• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2006.09a
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• pp.484-485
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• 2006

The process of coprecipitation of biocomposite hydroxyapatite/chitosan from aqueous solution at low temperature in alkali environnement was examined. We have shown that initially we have the formation of amorphous octocalcium phosphates $(Ca_8(HPO_4)(PO_4)_5,\;nH_2O:\;OCP)$ and the transferring from OCP to amorphous calcium phosphate $(Ca_9(PO_4)_3,\;nH_2O:\;TCP)$, and then from TCP to calcium-deficient hydroxyapatite $(Ca_{10-X}\;(HPO_4)_X(PO_4)_{6-x}(OH)_{2-X}\;:\;ACP)$ and hydroxyapatite $(Ca_{10}(PO_4)_6(OH)_2\;:\;HAP)$. The transformation of ACP to HAP was inhibited in the presence of chitosan. The result suggests that there is an affinity binding between ACP and chitosan and subsequently blocking the active growth site of ACP.

• Applied Chemistry for Engineering
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• v.8 no.6
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• pp.1000-1005
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• 1997

The properties of ceramics by solid-state reaction with hydroxyapatite[$Ca_{10}(PO_4)_6(OH)_2$], which was isolated from tuna bone by wet milling process were investigated. The bulk density $2.93g/cm^3$ at $1350^{\circ}C$ was close to the calculated density $3.21g/cm^3$. On X-ray measurements, the major phases were identified as hydroxyapatite at below $1300^{\circ}C$, but the whitlockite [$Ca_3(PO_4)_2$] phases were appeared due to a decomposition of hydroxyapatite with temperature. The microstructures of sintering specimens were shown as small closed pores between grain boundaries. The mean bending strength of the sintered hydroxyapatite by solid-state reaction is about 58 MPa and this value is higher than that of the articular cartilage maximum strength, 40MPa.

• Proceedings of the IEEK Conference
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• 2001.10a
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• pp.469-471
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• 2001

Dry grinding of a mixture of CaCO$_3$ and Ca(H$_2$PO$_4$)$_2$.$H_2O$ was conducted using a planetary ball mill in order to investigate solid state reaction for a synthesis of hydroxyapatite(Ca$_{10}$(PO$_4$)$_{6}$(OH)$_2$, HAp) through mechanochemical treatment method. The raw materials, which are composed of waste oyster and calcium biphosphate Ca(H$_2$PO$_4$)$_2$.$H_2O$, were mixed and then treated mechanochemically. The synthesis of hydroxyapatite(Ca$_{10}$(PO$_4$)$_{6}$(OH)$_2$, HAp) from the mixture was almost completed by about 60 minute grinding. The formation of HAp monophase in the ground mixture was characterized through X-ray diffraction (XRD) analysis. Moreover, the formation of HAp monophase depending on the grinding time was improved by increasing the grinding time.ime.ime.

• Analytical Science and Technology
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• v.13 no.2
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• pp.208-214
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• 2000

The formation and dissolution of hydroxides, carbonates and hydroxyapatite (HAp), which depend on the pH of solution, are important factor for the preparation of homogeneous and fine HAp, $Ca_{10-x}(HPO_4)_x(PO_4)_{6-x}(OH)_{2-x}(x=0)$, ceramic powder from the $Ca-PO_4-H_2O$ system. Since the solubility of each complex ion is a linear function of pH, the solubility diagram can be obtained by plotting the logarithmic molar concentrations calculated from the values of the equilibrium constants and solubility products for hydroxides, carbonates, and hydroxyapatite. The optimum pH condition for the formation of single phase $Ca_{10-x}(HPO_4)_x(PO_4)_{6-x}(OH)_{2-x}(x=0)$ powder in $Ca-PO_4-H_2O$ system at $25^{\circ}C$ was estimated as $10.5{\pm}0.5$ through the theoretical consideration. The HAp powder dried at $80^{\circ}C$ showed a fine agglomerated particles with a size of 75 nm. The HAp powder calcined at $1,000^{\circ}C$ consisted of nearly homogeneous particles with a size of 450 nm. Even though the dried HAp particles consisted of agglomeration, mechanical properties were superior due to fine microstructure after sintering.

• Journal of the Korean Ceramic Society
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• v.41 no.4
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• pp.289-296
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• 2004

Whisker and short rod shaped hydroxyapatite (Ca$_{10}$(PO$_4$)$_{6}$(OH)$_2$ with stoichiometric composition (Ca/P=1.62 -1.67, molar ratio) has been synthesized by hydrolysis and hydrothermal reaction of aqueous $\alpha$-Ca$_3$(PO$_4$)$_2$($\alpha$-TCP) solution (pH 11), respectively. The shape of resultant HAp was mainly dependent on synthetic route and the microstructural development was on processing condition. In hydrolysis processing, the degree of intersection of whiskerlike particles and agglomeration in the apsis line increased with increasing reaction time. In hydrothermal synthesis, the reaction product obtained under excessive reaction time ($\geq$3 h at 20$0^{\circ}C$) was severely agglomerated without further grain growth above certain critical size (0.75 ${\mu}{\textrm}{m}$ in length, 0.3${\mu}{\textrm}{m}$ 11m in diameter).

• The Korean Journal of Ceramics
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• v.5 no.2
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• pp.162-164
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• 1999

Microsotructure designed porous ceramics of calcium hydroxyapatite $(Ca_{10}(PO_4)_6(OH)_2)$ were prepared by hydrothermal method. The particle size, shape, and the micro-pore size of the porous hydroxyapatite ceramics could becontrolled. The hydroxyapatite was non-stoichiometric apatite with calcium deficient compositions (Ca/P ratio < 1.67). The composition of non-stoichiometric hydroxyapatite ceramics could be controlled from 1.50 to 1.63 in Ca/P ratio. The hydroxyapatite ceramics preparedc at $105^{\circ}C$ under the saturated vapor pressure for 20h were composed of rod-shaped crystals with about 10$\mu\textrm{m}$ in length with the mean aspect ratio of 40. The porous ceramics of calcium deficient hydroxyapatite had about 45% porosity with the inter-connecting pore structure. Porous hydroxyapatite ceramics prepared hydrothermally had the compressive strength of about 10 to 30 MPa. In addition, porous ceramics of $\beta$-tricalcium phosphate ($\beta-Ca_3(PO_4)_2$) were prepared from the calcium deficient hydroxyapatite.

• Bulletin of the Korean Chemical Society
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• v.28 no.4
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• pp.652-656
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• 2007

Hydroxyapatite [Ca10(PO4)6(OH)2, HAp] and titanium(Ti) metal are known to be excellent materials with high affinities for natural bone through the apatite. Tricalcium phosphate [Ca3(PO4)2, TCP] is a promising alternative material because it is similar to HAp in its physical properties and biocompatibility. To examine the influence of hydroxyapatite, tricalcium phosphate, pure titanium and pre-treated titanium on osteopontin expression in osteoblasts, RNA was extracted from proliferated and cultured osteoblast cells and OPN mRNA expression was observed by RT-PCR.

• Applied Chemistry for Engineering
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• v.8 no.6
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• pp.994-999
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• 1997

The sintering properties of hydroxyapatite isolated from tuna bone and hydroxyapatite-containing wollastonite sintered by solid-state reaction was investigated. As the sinterability of hydroxyapatite dependent upon the particle size by dry milling, it showed a sintering. But the hydroxyapatite-containing wollastonite was appeared good sinterability. On X-ray measurements, the major phases of hydroxyapatite-containing wollastonite by solid state reaction at $1250^{\circ}C$ were identified as hydroxyapatite and pseudowollastonite(${\alpha}-CaSiO_3$). And the phases appeared as whitlockite [$Ca_3(PO_4)_2$] by decomposition of hydroxyapatite at higher temperature above $1250^{\circ}C$. The shapes of microstructure on SEM images changed from porous to dense bulk by elevating temperature. The mean bending strength of hydroxyapatite-containing wollastonite sintered by solid-state reaction at $1300^{\circ}C$ was about 18 MPa, it was close to the cancellous bone's maximum strength, 20 MPa.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.31 no.5
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• pp.203-211
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• 2021

Octacalcium phosphate(OCP, Ca₈H₂(PO₄)₆·5H₂O) is one of biodegradable calcium phosphate materials with osteoconductivity and biocompatibility. It has the advantage of rapid bone formation and resorption due to the property of stimulating stromal cells to differentiate into osteoblasts. However, if OCP is inserted in body, it is immediately decomposed without maintaining of its shape as scaffolds due to their weak cohesive force between powder. On the other hand, hydroxyapatite (HA, Ca₁₀(PO₄)₆(OH)₂), which has a crystal structure similar to that of OCP, remains in the body without decomposition until the bone defect is restored. In this study, the degradation behavior of OCP/HA disc with different amount of HA in SBF (simulated body fluid) solution was characterized in terms of the weight loss, pH variation and microstructure change with immersion duration in SBF solution. As a result, the OCP/HA disc was not quickly decomposed and maintained its own shape for 2 weeks regardless of HA content. In particular, the surface of 40HA specimen was uniformly dissolved and then CDHA (calcium deficient hydroxyapatite) phase were formed onto the surface of disc after 7 days in SBF solution. It would be suggested that the 40HA specimen would be suitable candidate material as the scaffolds for the restoration of bone defect.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.15 no.2
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• pp.79-85
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• 2005

Commercial hydroxyapatite (HA) powders were calcined at the temperature range of $1000{\sim}1350^{\circ}C$ in air, for 2h, and the calcined powders were immersed in simulated body fluid (SBF) of pH 7.4 at $37^{\circ}C$ for 3 or 7 days. Thermal decomposition and their related dissolution behaviors of hydroxyapatite were investigated by XRD, FT-IR, and TEM. At the temperature of $1200^{\circ}C$, HA gradually releases its $OH^-$ ions and transforms to OHAP((oxyhydroxyapatite, ($Ca_{10}(PO_4)_6O_x(OH)_{2-2x}$)). HA thermally decomposes to ${\alpha}-TCP$ (${\alpha}-tricalcium$ phosphate) and TTCP (tetracalcium phosphate) phase at $1350^{\circ}C$. It was found that the surface dissolution of the hydroxyapatite powders was accelerated by non-stoichiometric composition and decomposed to ${\alpha}-TCP$ and TTCP.