• Journal of the Korean Crystal Growth and Crystal Technology
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• v.32 no.3
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• pp.96-102
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• 2022

Hydroxyapatite (HAp) was synthesized from calcium hydroxide (Ca(OH)₂) reacting with phosphoric acid (H₃PO₄) in aqueous solution. HAp powders were synthesized from extremely high concentration of precursor solutions over 3 M of Ca(OH)₂ aqueous suspension using modified process parameters such as phosphoric acid (H₃PO₄) pouring rate, aging time and post ball milling process. Regardless of phosphoric acid pouring rate, the DCPD (dicalcium phosphate dihydrate) was formed at room temperature and when heated above 700℃, β-TCP (tricalcium phosphate) was synthesized and the amount reached its maximum at 900℃. When the synthesized powder was sintered at 1150℃, β-TCP, a high temperature impurity phase, remained. The single HAp phase without DCPD was obtained from post ball-milled precipitates followed by 3 day aging. For the ball-milled precipitates even without the aging process, the desired single HAp phase without β-TCP could be obtained by heat treatment above 500℃. The post ball milling process provided a convenient route for HAp synthesis.

• Journal of the Korean Ceramic Society
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• v.41 no.9
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• pp.715-721
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• 2004

Hydroxyapatite (HAp)/Gelatin (GEL) homogeneous composites of four different composition ratio were prepared by the co-precipitation process with synthetic HAp and GEL as a binder, HAP/GEL composites were molding by cold isostatic pressing and were sintering by various condition in air. Crystallinity and structure of sintered HAp/GEL composites were investigated by XRD and FTIR. Also, the compressive strength and the fracture surface of sintered specimens were measured by UTM and SEM. HAp/GEL composites showed a phase transformation to partially ${\alpha}$, ${\beta}$-tricalcium phosphate at the sintered condition of 1200$^{\circ}C$ for 3 h. The porosity of sintered body was in the range of 1.2-30.2％. The compressive strength of the sintered specimens was in the range of 16.2-60.1㎫, and its strength of sintered HAp/GEL comosites was higher than expected when the porosity was considered.

• Proceedings of the KOSOMBE Conference
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• v.1997 no.05
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• pp.35-38
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• 1997

The interfacial bonding energy between laser surface treated HA layer and Ti alloy substrate was investigated using a mechanical push-out tester. The initial slope of shear-stress and reduced displacement curves, maximum interfacial bond strength and bonding energy were calculated from results of the push-out test. The calculated initial slpoes are 38 MPa for the Ti alloy(A), 65 MPa for the sandblast finished specimen(B), 95 MPa for the HA plasma spray coated specimen and 49 MPa for the laser surface treated specimen(D). The maximum interfacial bonding strength are 3 MPa for the A, 19 MPa for the B, 20 MPa for the C, 10 MPa for the D. The interfacial bonding energies are $3.3\times10^{-9}J/mm^2$ for the A, $15.5\times10^{-9}J/mm^2$ for the B, $15.6\times10^{-9}J/mm^2$ for the C and $18.3\times10^{-9}J/mm^2$ for the D. Microscopic observation shows that the breaking of the laser treated specimen had been occured through the boundary between HA layer and polymer resin, but the untreated specimen had been occured through the inside of HA coating layer.

• Journal of the Korean Ceramic Society
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• v.40 no.6
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• pp.566-571
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• 2003

Hydroxyapatite (HAp)/Polyacrylic Acid(PAA) homogeneous composites of four different composition ratio were preparation by co-precipitation process with synthetic HAp and PAA as a binder. HAP/PAA composites were molding by cold isostatic pressing and were sintering by various condition in air. Crystallinity and structure of sintered HAp/PAA composites were investigated by XRD and FT-IR. Also, the compressive strength and the fracture surface of sintered specimens were measured by UTM and SEM. HAp/PAA composites were showed phase transformation of partially ${\alpha}$, ${\beta}$-tricalcium phosphate at sintering condition of 1200$^{\circ}C$ and 3 h. The pore size and porosity of sintered body were showed the range of 0.2∼3.0 $\mu\textrm{m}$ and 0.49∼13.43%, respectively. The compressive strength of sintered specimens were appeared the range of 36.6∼58.2 MPa. From these results, the sintered HAp/PAA comosites can be accounted for the microporous HAp having a good compressive strength due to homogeneous pore morphology.

• Journal of the Korean Ceramic Society
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• v.45 no.10
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• pp.610-617
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• 2008

Multi-walled carbon nanotube(CNT) reinforced hydroxyapatite composite coating with a thickness of $5{\mu}m$ has been successfully deposited on Ti substrate using aerosol deposition(AD). The coating had a dense microstructure with no cracks or pores, showing good adhesion with the Ti substrate. Microstructural observation using field-emission scanning electron microscopy(FE-SEM) and transmission electron microscopy(TEM) showed that CNTs with original tubular morphology were found in the hydroxyapatite-CNT(HA-CNT) composite coating. Measurements of hardness and elastic modulus for the coating were performed by nanoindentation tests, indicating that the mechanical properties of the coating were remarkably improved by the addition of CNT to HA coating. Therefore, HA-CNT composite coating produced by AD is expected to be potentially applied to the coating for high load bearing implants.

• 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.

• Journal of the Korean Ceramic Society
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• v.26 no.3
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• pp.305-314
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• 1989

Effect of pH variation in starting solution for the making of hydroxyapatite powder was studied in relation to the sinterability of the powder and their mechanical properties of the sintered hydroxyapatite ceramics. The sinterability of hydroxyapatite powder prepared at different pH was found to be improved with increase in pH value of the starting solutions. Thus the powders prepared from the higher pH solutions including 10.5, 11.0 and 11.5 could be well densified almost upto theoretical density by firing for 1 hr at 1,00$0^{\circ}C$. But the powder based on pH 10 exhibited less sinterability even being fired at much higher temperature of 1,10$0^{\circ}C$, it gave only 90-95% of theoretical density. On the other hand the powder prepared on the lowest pH value 9.5 could not be well densified and it could obtain only 78% of theoretical density even by firing at 1,30$0^{\circ}C$ for 1hr. It was found that prismatic crystals of whitlockite were always included in the sintered bodies based on the lower pH values as a minority crystalline phase together with the major crystalline phase of hydroxyapatite and its inclusion might impair the sinterability of powder. However in the case of the higher pH, the powder contained only hydroxyapatite as a crystalline phase on sintering without any minorities. The sphere shape of crystals might help effectively the densification of the bodies. The best mechanical properties could be obtained from the body of pH 11 sintered at 1,10$0^{\circ}C$, which gave 99.5% of theoretical density, 662Kg/$\textrm{mm}^2$ of vickers hardness and 1,352Kg/$\textrm{cm}^2$ of diameteral compression strength.

• Korean Chemical Engineering Research
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• v.50 no.5
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• pp.923-928
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• 2012

Optimizing a water-phase suspending system is very important to manufacture high-quality suspension polymerized toners. Therefore, in this study, the effects of the molar ratio of calcium hydroxide ($CaOH_2$)/phosphoric acid ($H_3PO_4$)(Ca/P), which were used as inorganic suspending agents, and pH of the water-phase on the characteristics of styrene-based suspension polymerized toners were mainly investigated. At first, the water-phase was fixed to neutral condition (pH=7.5) and Ca/P molar ratio was changed from 1.5:1 to 1.76:1. As a result, an ideal calcium phosphate (hydroxyapatite) was prepared at the Ca/P molar ratio of 1.73:1 and polymerized toners prepared at this condition showed good particle size distribution, circularity and charging characteristic. Based on this result, Ca/P molar ratio was fixed to 1.73:1 and pH of the water-phase was changed to weak acidic (pH=5.5) and weak basic (pH=9.5) conditions. As a result, polymerized toners prepared under the weak acidic condition showed very good particle size distribution, circularity and charging characteristic along with excellent printing quality. High-quality suspension polymerized toners could be prepared via optimizing Ca/P molar ratio and pH of the water-phase.

• Journal of the Korean Ceramic Society
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• v.48 no.1
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• pp.26-33
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• 2011

The glass in the system of CaO-$SiO_2-P_2O_5$ and the corresponding glass-ceramics are prepared for bone cements and the behaviors of the hardening and hydroxyapatite formation were studied for the glass and glass-ceramic powders. The glass crystallized into apatite, $\alpha$-wollastonite and $\beta$-wollastonite depending on the glass composition when they were heat-treated at $950^{\circ}C$ for 4 h. A DCPD (dicalcium phosphate dihydrate : $CaHPO_4{\cdot}2H_2O$) was developed when the prepared glass and glass-ceramic powders were mixed with 3M-$H_3PO_4$ solution. The DCPD (Ca/P=1.0) transformed to HAp (Ca/P=1.67) when the bone cement was soaked in simulated body fluid (SBF), and this HAp formation strongly depended on the releasing capacity of $Ca^{2+}$ ions from the glass and glass-ceramic cements. The glass-ceramic bone cement containing $\alpha$-wollastonite crystals showed faster transformation of DCPD to HAp than other glass-ceramics containing $\alpha$- and $\beta$-wollastonite crystals. No hydroxyapatite was observed when the glass-ceramic bone cement containing apatite crystals (36P6C) was soaked in SBF even for 1 month, because no $Ca^{2+}$ ion can be released from the stable apatite crystals.

• 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.