temperatures (1000°-1150°C), with these effects being more significant as the level of silicon substitution was increased.
Abstract: The substitution of between 0 and 1.6 wt% silicon (Si-HA) in hydroxyapatite (HA) inhibited densification at low temperatures (1000°–1150°C), with these effects being more significant as the level of silicon substitution was increased. For higher sintering temperatures (1200°–1300°C), the sintered densities of HA and Si-HA compositions were comparable. Examination of the ceramic microstructures by scanning electron microscopy (SEM) showed that silicon substitution also inhibited grain growth at higher sintering temperatures (1200°–1300°C). The negative effect of silicon substitution on the sintering of HA at low temperatures (1000°–1150°C) was reflected in the hardness values of the ceramics. However, for higher sintering temperatures, e.g., 1300°C, where sintered densities were comparable, the hardness values of Si-HA compositions were equal to or greater than that of HA, reflecting the smaller grain sizes observed for the former.

145 citations

Journal Article•DOI•
Some features of the incorporation of oxygen in different oxidation states in the apatitic lattice—I On the existence of calcium and strontium oxyapatites

[...]

J.C. Trombe, G. Montel
01 Jan 1978-Journal of Inorganic and Nuclear Chemistry
TL;DR: The existence of calcium phosphate oxyapatite has been proved in this paper, and it is shown that this compound exists only under a vacuum (10 −4 to 10 −6 torr) or in sufficiently water-free gases (He, N 2 ), in the range of temperatures 850-1050°C.

143 citations

Journal Article•DOI•
The Infrared and Raman Spectra of β-and α-Tricalcium Phosphate (Ca3(Po4)2)

[...]

A. Jillavenkatesa1, Robert A. Condrate1•
Alfred University1
01 Dec 1998-Spectroscopy Letters
TL;DR: Factor group analysis was applied to interpret the vibrational spectra of β-and α-tricalcium phosphate (Ca3(PO4)2) as discussed by the authors, which predicts the number of bands formed due to the splitting of the fundamental vibrational modes of the PO4 3-ion.
Abstract: Factor group analysis was applied to interpret the vibrational spectra of β-and α-tricalcium phosphate (Ca3(PO4)2). The analysis predicts the number of bands formed due to the splitting of the fundamental vibrational modes of the PO4 3-ion. The number of the infrared and Raman bands predicted by this analysis for the two phases are drastically different and can be ascribed to the difference in atomic arrangements in the two phases resulting in greater shielding of the PO4 3-ions in the β-phase than in the α-phase. Discrepancies in the number of predicted and experimentally-observed bands can be attributed to the weak intensities of some vibrational modes or the convolution of vibrations and limited spectral resolution.

142 citations

Journal Article•DOI•
In vivo requirement for silicon in articular cartilage and connective tissue formation in the chick.

[...]

Edith M. Carlisle1•
University of California, Los Angeles1
01 Apr 1976-Journal of Nutrition
TL;DR: Findings provide the first evidence for a requirement for silicon in articular cartilage and connective tissue formation and that the site of action of silicon is in the glycosaminoglycan-protein complexes of the ground substance.
Abstract: Studies were undertaken to determine further effects of silicon deficiency in the chick. The diet and experimental conditions were the same as those used in previous studies to demonstrate the essentiality of silicon for growth and development. Skeletal and other abnormalities involving glycosaminoglycans in formation of articular cartilage and comb connective tissue were found to be associated with silicon deficiency. The bones of 1 day-old deutectomized cockerels fed a silicon supplemented diet and killed at 4 weeks of age had significantly greater amounts of articular cartilage and water as compared with the silicon deficient group and also a greater proportion of hexosamine in the cartilage. The greater water content in bones of the silicon supplemented chicks coincided with a larger content of glycosaminoglycans in the articular cartilage. A similar relationship was obtained in cockerel comb. In addition to larger amounts of connective tissue and of total hexosamine in combs of the supplemented group, a higher percentage of hexosamine and a higher silicon content was found. These findings provide the first evidence for a requirement for silicon in articular cartilage and connective tissue formation and that the site of action of silicon is in the glycosaminoglycan-protein complexes of the ground substance.

141 citations

Journal Article•DOI•
Synthesis and characterization of single-phase silicon-substituted α-tricalcium phosphate

[...]

Joel Reid, L. Tuck1, Michael Sayer1, Karen Fargo, Jason A. Hendry •
Queen's University1
01 May 2006-Biomaterials
TL;DR: In this article, the lattice parameters of single-phase Si- α -TCP prepared with 0.87% silicon are a = 1 2.8 7 4 (1 ) A, b = 2 7.3 7 2 (2 ) A, c = 1 5.2 2 5 (1) A, and β = 12 6.3 8 ( 1 ) °.

138 citations

"Accurate characterization of pure s..." refers background or methods in this paper

  • ...The first evid nce for this was provided by the few 91 accurate analyses available in the literature which show that SiHA powders can contain 92 crystallized [16, 30-35] and amorphous [16, 34, 3638] impurities....

    [...]

  • ...107 Several methods are used to prepare Si-substituted hydroxyapatites (SiHAs), such as 108 the sol-gel route [48], resuspension processes [20, 33, 34, 63-66], solid state reactions [10, 109 67], hydrothermal techniques [17, 68, 69], mechanoc hemical methods [70], magnetron 110 sputtering [14], pulsed laser deposition [51, 71], electrophoretic deposition [72] and 111 precipitation from aqueous solutions....

    [...]

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