Powder X-ray diffraction studies of hydroxyapatite and β-TCP mixtures processed by high energy dry milling

Kostov‐Kytin, Vladislav; Dyulgerova, Elena; Ilieva, Radost; Petkova, V.

doi:10.1016/j.ceramint.2018.02.094

Cited by 19 publications

(15 citation statements)

References 19 publications

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“…XRD analysis of the second batch of products (WH-4, WH-5 and WH-6) is shown in Figure 3. XRD diffractogram of WH-4 shows the maximum peaks of hydroxyapatite (JCDPS 00-009-0432), β-TCP WH (JCDPS 00-009-0169) [19,41] and some of TCMP (JCDPS 01-077-6692) [26,30] XRD analysis of the second batch of products (WH-4, WH-5 and WH-6) is shown in Figure 3. XRD diffractogram of WH-4 shows the maximum peaks of hydroxyapatite (JCDPS 00-009-0432), β-TCP WH (JCDPS 00-009-0169) [19,41] and some of TCMP (JCDPS 01-077-6692) [26,30].…”

Section: Resultsmentioning

confidence: 99%

Synthesis, Characterization and Process Optimization of Bone Whitlockite

et al. 2020

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Whitlockite, being the second most abundant bio-mineral in living bone, finds huge applications in tissue regeneration and implants and its synthesis into its pure form has remained a challenge. Although precipitation of whitlockite phase has been reported recently in many publications, effects of various parameters to control such phase as well as conditions for the bulk preparation of this extremely important bio-mineral have not been investigated so far. In this work, we report the precipitation of pure whitlockite phase using common precursors. As reported in the literature, whitlockite is stable in a narrow pH range, therefore; optimization of pH for the stabilization of whitlockite phase has been investigated. Additionally, in order to narrow down the optimum conditions for the whitlockite precipitation, effect of temperature and heating conditions has also been studied. The obtained solids were characterized using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). From PXRD analysis, it was observed that heating the precursor’s mixture at 100 °C with subsequent aging at the optimized pH resulted in the precipitation of pure whitlockite phase. These results were further confirmed by TGA, SEM and Raman spectroscopy analysis and it was confirmed that the conditions reported here favor whitlockite precipitation without formation of any secondary phase. These reaction conditions were further confirmed by changing all the parameters like aging, heating time, feed rate of precursors one by one. From PXRD analysis of these samples, it was concluded that not only pH but temperature, heating time, aging time and feed rate effect simultaneously on the precipitation of pure whitlockite phase and a subtle change in any of these parameters could lead to the formation of undesired stable secondary calcium phosphate phases.

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Section: Resultsmentioning

confidence: 99%

Synthesis, Characterization and Process Optimization of Bone Whitlockite

et al. 2020

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“…Figure 1 shows the characteristic XRD spectra for all samples. When all the prepared samples were analyzed by X-ray diffraction, their patterns were characteristic of the hexagonal apatite phase [28,29]. Few XRD peaks are characteristic of carbonated hydroxyapatite (with 2θ from 26-40) ( Figure 1).…”

Section: Crystal Structurementioning

confidence: 99%

Ion-Substituted Carbonated Hydroxyapatite Coatings for Model Stone Samples

et al. 2019

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Carbonated hydroxyapatite derivatives (CHAp) and its metallic derivatives (Ag, Sr, Ba, K, Zn) have been prepared and characterized in this paper and their coating capacity on some model stone samples have been evaluated and discussed. These compounds were characterized by using several analytical tools, including X-ray diffraction analysis (XRD), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), to determine the purity of the CHAp sample. The XRD and FTIR results confirmed the presence of AB-carbonated type CHAp. The thermal analysis (TGA) established two stages of weight loss that occured during the heating process: The first weight loss between 30–225 °C corresponding to the partial carbonate release from OH-channel and the second one between 226–700 °C, corresponding to some thermal reactions, possibly to the generation of calcium phosphate. The efficiency and suitability of these products on model stone samples were evaluated by monitoring the resistance to artificial weather (freeze–thaw), and pore structure changes (surface area, pore volume, pore diameter). Meanwhile, optical microscopy (OM) and Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM–EDS) techniques showed the particles size and surface morphology of the samples, as well as information on its chemical composition. Also, the compressive strength of these new compounds as coatings revealed a homogeneity and strengthen of these model stone samples.

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“…The composition and crystallinity of the biologically generated minerals were analyzed with an X-ray diffractometer [ 30 , 31 ]. The atomic composition of the extracted nanocrystals was genuine HAP, Ca 10 (PO 4 ) 6 (OH) 2 ; the atomic composition of the commercial bony nanoparticles was identified as calcium phosphate hydrates, Ca 3 (PO 4 ) 2 ∙xH 2 O ( Figure 6 ).…”

Section: Resultsmentioning

confidence: 99%

Innate Biomineralization

Tian

Watanabe

Martin

et al. 2020

IJMS

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In vertebrates, biomineralization is a feature considered unique to mature osteoblasts and odontoblasts by which they synthesize hydroxyapatite (HAP), which is deposited in the collagen matrix to construct endoskeleton. For many decades, the mechanisms that modulate differentiation and maturation of these specialized cells have been sought as a key to understanding bone-remodeling defects. Here, we report that biomineralization is an innate ability of all mammalian cells, irrespective of cell type or maturation stage. This innate biomineralization is triggered by the concomitant exposure of living cells to three indispensable elements: calcium ion, phosphoester salt, and alkaline phosphatase. Any given somatic cell, including undifferentiated mononuclear cells, can undergo a biomineralization process to produce calcium-phosphate agglomerates. The biologically generated minerals under such conditions are composed of genuine HAP crystallites of Ca10(PO4)6(OH)2 and 5–10 nanometer (nm) in size. This discovery will profoundly improve our understanding of bone metabolism and ectopic calcifications.

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Powder X-ray diffraction studies of hydroxyapatite and β-TCP mixtures processed by high energy dry milling

Cited by 19 publications

References 19 publications

Synthesis, Characterization and Process Optimization of Bone Whitlockite

Synthesis, Characterization and Process Optimization of Bone Whitlockite

Ion-Substituted Carbonated Hydroxyapatite Coatings for Model Stone Samples

Innate Biomineralization

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