• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.5
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• pp.203-207
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• 2019

Calcium phosphates such as hydroxyapatite (HAp), tricalcium phosphate (${\beta}$-TCP), and biphasic calcium phosphate (BCP, HAp/${\beta}$-TCP) have been prepared via hydrothermal treatment. The synthesis was conducted by reacting ($Ca(OH)_2$) aqueous solution with phosphoric acid ($H_3PO_4$) under different hydrothermal synthesis conditions (temperatures up to $150^{\circ}C$ and pH lower than 12). The effects of initial precursor Ca/P ratio (1.30, 1.50 and 1.67) and post heat treatment on the phase evolution behavior of the powders and sintered ceramics were investigated. The phases of resulting powders and sintered ceramics were controllable by adjusting the initial Ca/P ratio. A single HAp phase without any noticeable second phase was obtained for the initial Ca/P ratio of 1.67 in the overall heat treatment range. Pure ${\beta}$-TCP and biphasic calcium phosphate (HAp/${\beta}$-TCP) were synthesized from precursor solutions having Ca/P molar ratios of 1.30 and 1.50, respectively, after having been heat treated at $900^{\circ}C$ or higher. Dense ceramics with translucency were obtained at considerably lower sintering temperatures.

• Korean Journal of Materials Research
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• v.26 no.8
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• pp.449-453
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• 2016

$HA(hydroxyapatite)/{\beta}-TCP$ (tricalcium phosphate) biomaterial (BCP; biphasic calcium phosphate) is widely used as bone cement or scaffolds material due to its superior biocompatibility. Furthermore, $NH_4HCO_3$ as a space holder (SH) has been used to evaluate feasibility assessment of porous structured BCP as bone scaffolds. In this study, using a spark plasma sintering (SPS) process at 393K and 1373K under 20MPa load, porous $HA/{\beta}-TCP$ biomaterials were successfully fabricated using $HA/{\beta}-TCP$ powders with 10~30 wt% SH, TiH2 as a foaming agent, and MgO powder as a binder. The effect of SH content on the pore size and distribution of the BCP biomaterial was observed by scanning electron microscopy (SEM) and a microfocus X-ray computer tomography system (SMX-225CT). The microstructure observations revealed that the volume fraction of the pores increased with increasing SH content and that rough pores were successfully fabricated by adding SH. Accordingly, the cell viabilities of BCP biomaterials were improved with increasing SH content. And, good biological properties were shown after assessment using Hanks balanced salt solution (HBSS).

• 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.

• 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 Crystal Growth and Crystal Technology
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• v.30 no.4
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• pp.143-149
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• 2020

Calcium phosphates recognized as important bio-materials have been successfully synthesized by simple precipitation using waste abalone shells, which are rich mineral sources of calcium. Calcium hydroxide (Ca(OH)₂) originated from abalone shells was used as calcium source (precursor) for the preparation. Synthesis of calcium phosphates was performed by reacting calcium hydroxide with phosphoric acid (H₃PO₄) in aqueous solution. The initial precursor Ca/P ratios were adjusted to 1.50, 1.59 and 1.67, and the effect of the composition and the heat treatment on the synthesized powders and sintered bodies was investigated. The phases of the sintered ceramics prepared at 1150℃ were hydroxyapatite (HAp), β-tricalcium phosphate (β-TCP), and biphasic phosphate (HAp with β-TCP)), which were determined by the initial precursor Ca/P ratios. The results demonstrate the possibility for the synthesis of high value-added calcium phosphates from economical starting materials with low cost and high availability.

• Korean Journal of Materials Research
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• v.25 no.4
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• pp.165-170
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• 2015

Ceramics biomaterials are useful as implant materials in orthopedic surgery. In this study, porous HA(hydroxyapatite)/${\beta}$-TCP(tricalcium phosphate) composite biomaterials were successfully fabricated using HA/${\beta}$-TCP powders with 10-30 wt% $NH_4HCO_3$ as a space holder(SH) and $TiH_2$ as a foaming agent, and MgO powder as a binder. The HA/${\beta}$-TCP powders were consolidated by spark plasma sintering(SPS) process at $1000^{\circ}C$ under 20 MPa conditions. The effect of SH content on the pore size and distribution of the HA/${\beta}$-TCP composite was observed by scanning electron microscopy(SEM) and a microfocus X-ray computer tomography system(SMX-225CT). These microstructure observations revealed that the volume fraction of the pores increased with increasing SH content. The pore size of the HA/${\beta}$-TCP composites is about $400-500{\mu}m$. The relative density of the porous HA/${\beta}$-TCP composite increased with decreasing SH content. The porous HA/${\beta}$-TCP composite fabricated with 30%SH exhibited an elastic modulus similar to that of cortical bone; however, the compression strength of this composite is higher than that of cortical bone.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.20 no.5
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• pp.237-242
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• 2010

Magnesium-substituted BCP (biphasic calcium phosphate) powders were prepared by incorporating small amounts of magnesium into the structure of different hydroxyapatite (HAp)/${\beta}$-tricalcium phosphate (${\beta}$-TCP) ratios through coprecipitation method. A series of magnesium substitutions ranging from 0, 0.5, and 1.0 wt%, which are comparable to the measured magnesium contents, were performed. The obtained powders were characterized by the following analytical techniques: X-ray diffraction analysis (XRD), Thermo Gravimetric Analyzer (TGA) and Fourier transform infrared spectroscopy (FT-IR). The results have shown that substitution of magnesium in the calcium-deficient apatites resulted in the formation of biphasic mixtures of different HAP/${\beta}$-TCP ratios after heating above $1000^{\circ}C$. The 1.0 wt% magnesiumsubstituted-BCP were soaked in Hank's solutions after 2 weeks to observe the morphology of the biocement, especially needle-like hydroxyapatite crystals and to estimate the length and diameter of nanoneedle crystals.

• Journal of the Korean Ceramic Society
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• v.41 no.12 s.271
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• pp.921-928
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• 2004

Calcium phosphate powders have been prepared by using $Ca(OH)_2\;and\;H_{3}PO_4$ solution under various conditions such as pH, calcination temperature, and reaction time. ${\beta}-TCP({\beta}-tricalcium phosphate)$and HAp(hydroxyapatite) were synthesized at pH=5.21 and pH > 7.62, respectively. From XRD results, $Ca(OH)_2\;and\;H_{3}PO_4$ solution reacted quickly to form HAp, which was structurally stable up to 16h. Calcination temperature having good crystallinity is revealed to be at $1200^{\circ}C$. SEM analysis showed that ${\beta}-TCP$ and HAp with needle type were synthesized at pH 5.21 and pH 7.62, respectively. However, at pH 9.16, tiny and homogeneous HAp having sphere was prepared and rearranged to show needle morphology. HAp synthesized at pH 9.16 was utilized as bonechina body and calcined. The sample was analyzed its crystallinity, water absorbtion, color, and shape to check physical properties.

• Journal of the Korean Ceramic Society
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• v.41 no.8
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• pp.582-587
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• 2004

Biphasic Calcium Phosphate (BCP) consisted of hydroxyapatite (HAp) and $\beta$-tricalcium phosphate (P-TCP) has been prepared by solid state reaction. The size reduction of the resultant BCP agglomerate was carried out by reaction with hot water under atmospheric condition uld also under high pressure using an autoclave. The influence of processing conditions on the change of crystalline phase and composition, relative amount of constituent, specific surface area, and microstructure was investigated by means of XRD, FT-IR, BET method using a nitrogen adsorption and SEM.

• Journal of Periodontal and Implant Science
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• v.38 no.2
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• pp.163-170
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• 2008

Purpose: Biphasic calcium phosphates have been of great interest recently. Mixing adequate ratios of hydroxyapatite(HA) and beta-tricalcium phosphate($\beta$-TCP) allowed to control the resorption rate without distorting its osteoconductive property. This study evaluated the bone formation effect of newly developed biphasic calcium phosphate(BCP) in calvarial defect of rabbits. Materials and Methods: 6 male New Zealand rabbits were used. Four defects with 8mm in diameter were created on each animal. BCP with HA/$\beta$-TCP ratio of 7:3 and particle size of $0.5{\sim}1.0\;mm$ was used as the test group and bovine bone with $0.25{\sim}1.0\;mm$ particle size, as the control group. Both test and control group materials were randomly implanted in the calvarial defects and were covered witha polymer membrane. The animals were sacrificed after 12, 24, and 48 weeks of implantation under general euthanasia. Resin blocks were obtained and were stained by masson's trichrome for histological observation. Results: Overall results were uneventful without any defect exposure or inflammation. The amount of new bone formation and bone maturity increased with increase in healing period at both groups. New bone in test group was mostly formed along the material particle surrounded by osteoblasts, and observation of osteoblastic stream was also present. Bone maturity increased as it was closer to thedefect margins. Under the same healing period, the test group showed more bone formation than the control group with more stable bovine bone particles remaining even after 48 weeks, whereas considerable resorption took place in BCP. Almost total defect closure was observed in test group with new bone formation in the central part of the defect. However, limited new bone formation was observed in the control group. Conclusion: Within the limits of the study, the present study reveals the newly developed BCP to be a good osteoconductive material. However, further studies are needed to be conducted in a different study model with a larger sample size.