Synthesis and characterization of hydroxyapatite crystals: A review study on the analytical methods

Koutsopoulos, Sotirios

doi:10.1002/jbm.10280

Cited by 1,474 publications

(1,277 citation statements)

References 74 publications

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“…1A) exhibited the expected peaks (29), and XRD patterns of both hexagonal prisms (SI Appendix, Fig. S1A, red curve) and platelets (SI Appendix, Fig.…”

Section: Preparation and Characterization Of Mineral Surfacesmentioning

confidence: 97%

Energetic basis for the molecular-scale organization of bone

Tao

Battle

Pan

et al. 2014

Proc. Natl. Acad. Sci. U.S.A.

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The remarkable properties of bone derive from a highly organized arrangement of coaligned nanometer-scale apatite platelets within a fibrillar collagen matrix. The origin of this arrangement is poorly understood and the crystal structures of hydroxyapatite (HAP) and the nonmineralized collagen fibrils alone do not provide an explanation. Moreover, little is known about collagen-apatite interaction energies, which should strongly influence both the molecular-scale organization and the resulting mechanical properties of the composite. We investigated collagen-mineral interactions by combining dynamic force spectroscopy (DFS) measurements of binding energies with molecular dynamics (MD) simulations of binding and atomic force microscopy (AFM) observations of collagen adsorption on single crystals of calcium phosphate for four mineral phases of potential importance in bone formation. In all cases, we observe a strong preferential orientation of collagen binding, but comparison between the observed orientations and transmission electron microscopy (TEM) analyses of native tissues shows that only calcium-deficient apatite (CDAP) provides an interface with collagen that is consistent with both. MD simulations predict preferred collagen orientations that agree with observations, and results from both MD and DFS reveal large values for the binding energy due to multiple binding sites. These findings reconcile apparent contradictions inherent in a hydroxyapatite or carbonated apatite (CAP) model of bone mineral and provide an energetic rationale for the molecular-scale organization of bone.biomineralization | bone | protein-mineral interface | dynamic force spectroscopy B one is a natural protein-mineral composite consisting of nonstoichiometric nanometer-scale carbonated apatite crystallites inside a fibrillar protein matrix. The matrix is mainly composed of type I collagen and is organized on multiple length scales (1, 2). At the shortest scale, three polypeptide chains form a triple helix referred to as a tropocollagen molecule that is ∼300 nm in length and 1.5 nm in diameter. These helices are arranged in a quasi-hexagonal bundle in which they overlap and intertwine to form microfibrils containing "hole zones," where there is a gap between the N termini of one helix and the C termini of another (3-5). These microfibrils are further bundled both laterally and longitudinally to form native collagen (3, 4).Within this highly organized scaffold, apatite crystallites form nanometer-scale platelets (6-9) with their [001] axes preferentially aligned parallel to the fibril axis (10-15) and the platelet faces defined by {100} crystal planes (16). Recent in vitro investigations of hydroxyapatite (HAP) formation within collagen fibrils revealed a multistage process in which amorphous calcium phosphate (ACP) first infiltrated through the hole zones and then converted into HAP platelets with initial mineral deposition occurring near the hole zones (11, 13). In vitro transmission electron microscopy (TEM) and atomic force microscop...

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“…1A) exhibited the expected peaks (29), and XRD patterns of both hexagonal prisms (SI Appendix, Fig. S1A, red curve) and platelets (SI Appendix, Fig.…”

Section: Preparation and Characterization Of Mineral Surfacesmentioning

confidence: 97%

Energetic basis for the molecular-scale organization of bone

Tao

Battle

Pan

et al. 2014

Proc. Natl. Acad. Sci. U.S.A.

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“…The band assigned to P-O stretching is shifted towards higher wavenumbers in comparison to crystalline HAp (962 cm −1 ) because materials were still in an elastic or liquid form (some ethanol remained inside) during the examination [29]. The spectra were recorded after synthesis of the sols and after 24 hours of drying.…”

Section: Resultsmentioning

confidence: 99%

Examination of Sol-Gel Derived Hydroxyapatite Enhanced with Silver Nanoparticles using OCT and Raman Spectroscopy

Głowacki

Gnyba

Strąkowska

et al. 2017

Metrology and Measurement Systems

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Hydroxyapatite (HAp) has been attracting widespread interest in medical applications. In a form of coating, it enables to create a durable bond between an implant and surrounding bone tissues. With addition of silver nanoparticles HAp should also provide antibacterial activity. The aim of this research was to evaluate the composition of hydroxyapatite with silver nanoparticles in a non-destructive and non-contact way. For control measurements of HAp molecular composition and solvent evaporation efficiency the Raman spectroscopy has been chosen. In order to evaluate dispersion and concentration of the silver nanoparticles inside the hydroxyapatite matrix, the optical coherence tomography (OCT) has been used. Five samples were developed and examineda reference sample of pure HAp sol and four samples of HAp colloids with different silver nanoparticle solution volume ratios. The Raman spectra for each solution have been obtained and analyzed. Furthermore, a transversesectional visualization of every sample has been created and examined by means of OCT.

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“…The peaks at 3437 and 1637 cm -1 are relative to the bending modes of the hydroxyl group in the adsorbed water, while the peaks at 3571 and 633 cm -1 are assigned to the stretching vibration of the hydroxyl group in the crystalline structure of HAp. 33,35,40,[50][51][52][53][54][55][56][57] From Figure S1, it can be seen that, with decreasing degree of crystallinity, the intensity of the absorption bands appearing at 3437 and 1637 cm -1 increases, while the intensity of the bands at 3571 and 633 cm -1 decreases. Therefore, according to the results presented here, the change in the intensity of the aforementioned peaks could be used as an alternative to the XRD patterns for determination of the degree of crystallinity.…”

Section: The Fraction Of the Crystalline Phase In Hap Nanoparticlesmentioning

confidence: 99%

“…Moreover, the weak peaks at 1400-1600 cm -1 , associated with the carbonate ν 3 absorption band, indicate the presence of low amounts of carbonate impurities in the structure of HAp. [53][54][55][56][57][58][59][60][61] According to the IR spectra, the intensity of these peaks increased as the crystalline fraction decreased. Therefore, the presence of carbonate in the apatite lattice causes a decrease in crystallinity.…”

Section: The Fraction Of the Crystalline Phase In Hap Nanoparticlesmentioning

confidence: 99%

“…Meanwhile the weak peak at about 873 cm -1 may be attributed to the carbonate groups or low amount of hydrogen phosphate in the crystalline structure of HAp. [53][54][55] Further analysis of the IR spectra in the region of 1400-1600 cm -1 provided information on the sites in which the carbonate groups were substituted. Although the published data in the literature has led to some contradictory explanations regarding which bands correspond to the A-type (carbonate replacing OH -ions), B-type (carbonate replacing PO 4 3-ions), or mixed AB-type carbonate substitution, the results of IR analysis in recent studies [53][54][55][58][59][60] indicate that the nanoparticles synthesized in the present work correspond mostly to a mixed AB-type substitutions of CO 3 2-in the hydroxyapatite lattice along with the predominance of B-type substitution.…”

Section: The Fraction Of the Crystalline Phase In Hap Nanoparticlesmentioning

confidence: 99%

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Design of experiments (DOE) for the optimization of hydrothermal synthesis of hydroxyapatite nanoparticles

Sadat‐Shojai¹,

Atai²,

Nodehi³

2011

J. Braz. Chem. Soc.

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O objetivo deste trabalho foi investigar a influência de diversos parâmetros de reação sobre as propriedades de nanopartículas de hidroxiapatita (HAp) preparadas pelo método hidrotérmico. Os dados da literatura descrevem condições experimentais variadas para a síntese hidrotérmica de HAp. Uma abordagem específica foi então utilizada para avaliar os fatores estatisticamente influentes entre aqueles descritos na literatura. O papel de cada parâmetro experimental também foi discutido no contexto da nucleação de partículas e do mecanismo de crescimento de cristais. Dentro das variáveis selecionadas, temperatura e pH foram os fatores que mais afetaram a composição e morfologia da HAp. Além disso, neste estudo, diferentes morfologias variando de nanopartículas cilíndricas do tipo bastonete a esféricas com várias características foram obtidas com sucesso, o que pode ser aplicável na preparação de várias biocerâmicas de HAp.The aim of this work was to investigate the influence of different reaction parameters on the properties of hydroxyapatite (HAp) nanoparticles prepared by the hydrothermal method. The literature data describe widely different experimental conditions for the hydrothermal synthesis of HAp. A specific approach was therefore used to evaluate the statistically influential factors among those described in the literature. The role of each experimental parameter was also discussed within the framework of particle nucleation and crystal growth mechanism. Among the selected variables, temperature and pH were found to be the most significant factors affecting the composition and morphology of the HAp. Moreover, in the present study, different morphologies ranging from rod-like to spherical nanoparticles with various characteristics were successfully obtained, which can be applicable for the preparation of various HAp bioceramics.

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Synthesis and characterization of hydroxyapatite crystals: A review study on the analytical methods

Cited by 1,474 publications

References 74 publications

Energetic basis for the molecular-scale organization of bone

Energetic basis for the molecular-scale organization of bone

Examination of Sol-Gel Derived Hydroxyapatite Enhanced with Silver Nanoparticles using OCT and Raman Spectroscopy

Design of experiments (DOE) for the optimization of hydrothermal synthesis of hydroxyapatite nanoparticles

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