Effect of the temperature and sintering time on the thermal, structural, morphological, and vibrational properties of hydroxyapatite derived from pig bone

Ramirez-Gutierrez, C.F.; Londoño‐Restrepo, Sandra M.; Real, Alicia Del; Mondragón, M.A.; Rodríguez‐García, Mario E.

doi:10.1016/j.ceramint.2017.03.046

Cited by 69 publications

(34 citation statements)

References 12 publications

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“…Raw samples were labeled as B‐Raw for bovine, P‐Raw for porcine, and H‐Raw for the human. Afterward, the samples were incinerated at the same time using a Felisa (Mexico) furnace at 720 °C at a heating rate of 6°C/min and a sintering time of 10 min and later cooled inertially into the furnace in the presence of air . The annealed samples were labeled as B‐720 for bovine, P‐720 for porcine, and H‐720 for the human.…”

Section: Methodsmentioning

confidence: 99%

Effect of the crystal size on the infrared and Raman spectra of bio hydroxyapatite of human, bovine, and porcine bones

Londoño‐Restrepo

Zubieta‐Otero

Jeronimo‐Cruz

et al. 2019

J Raman Spectroscopy

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The optical properties of hydroxyapatites (HAps) and bio HAps have been studied using Raman and infrared (IR) spectroscopies to describe their crystalline quality. However, the size of the HAp crystals and their crystalline order effects have not been considered yet. This paper focuses on the study of the effect of the change in the crystallites size have on the width of the IR and Raman spectra for defatted and deproteinized bones as well as incinerated biogenic HAp obtained from bovine, porcine, and human bones. Bone samples were analyzed through Raman and IR spectroscopies, X‐ray diffraction (XRD), transmission electron microscopy (TEM), inductively coupled plasma (ICP), and scanning electron microscopy (SEM). The Raman and IR spectra for raw samples showed broad bands but, after calcination at 720 °C, became narrow and well defined. TEM images showed that all raw crystallites are ordered nanoplates contrary to the so far well‐established concept that biogenic HAps have low crystalline quality. XRD data confirmed that raw samples display broad peaks that correlated with the HRTEM images of ordered nanocrystals. This fact confirmed that the broad Raman and IR bands of raw clean bones come from nanocrystal plates. SEM analysis confirmed the increase in the crystal size after calcination from nanomicron to submicron dimensions due to a coalescence phenomenon. These results imply that the interpretation of Raman and IR spectra in the case of HAp nanoparticles has been erroneous. These results contribute to the design of biomaterials for tissue engineering based on biogenic HAp for bone regeneration.

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Section: Methodsmentioning

confidence: 99%

Effect of the crystal size on the infrared and Raman spectra of bio hydroxyapatite of human, bovine, and porcine bones

Londoño‐Restrepo

Zubieta‐Otero

Jeronimo‐Cruz

et al. 2019

J Raman Spectroscopy

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“…Other studies also found that bovine‐derived bone grafts may decompose when annealed at 1100 °C, 1200 °C, or 1300 °C for 2 h. In our study, the crystallinity degree and crystallite size were similar among groups with different annealing temperatures, which could be partly explained by the diverse sintering time used in this study. Under steady conditions, a longer sintering time is equivalent to the effect of higher temperature …”

Section: Resultsmentioning

confidence: 99%

“…Under steady conditions, a longer sintering time is equivalent to the effect of higher temperature. 18 The surface morphology of bovine-derived bone grafts reported varied as the thermal treatment differed. Niakan et al suggested sintering at 750 C as the optimum temperature compared with 600 C and 900 C, with clearly visible natural interconnected porous structure.…”

Section: Discussionmentioning

confidence: 99%

The optimization of sintering treatment on bovine‐derived bone grafts for bone regeneration: in vitro and in vivo evaluation

Lin

et al. 2019

J Biomed Mater Res

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Modifications of sintering temperature and treatment time of bovine‐derived bone grafts affect their physicochemical properties and further influence biological activity. Three different temperature sintered bovine‐derived bone grafts: group I (300 °C 3 h), group II (300 °C 3 h plus 530 °C 6 h), and group III (300 °C 3 h plus 1000 °C 2 h) and Bio‐Oss® were characterized and then compared in vitro for their effects on bone marrow stromal cells (BMSCs) migration, proliferation, and differentiation as estimated by cell migration assay, Alkaline phosphatase (ALP) activity assay, and Alizarin red staining. Further, the four bone grafts were implanted into the calvarial defects of rabbits to evaluate bone regeneration and graft degradation. The four deproteinized bovine‐derived bone grafts displayed different surface topography. Group II displayed the highest potential of attracting cells. Both groups I and II markedly promote BMSCs differentiation. After 6 and 12 weeks, defects grafted with groups I and II displayed a significant higher bone fraction than defects grafted with group III and Bio‐Oss®. Bone graft remnants remained in all four groups. Taken together, sintering at 300 °C for 3 h and sintering at 300 °C for 3 h with an addition of 530 °C for 6 h of bovine‐dervied bone grafts displayed potential use in bone regeneration. © 2019 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 108B:272–281, 2020.

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“…Afterward, the samples were incinerated at the same time using a Felisa (Mexico) furnace at 720 °C at a heating rate of 6 °C/min and a sintering time of 10 min as is shown in the thermal profile (Fig. 1) and later cooled inertially into the furnace in presence of air (20, 21). The annealed samples were labeled as B-720 for bovine, P-720 for porcine, and H-720 for human.…”

Section: Methodsmentioning

confidence: 99%

Effect of the Crystal Size of Biogenic Hydroxyapatites on IR and Raman Spectra

Londoño‐Restrepo

Zubieta‐Otero

Jeronimo‐Cruz

et al. 2018

Preprint

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19This work focuses on the analysis of the impact that raw and calcined biogenic 20 hydroxyapatite crystal size has on the Raman and infrared spectra. To this end, bovine, 21 porcine, and human bones samples were defatted and deproteinized as well as calcinated at 22 720°C and then analyzed through Raman and Infrared spectroscopies, Transmission 23 Electron Microscopy (TEM), Inductively Coupled Plasma (ICP), and Scanning Electron 24 Microscopy (SEM). Raman and IR spectra for raw samples showed broad bands while after 25 calcination bands became narrow and well defined. TEM images showed that all raw 26 crystallites are nano-plates with a high crystalline quality contrary to the so far well-27 established concept that biogenic hydroxyapatites have low crystalline quality. This fact 28 confirmed that the broad Raman and infrared bands of raw clean bones come from 29 nanocrystal-plates. SEM analysis confirmed the increase in the size of the crystals after 30 calcination from nano to sub-micron dimensions due to a coalescence phenomenon. 31 32 33 34 35 36 37 38 39 40Nowadays bio-ceramic materials like hydroxyapatites are growing in importance in 41 different fields, particularly in tissue engineering for medical and dental applications. The 42 hydroxyapatite obtained from natural sources is called bio-hydroxyapatite (BIO-HAp), and 43 its main difference with synthetic apatites is that it is a carbonated hydroxyapatite which 44 contains other elements such as Na, Mg, Mn, Fe, among others (1, 2). 45The physicochemical characterization of raw bone as well as BIO-HAp obtained through 46 different methodologies is still an open problem due to the complexity of the material. 47Infrared and Raman spectroscopies have been extensively used to study these materials to 48 monitor the removal of the organic matrix from the mineral phase as well as to identify 49 different mineral phases and to study the changes in the crystalline quality of HAp caused 50 by thermal processes (3, 4). However, no studies about the influence of the crystal size on 51 the vibrational properties of synthetic and natural hydroxyapatites have been reported in 52 detail. Usually, when these spectroscopies are used to study the vibrational states in 53 synthetic and natural hydroxyapatites (5), the full width at the half maximum (FWHM) of a 54 characteristic peak is used to determine the crystalline quality of HAp crystals and for 55 clinical diagnostic (6). However, this criterion must be discussed in detail in the case of 56 nanostructures. 57It is well established in the literature that nanosized crystals produce wider Raman bands 58 than micro-sized ones as can be found for semiconductors as Si (7, 8). The phonon 59 confinement model has been proposed to explain Raman spectra in nanosized systems 60 because the surface states must be considered (9-12). According to Gao et al. (13), the 61 underlying mechanism behind the size-dependent Raman shifts is still quite controversial 62 and an open problem. They proposed a theoretical method to explain th...

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Effect of the temperature and sintering time on the thermal, structural, morphological, and vibrational properties of hydroxyapatite derived from pig bone

Cited by 69 publications

References 12 publications

Effect of the crystal size on the infrared and Raman spectra of bio hydroxyapatite of human, bovine, and porcine bones

Effect of the crystal size on the infrared and Raman spectra of bio hydroxyapatite of human, bovine, and porcine bones

The optimization of sintering treatment on bovine‐derived bone grafts for bone regeneration: in vitro and in vivo evaluation

Effect of the Crystal Size of Biogenic Hydroxyapatites on IR and Raman Spectra

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