• Journal of the Korean Crystal Growth and Crystal Technology
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• v.11 no.3
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• pp.115-119
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• 2001

Hydroxyapatite-yttria stabilized zirconia bioceramics containing fine zirconia particles were prepared as 3-layered functionally graded materials (FGMs) using a spark plasma sintering (SPS) and hot pressing (HP) apparatuses. The pretreatment of the raw hydroxyapatite promoted the sinterability of hydroxyapatite. The maximum density of pretreated FGM composites could be obtained at lower temperature than that for he untreated FGM samples. No decomposition from hydroxyapatite to three calcium phosphate (TCP) was observed in FGMs of HAp-$ZrO_2$ sintered below $1200^{\circ}C$ for 8 min under 10 MPa by SPS. However, the transformation of the tetragonal zirconia to the cubic modification had occurred in FGMs at this temperature. The presence of zirconia i.e. stress induced transformation of zirconia may be expected to enhance the mechanical properties of HAp-$ZrO_2$ FGM. The SPS is concluded as a better method to fabricated the FGM with dense and high strength compared with HP process.

• Journal of the Korean Ceramic Society
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• v.45 no.10
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• pp.573-578
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• 2008

In the preparation of hydroxyapatite(HAp)/gelatin(GEL) nanocomposite, GEL matrix was modified by the introduction of chondroitin sulfate(ChS) to obtain a strongly organized composite body. The formation reaction of the HAp/GEL-ChS nanocomposite was then investigated via XRD, DT/TGA, FT-IR, TEM and SEM. The organic-inorganic interaction between HAp nanocrystallites and GEL molecules was confirmed from DT/TGA and FT-IR. According to the DT/TGA results, the exothermal temperature zone between 300 and $550^{\circ}C$ showed an additional peak temperature that indicated the decomposition of the combined organics of the GEL and ChS. From the FT-IR analysis, calcium phosphate(Ca-P) was covalently bound with the GEL macromolecules modified by ChS. From TEM and ED, the matrix of the GEL-ChS molecules was mineralized by HAp nanocrystallites and the dense dried nanocomposite body was confirmed from SEM micrographs.

• Restorative Dentistry and Endodontics
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• v.19 no.1
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• pp.27-44
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• 1994

The purpose of this study was to determine the effects of pH, temperature and time on the synthesis of hydroxyapatite(HAP) by spontaneous precipitation under relatively physiologic condition. Specimens were obtained from aqueous system with various pH, temperature and experimental time. Chemical composition, crystallographic structure and crystallinity of the synthetic HAP were evaluated by Infrared spectroscopy and powdered X-ray diffraction method. The following results were obtained. 1. No precipitate was obtained under pH 5.5. 2. All the specimens were concluded as HAP except one that was obtained under the condition of pH 6.5, $25^{\circ}C$ and 1 day. It was concluded as dicalcium phosphate dihydrate(DCPD). 3. The crystallinity of HAP was enhanced by increases in pH, temperature and time of the preparation. But, the crystallinity of the synthetic HAP was lower than that of the mineral HAP. 4. Intermediates such as DCPD and octacalcium phosphate were formed on the process of the synthesis of HAP.

• Korean Journal of Materials Research
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• v.19 no.2
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• pp.85-89
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• 2009

Nano-crystalline hydroxyapatite (HAp) films were formed at the Ti surface by a single-step microarc oxidation (MAO), and HAp-zirconia composite (HZC) films were obtained by subsequent chemical vapor deposition (CVD) of zirconia onto the HAp. Through the CVD process, zero- and one-dimensional zirconia nanostructures having tetragonal crystallinity (t-ZrO2) were uniformly distributed and well incorporated into the HAp crystal matrix to form nanoscale composites. In particular, (t-$ZrO_2$) was synthesized at a very low temperature. The HZC films did not show secondary phases such as tricalcium phosphate (TCP) and tetracalcium phosphate (TTCP) at relatively high temperatures. The most likely mechanism for the formation of the t-$ZrO_2$ and the pure HAp at the low processing temperature was proposed to be the diffusion of $Ca^{2+}$ ions. The HZC films showed increasing micro-Vickers hardness values with increases in the t-$ZrO_2$ content. The morphological features and phase compositions of the HZC films showed strong dependence on the time and temperature of the CVD process. Furthermore, they showed enhanced cell proliferation compared to the $TiO_2$ and HAp films most likely due to the surface structure change.

• Proceedings of the Materials Research Society of Korea Conference
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• 2009.11a
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• pp.12.1-12.1
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• 2009

Nano-hydroxyapatite (N-HAp)has shown the pivotal role in producing bone-regenerative materials since it has similarity to natural bone minerals in terms of size, morphology, and the composition. Currently, the combination of biopolymers and N-HAp is recognizedas an attractive approach in generating hybrid scaffolds for bone tissueengineering. Surface engineering is an important issue since it determines whether cells can effectively adhere and proliferate on porous scaffolds. We aim to develop a synthetic approach to porous 3D scaffolds by immobilizing N-HAp on pore surfaces. The discrete nano-level anchoring of N-HAp on the scaffold pore surface is achieved using surface-repellent stable colloidal N-HAp with surface phosphate functionality. This rational surface engineering enables surface-anchored N-HAp to express its overall intrinsic bioactivity,since N-HAp is not phase-mixed with the polymers. The porous polymer scaffolds with surface-immobilized N-HAp provide more favorable environments thanconventional bulk phase-mixed polymer/N-HAp scaffolds in terms of cellular interaction and growth. In vitro biological evaluation using alkalinephosphatase activity assay supports that immobilized N-HAp on pore surfaces of polymer scaffolds contributed to the more enhanced in vitro osteogenicpotential. Besides, the scaffolds with surface-exposed N-HAp provide favorable environments for enhanced in vivo bone tissue growth, estimated by characteristic biomarkers of bone formation such as collagen. The results suggest that newly developed hybrid scaffolds with surface-immobilized N-HApmay serve as a useful 3D substrate with pore surfaces featuring excellent bonetissue-regenerative properties. Acknowledgement. This research was supported by a grant (code #: 2009K000430) from 'Center for Nanostructured Materials Technology' under '21st Century Frontier R&D Programs' of the Ministry of Education, Science and Technology, Korea.

• Korean Journal of Materials Research
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• v.21 no.6
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• pp.347-351
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• 2011

Hydroxyapatite (HAp) powders with different crystallinities were synthesized at various calcination temperatures through the co-precipitation of $Ca(OH)_2$ and $H_3PO_4$. The degradation behavior of these HAp powders with different crystallinities was assessed in a simulated body fluid solution (SBF) for 8 weeks. Below $800^{\circ}C$, the powders were nonstochiometric HAp, and the single HAp phase was successfully synthesized at $800^{\circ}C$. The degree of crystallinity of the HAp powders increased with an increasing calcination temperature and varied in a range from 39.6% to 92.5%. In the low crystallinity HAp powders, the Ca and P ion concentrations of the SBF solution increased with an increasing soaking time, which indicated that the low crystallinity HAp degraded in the SBF solution. The mass of the HAp powders linearly decreased with respect to the soaking time, and the mass loss was higher at lower crystallinities. The mass loss ranged from 0.8% to 13.2% after 8 weeks. The crystallinity of the HAp powders increased with an increasing soaking time up to 4 weeks and then decreased because of HAp degradation. The pH of the SBF solution did not change much throughout the course of these experiments. These results suggested that the crystallinity of HAp can be used to control the degradation.

• Korean Journal of Materials Research
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• v.14 no.11
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• pp.786-789
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• 2004

Hydroxyapatite powder was injected into thehole of teeth. The microstructure of teeth and HAp were observed after immersed in $9\%$ salin solution at $37^{\circ}C$ from 1month to 6 months. The junction morphology of hydroxyapatite and tooth was enhanced and particle size of hydroapatite was decreased with increasing time. The firm waxy body was found due to the hardening of hydroxyapatite fine powder resulting from the destruction of initial powder with swelling. It is suggested that the junction morphology of hydroxyapatite and tooth was observed due to the $Ca^{2+}$ ion shift of hydroxyapatite.

• Journal of the Korean Ceramic Society
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• v.44 no.3 s.298
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• pp.133-136
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• 2007

The crystal morphology of hydroxyapatite [HAp] phase in gelatin [GEL] matrices was investigated with the condition of a GEL precursor treatment in an aqueous solution of $H_{3}PO_{4}$ at $37-80^{\circ}C$. Needle-shaped nanocomposite particles were prepared through a dynamic reaction during a coprecipitation process using a phosphoric GEL solution. Various types of mineralized morphology appeared with a phosphorylated condition of the GEL solution. HAp/GEL nanocomposite slurries showed the existence of an octacalcium phosphate [OCP] phase during the process.

• Applied Chemistry for Engineering
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• v.34 no.6
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• pp.670-673
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• 2023

The biocompatibility of hydroxyapatite (HAP) has led to its application in various fields. To accomplish practical biological applications, such as drug/gene delivery, the colloidal stability of HAP in phosphate-buffered saline (PBS) is particularly important. In this study, we prepared a glycerol incorporated-HAP (Gly-HAP) by heating HAP in a glycerol environment at 200 ℃. To compare morphology and colloidal stability, HAP prepared at room temperature (RT-HAP) was thermally treated in water at 200 ℃ (H₂O-HAP). The heat treatment of HAP in both water and glycerol solutions results in an increase in the crystallinity of HAPs. Due to the low solubility of HAP in glycerol and the adsorption of glycerol on the HAP surface, crystal growth is limited. However, the heat-treated HAP under water increased in size by approximately four times compared to the initial crystallites. Compared to RT-HAP and H₂O-HAP, Gly-HAP shows improved colloidal stability in PBS, which originates from the adsorption of glycerol on the HAP surface that inhibits the agglomeration of individual HAP precipitates.

• Carbon letters
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• v.16 no.4
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• pp.233-240
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• 2015

Electrochemical synthesis was employed to prepare a novel hydroxyapatite/graphene (HAP/Gr) composite powder suitable for medical applications as a hard tissue implant (scaffold). The synthesis was performed in a homogeneous dispersion containing Na₂H₂EDTA·2H₂O, NaH₂PO₄ and CaCl₂ with a Ca/EDTA/PO₄³⁻ concentration ratio of 0.25/0.25/0.15M, along with 0.01 wt% added graphene nanosheets, at a current density of 137 mA cm⁻² and pH value of 9.0. The field emission scanning electron microscopy and transmission electron microscopy observations of the composite HAP/Gr powder indicated that nanosized hydroxyapatite particles were uniformly placed in the graphene overlay. Raman spectroscopy, Fourier transform infrared spectroscopy and X-ray diffraction confirmed graphene incorporation in the HAP/Gr powder. The electrochemically prepared HAP/Gr composite powder exhibited slight antibacterial effect against the growth of the bacterial strain Staphylococcus aureus.