• 한국재료학회지
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• 제28권3호
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• pp.142-147
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• 2018

${\beta}-Tricalcium$ phosphate (TCP) was added to $Al_2O_3$ to make a biomaterial with good mechanical properties. Using a TCP powder synthesized by a polymer complexation method, $Al_2O_3$ composites containing 30 wt% TCP were fabricated and characterized for densification, phase, microstructure, strength, and fracture toughness. With optimizing the powder preparation conditions, a high densification of 97 % was obtained by sintering at $1350^{\circ}C$ for 2 h. No reaction between the two components occurred and there was no transition to ${\alpha}-TCP$. TCP grains with a size of $2-4{\mu}m$ were well surrounded by $Al_2O_3$ grains with a size of $1{\mu}m$ or less. Strength 61(Brazilian) or 187(3-p MOR) MPa, and fracture toughness 1.7 (notched beam) or 2.5 (indentation) $MPa{\cdot}m^{1/2}$ were obtained, which are large improvements over the strength of $TCP/Al_2O_3$ composites and toughness of TCP and hydroxyapatite in previous studies.

• 한국세라믹학회지
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• 제30권11호
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• pp.905-910
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• 1993

$\alpha$-tricalcium phosphate($\alpha$-TCP) powders were synthesized and their hydration properties were investigated in Tris. solution. Two kinds of $\alpha$-TCP powder samples were prepared; the one is reaction product of CaHPO4.2H2O and CaCO3, and another is that of hydroxyapatite(HAp) and $\beta$-Ca2P2O7. They were satisfied with Ca/P mole ratio 1.5 and were heated at 150$0^{\circ}C$ for 5 hours. In the hydration of $\alpha$-TCP samples the powder which was synthesized from HAp and $\beta$-Ca2P2O7 was hydrated faster than that from CaHPO4.2H2O and CaCO3. The hydration reaction of $\alpha$-TCP powder transformed rapidly into HAp accompanying setting and hardening. It was realized that the hydration reaction of $\alpha$-TCP was due to the solution-precipitation mechanism and the hydrates from the reaction were Ca-deficient HAp having funtional group HPO42-.

• 한국결정성장학회지
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• 제30권6호
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• pp.244-250
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• 2020

β-삼인산칼슘(β-tricalcium phosphate, β-TCP, Ca3(PO4)2)은 뼈와 유사한 성분을 가지는 인산 칼슘계 세라믹 중 하나로, 생분해성과 골 전도성을 가지고 있어 골 대체재 등으로 다양하게 사용된다. 이러한 β-TCP의 생체 활성과 골유도성을 향상시키기 위해 다양한 이온 치환 연구가 진행되어왔으며 그 중 철 이온은 필수 미량 원소로 체내에서 다양한 기능을 한다. 본 연구에서는 β-TCP에 철 이온이 치환되었을 때 열처리 온도에 따른 구조의 변화를 분석하고, 이에 따른 생분해 특성을 평가하였다. 또한 분해 후의 구조를 분석하여 분해 거동을 확인하였다. 철 이온을 치환한 β-TCP는 공침법으로 합성을 하였고, 925℃와 1100℃에서 하소 처리를 실시하였다. X-선 회절 분석과 Rietveld refinement를 이용하여 구조 분석을 실시하였다. 철 이온은 온도에 따라 Fe2+ 또는 Fe3+ 상태로 바뀌기 때문에 β-TCP에 치환되었을 때 열처리 온도에 따라 치환 위치(Ca(4), Ca(5))가 바뀌고, 1100℃에서 열처리를 실시한 철 이온 치환 β-TCP의 분해 속도가 가장 빨랐다. 또한 세포 증식 특성이 향상된 것을 통해 β-TCP에 철 이온을 치환하는 것이 생체적합성과 생체 활성 특성을 향상시키고 골 결손부 회복 등 더욱 다양한 분야에 사용될 수 있을 것으로 기대된다.

• 한국세라믹학회지
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• 제39권11호
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• pp.1103-1107
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• 2002

생체재료의 일환으로 사용되고 있는 ${\beta}$-TCP(${\beta}$-Tricalcium Phosphate)를 합성하기 위하여 주원료인 칼슘을 화학약품이 아닌 천연재료인 달걀껍질을 이용하여 실험을 하였고, 이를 인산(phosphoric acid)과 혼합하여 ${\beta}$-TCP를 합성하였다. 본 연구에서는 인산의 혼합 량, 하소온도의 변화 그리고 달걀껍질의 출발물질 상태 등의 변수를 두고 실험을 실시하였다. 실험 변수에 따른 결과는 XRD 분석에 의해 결정상을 관찰하고, SEM에 의해 미세구조를 관찰하여 특성분석을 하였다. $900{\circ}$에서 하소한 달걀껍질을 인산과 함께 습식으로 볼 밀링 한 후, 이를 건조시켜 $900{\circ}$에서 1시간 동안 열처리하여 비교적 좁은 입도분포의 ${\beta}$-TCP 분말을 얻을 수 있었다. 차후 합성된 분말의 소결체를 이용하여, 생체 친화성과 뼈 속으로 대체되는 속도 등을 실험할 예정이다.

• 한국세라믹학회지
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• 제52권5호
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• pp.374-379
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• 2015

Mullite-matrix and $Al_2O_3$-matrix composites were fabricated with 30 wt% hydroxyapatite (HA) and tricalcium phosphate (TCP), respectively, as additives to give bioactivity. A diphasic gel process was employed to lower the densification temperature of the mullite matrix to $1320^{\circ}C$. A polymer complexation process was used to synthesize a TCP powder that was fully densified at $1250^{\circ}C$, for application to the matrix. For the HA/mullite composite, HA decomposed during sintering by reactions with the matrix components of $Al_2O_3$ and $SiO_2$, resulting in a mixture of $Al_2O_3$, TCP, and other minor phases with a low densification of less than 88% of the theoretical density (TD). In contrast, the TCP/$Al_2O_3$ composite was highly densified by sintering at $1350^{\circ}C$ to 96%TD with no reaction between the components. Different from the TCP monolith, the TCP/$Al_2O_3$ composite also showed a fine microstructure and intergranular fracture, both of which characteristics are advantageous for strength and fracture toughness.

• Journal of Ceramic Processing Research
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• 제20권6호
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• pp.655-659
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• 2019

Calcium phosphates such as HA (hydroxyapatite), β-TCP (tricalcium phosphate) and biphasic HA/β-TCP, were synthesized by wet chemical precipitation in aqueous solution combined with ball milling process. Nanosize powders of the calcium phosphates were synthesized using Ca(OH)2 and H3PO4. The effects of initial precursor Ca/P ratio (1.30, 1.50 and 1.67), ball milling process and post heat-treatment on the phase evolution behavior of the powders were investigated. The phase of resulting powder was controllable by adjusting the initial Ca/P ratio. HA was the only phase for as-prepared powders in both cases of Ca/P ratios of 1.50 and 1.67. The single HA phase without any noticeable second phase was obtained for the initial Ca/P ratio of 1.67 in the overall heat-treatment range. Pure β-TCP and biphasic calcium phosphate (HA/β-TCP) were synthesized from precursor solutions having Ca/P molar ratios of 1.30 and 1.50, respectively, after having been heat-treated above 700 ℃. The β-TCP phase has appeared on the pre-existing DCPD (dicalcium phosphate dihydrate) and/or HA phase. Dense ceramics having translucency were obtained at a considerably lower sintering temperature. The modified process offered a fast, convenient and economical route for the synthesis of calcium phosphates.

• Advanced Composite Materials
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• 제18권3호
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• pp.287-295
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• 2009

$\beta$-Tricalcium phosphate ($\beta$-TCP) particles reinforced bioresorbable plastics poly-L-lactide (PLLA) composites were prepared by injection molding. The nominal weight ratio of $\beta$-TCP was selected as 5, 10 and 15%. In order to clarify effects of the PLLA crystallinity on the mechanical properties, the specimens were heat treated isothermally. Results of differential scanning calorimetry indicated that the PLLA crystallinity increased with increasing heat treatment temperature. Bending and compressive tests were conducted on the specimen with different $\beta$-TCP contents and crystallinities. The results show that the bending and compressive moduli increased with increasing $\beta$-TCP contents and crystallinity. On the other hand, bending strength decreased with increasing $\beta$-TCP contents. Maximum bending strength was obtained at the heat treatment of $70^{\circ}C$ for 24 h, whereas compressive 0.2% proof strength increased with increasing heat treatment temperature. This difference is attributed to the difference in the microscopic damages.

• 한국세라믹학회지
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• 제40권6호
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• pp.608-614
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• 2003

pH 9.1, 9$0^{\circ}C$, 6시간의 조건에서 $\alpha$-tricalcium phosphate ($\alpha$-Ca$_3$(PO$_4$)$_2$)의 가수분해반응에 의해서 잘 발달된 수산화아파타이트 휘스커상 (길이 5$mu extrm{m}$,지름 0.5$\mu\textrm{m}$)이 합성되었다 수산화아파타이트로 $\alpha$-Ca$_3$(PO$_4$)$_2$의 전환에 미치는 반응조건(온도, 시간, pH)의 영향이 조사되었다. 아울러 XRD, SEM, ICP, TGA와 같은 분석기기를 사용하여 수산화아파트의 미세구조, 조성, 열적 안정성을 검토하였다.

• 한국CDE학회논문집
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• 제13권6호
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• pp.421-428
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• 2008

This article investigates the fabrication of polycaprolactone (PCL) composites filled with different volume fractions (10-30%) of tricalcium phosphate (TCP) by selective laser sintering (SLS) for tissue engineering scaffolds. Optimal processing parameters for each composition were developed by design of experiments (DOE). Specimens for compressive testing for each composition were fabricated and tested. The results showed that the compressive modulus increases as a function of TCP volume fraction. The experimentally measured compressive moduli were compared with moduli predicted by Halpin's theoretical model and were found to be in excellent agreement. This result proved that experimentally determined processing parameters for each composition were well optimized.

• 한국결정성장학회지
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• 제15권2호
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• pp.79-85
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• 2005

수산화아파타이트 상용분말을 $1000{\sim}1350^{\circ}C$ 온도범위에서 2시간 동안 공기 중에서 하소한 다음, pH 7.4인 유사 생체용액에 넣고 $37^{\circ}C$에서 3일 또는 7일간 침적실험을 행하였다. 열분해에 따른 수산화아파타이트 분말의 용해 거동은 XRD, FTIR, TEM을 이용해 비교분석 하였다. $1200^{\circ}C$에서 하소된 수산화아파타이트 분말은 격자 내 $OH^-$ 이온들의 탈수로 인하여 OHAP(oxyhydroxyapatite, ($Ca_{10}(PO_4)_6O_x(OH)_{2-2x}$)로 전이하였다. $1350^{\circ}C$에서 수산화아파타이트 분말 일부가 ${\alpha}-TCP$(${\alpha}-tricalcium$ phosphate)와 TTCP (tetracalcium phosphate)로 열분해 되었다. 수산화아파타이트 분말의 열분해로 인해 생성된 ${\alpha}-TCP$, TTCP 및 비화학양론조성의 OHAP 조성들이 수산화아파타이트 분말의 표면용해를 진전시켰다.