Hydrothermal synthesis of hydroxyapatite powders using Response Surface Methodology (RSM)

Ebrahimi, Shamsi; Sipaut, Coswald Stephen; Arshad, Sazmal Effendi

doi:10.1371/journal.pone.0251009

Cited by 35 publications

(17 citation statements)

References 36 publications

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“…It is well known that crystalline hydroxyapatite can be obtained using the hydrothermal method in a relatively wide temperature range (from 70 °C to 200 °C) [ 4 , 44 , 45 , 46 ]. An important advantage of using the hydrothermal process for HAp synthesis, besides controlled morphology and nanometer particle size, is that no hydroxyl defects are produced in the structure [ 44 ].…”

Section: Resultsmentioning

confidence: 99%

Hydroxyapatite from Natural Sources for Medical Applications

et al. 2022

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The aim of this work is to study the physical-chemical, mechanical, and biocompatible properties of hydroxyapatite obtained by hydrothermal synthesis, at relatively low temperatures and high pressures, starting from natural sources (Rapana whelk shells), knowing that these properties influence the behavior of nanostructured materials in cells or tissues. Thus, hydroxyapatite nanopowders were characterized by chemical analysis, Fourier-transform infrared spectroscopy (FT-IR), dynamic light scattering (DLS), scanning electron microscopy (SEM), and X-ray diffraction (XRD). In vitro studies on osteoblast cell lines (cytotoxicity and cell proliferation), as well as preliminary mechanical tests, have been performed. The results showed that the obtained powders have a crystallite size below 50 nm and particle size less than 100 nm, demonstrating that hydrothermal synthesis led to hydroxyapatite nanocrystalline powders, with a Ca:P ratio close to the stoichiometric ratio and a controlled morphology (spherical particle aggregates). The tensile strength of HAp samples sintered at 1100 °C/90 min varies between 37.6–39.1 N/mm2. HAp samples sintered at 1300 °C/120 min provide better results for the investigated mechanical properties. The coefficient of friction has an appropriate value for biomechanical applications. The results of cell viability showed that the cytotoxic effect is low for all tested samples. Better cell proliferation is observed for osteoblasts grown on square samples.

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Section: Resultsmentioning

confidence: 99%

Hydroxyapatite from Natural Sources for Medical Applications

et al. 2022

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“…HAp was synthesized based on our previous paper [16] with a hydrothermal method using two raw materials (Merck, Darmstad, Germany): Ca(NO 3 ) 2 .4H 2 O as calcium precursor and (NH4) 2 HPO 4 as phosphate precursor (Equation ( 1)). In summary, 4.723 g (1 M) of Ca(NO 3 ) 2 .4H 2 O and 1.584 g (0.67M) of (NH4) 2 HPO 4 were dissolved in 20 mL of deionized water.…”

Section: Synthesis Of Hapmentioning

confidence: 99%

Synthesis of Hydroxyapatite/Bioglass Composite Nanopowder Using Design of Experiments

Ebrahimi

Sipaut

2022

Nanomaterials

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Composite scaffolds of hydroxyapatite (HAp) nanoparticles and bioactive glass (BG) were applied as an appropriate selection for bone tissue engineering. To this end, HAp/BG composite was synthesized by a hydrothermal method using Design of Experiments (DOE) with a combined mixture–process factor design for the first time. The input variables were hydrothermal temperature at three levels (i.e., 100, 140, 180 °C) as a process factor and two mixture components in three ratios (i.e., HAp 90, 70, 50; BG 50, 30, 10). The degree of crystallinity and crystal size in the composite were the output variables. XRD showed that only a small fraction of BG was crystallized and that a wollastonite phase was produced. The XRD results also revealed that incorporation of Si into the HAp structure inhibited HAp crystal growth and restricted its crystallization. The FTIR results also showed that the intensity of the hydroxyl peak decreased with the addition of silicon into the HAp structure. DOE results showed that the weight ratio of the components strongly influenced the crystal size and crystallinity. SEM and FTIR results identified the greatest bioactivity and apatite layer formation in the Si-HAp sample with an HAp70/BG30 ratio after 14 days immersion in simulated body fluid (SBF) solution, as compared to other ratios and HAp alone. Therefore, the combination of HAp and BG was able to yield a HAp/BG composite with significant bioactivity.

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“…HAp and HAp/BG powders were synthesized based on our previous papers [22,23]. Briefly: HAp nano-powder was synthesized by the hydrothermal method using Ca(NO 3 ) 2 •4H 2 O and (NH 4 ) 2 HPO 4 as starting materials, with stoichiometric ratio Ca/P = 1.67.…”

Section: Fabrication Of Hap and Its Composite Cementsmentioning

confidence: 99%

The Effect of Liquid Phase Concentration on the Setting Time and Compressive Strength of Hydroxyapatite/Bioglass Composite Cement

Ebrahimi

Sipaut

2021

Nanomaterials

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Composite scaffolds of hydroxyapatite (HAp) nanoparticles and bioactive glass (BG) have been applied as appropriate materials for bone tissue engineering. In this study, hydroxyapatite/bioglass cement in different ratios was successfully fabricated. To prepare HAp and HAp/BG cement, synthesized HAp and HAp/BG powder were mixed in several ratios, using different concentrations of sodium hydrogen phosphate (SP) and water as the liquid phase. The liquid to powder ratio used was 0.4 mL/g. The results showed that setting time increased with BG content in the composite. The results also showed that with the addition of bioglass to the HAp structure, the density decreased and the porosity increased. It was also found that after immersion in simulated body fluid (SBF) solution, the compressive strength of the HAp and HAp/BG cements increased with BG concentration up to 30 wt.%. SEM results showed the formation of an apatite layer in all selected samples after immersion in SBF solution. At 30 wt.% BG, greater nucleation and growth of the apatite layer were observed, resulting in higher bioactivity than pure HAp and HAp/BG in other ratios.

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Hydrothermal synthesis of hydroxyapatite powders using Response Surface Methodology (RSM)

Cited by 35 publications

References 36 publications

Hydroxyapatite from Natural Sources for Medical Applications

Hydroxyapatite from Natural Sources for Medical Applications

Synthesis of Hydroxyapatite/Bioglass Composite Nanopowder Using Design of Experiments

The Effect of Liquid Phase Concentration on the Setting Time and Compressive Strength of Hydroxyapatite/Bioglass Composite Cement

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