• 한국결정성장학회지
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• 제30권4호
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• pp.143-149
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• 2020

전복패각을 Ca원으로 이용하여 바이오 소재로 중요한 인산칼슘(calcium phosphates)들을 침전법을 통해 합성하였다. 전복패각에서 유래한 수산화칼슘(Ca(OH)₂)을 칼슘 공급원(전구체)으로 사용하였다. 수용액상에서 수산화칼슘과 인산(H₃PO₄)을 반응시켜 침전반응을 유도하여 인산칼슘화합물로의 합성을 유도하였다. 초기 전구체 Ca/P 비율을 1.50, 1.59 및 1.67로 조절하였으며 이 조성변화와 침전물에 대한 열처리가 분말 및 소결체의 물성에 미치는 영향에 대해 조사하였다. 초기 전구체 Ca/P 비율을 조절함으로써 소결체 상합성의 조절이 가능하였고, 1150℃에서 소결한 소결체에서(hydroxyapatite(HAp), β-tricalcium phosphate(β-TCP) 및 HAp와 β-TCP가 혼합된 2상 인산칼슘(BCP, HA/β-TCP))들이 합성되었다. 이러한 결과는 저비용, 고가용성을 가지는 경제적인 출발물질로부터 고부가가치 인산칼슘을 합성할 수 있는 가능성을 보여주었다.

• 한국세라믹학회지
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• 제50권4호
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• pp.275-279
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• 2013

The purpose of this study was to prepare calcium phosphate cement [CPC] for use in artificial bone. Nano-crystalline calcium phosphate [CaP] was precipitated at $37^{\circ}C$ using highly active $Ca(OH)_2$ in DI water and an aqueous solution of $H_3PO_4$. From the XRD measurements, the nano-CaP powder was close to apatitic TCP phase and the powders fired at $800^{\circ}C$ showed a critical ${\beta}$-TCP phase. A mixture of one mole $CaCO_3$ and two moles di-calcium phosphate was calcined at $1100^{\circ}C$ to make a reference ${\beta}$-TCP material. The nano-CaP powders were added to the normal ${\beta}$-TCP matrix and fired at $900^{\circ}C$ to make a ${\beta}$-TCP block. The sintered block showed improved mechanical strength, which was caused by the solid state interaction between nano-CaP and normal ${\beta}$-TCP.

• The Korean Journal of Ceramics
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• 제5권2호
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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.

• 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.

• 한국세라믹학회지
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• 제53권6호
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• pp.670-675
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• 2016

Calcium phosphate crystallites were prepared by wet chemical method for use in artificial bone. In order to obtain ${\beta}$-tricalcium phosphate (TCP), nano-crystalline calcium phosphate (CaP) was precipitated at $37^{\circ}C$ and at $pH5.0{\pm}0.1$ under stirring using highly active $Ca(OH)_2$ in DI water and an aqueous solution of $H_3PO_4$. The precipitated nano-crystalline CaP solution was kept at $90^{\circ}C$ for the growth of CaP crystallites. Through the growing process of CaP crystallites, we were able to obtain various sizes of rectangular CaP crystallites according to the crystal growing times. Dry nano-crystalline CaP powders at $37^{\circ}C$ were mixed with dry macro-crystalline CaP crystallites and the shaped mixture sample was fired at $1150^{\circ}C$ to make a ${\beta}-TCP$ block. Several tens of nm powders were uniformly coated on the surface, which was comprised of powders of several tens of ${\mu}m$, using a vibrator. The mixing ratio between the nanometer powders and the micrometer powders greatly affected the mechanical strength of the mixture block; the most appropriate ratio of these two materials was 50 wt% to 50 wt%. The sintered block showed improved mechanical strength, which was caused by the solid state interaction between the nano-crystalline ${\beta}-TCP$ and the macro-crystalline ${\beta}-TCP$.

• Journal of Microbiology and Biotechnology
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• 제15권6호
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• pp.1273-1279
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• 2005

Penicillium oxalicum strain CBPS-3F-Tsa, an efficient phosphate solubilizing fungus, was evaluated for its production of organic acid in vitro and effect of inoculation on the growth promotion of Maize under greenhouse conditions. The fungus solubilized 129.1, 118.8, and 54.1 mg P/1 of tricalcium phosphate [$Ca_{3}(PO_{4})_{2}$], aluminum phosphate ($A1PO_{4}$),and ferric phosphate ($FePO_{4}$), respectively, after 72 h of incubation. Malic acid, gluconic acid, and oxalic acid were detected in the flasks supplemented with various phosphate sources [240, 146, 145 mM/1 $A1PO_{4},\;FePO_{4},\;and\;Ca_{3}(PO_{4})_{2}$, respectively] together with a large amount of malic acid followed by the other two. The effects of inoculation of P. oxalicum CBPS-3F-Tsa on maize plants were studied under pot culture conditions. P. oxalicum CBPS-3F-Tsa was inoculated to maize plants alone or together with inorganic phosphates in the form of fused phosphates (FP) and rock phosphates (RP). Inoculation of P. oxalicum CBPS-3F-Tsa increased the plant growth and N and P accumulation in plants, compared with control plants, and also had positive effects when applied with RP. The results of this study show that the fungus P. oxalicum strain CBPS-3F-Tsa could solubilize different insoluble phosphates by producing organic acids, particularly malic acid, and also improved the efficiency of RP applied to maize plants.

• Journal of the Korean Association of Oral and Maxillofacial Surgeons
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• 제34권1호
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• pp.36-48
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• 2008

To repair bone defects in the oral and maxillofacial field, bone grafts including autografts, allografts, and artificial bone are used in clinical dentistry despite several disadvantages. The purpose of this study was to evaluate new bone formation and healing in rat calvarial bone defects using hydroxyapatite (HA, $Ca_{10}[PO_4]_6[OH]_2,\;Bongros^{(R)}$, Bio@ Co., KOREA) and tricalcium phosphate (${\beta}-TCP,\;Ca_3[PO_4]_2$, Sigma-Aldrich Co., USA) mixed at various ratios. Additionally, this study evaluated the effects of type I collagen (Rat tail, BD Biosciences Co., Sweden) as a basement membrane organic matrix. A total of twenty, 8-week-old, male Sprague-Dawley rats, weighing 250-300g, were divided equally into a control group (n=2) and nine experimental groups (n=2, each). Bilateral, standardized transosseous circular calvarial defects, 5.0 mm in diameter, were created. In each experimental group, the defect was filled with HA and TCP at a ratio of 100:0, 80:20, 70:30, 60:40, 50:50, 40:60, 30:70, 20:80, and 0:100 with or without type I collagen. Rats were sacrificed 4 and 8 weeks post-operation for radiographic (standardized plain film, Kodak Co., USA), histomorphologic (H&E [Hematoxylin and Eosin], MT [Masson Trichrome]), immunohistochemical staining (for BMP-2, -4, VEGF, and vWF), and elementary analysis (Atomic absorption spectrophotometer, Perkin Elmer AAnalyst $100^{(R)}$). As the HA proportion increased, denser radiopacity was seen in most groups at 4 and 8 weeks. In general radiopacity in type I collagen groups was greater than the non-collagen groups, especially in the 100% HA group at 8 weeks. No new bone formation was seen in calvarial defects in any group at 4 weeks. Bridging bone formation from the defect margin was marked at 8 weeks in most type I collagen groups. Although immunohistochemical findings with BMP-2, -4, and VEGF were not significantly different, marked vWF immunoreactivity was present. vWF staining was especially strong in endothelial cells in newly formed bone margins in the 100:0, 80:20, and 70:30 ratio type I collagen groups at 8 weeks. The calcium compositions from the elementary analysis were not statistically significant. Many types of artificial bone have been used as bone graft materials, but most of them can only be applied as an inorganic material. This study confirmed improved bony regeneration by adding organic type I collagen to inorganic HA and TCP mixtures. Therefore, these new artificial bone graft materials, which are under strict storage and distribution systems, will be suggested to be available to clinical dentistry demands.

• 한국세라믹학회지
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• 제41권12호
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• pp.921-928
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• 2004

수용액의 pH, 소성온도, 반응시간 등을 변화한 조건하에서 $Ca(OH)_2$와 $H_{3}PO_4$ 수용액을 이용하여 인산칼슘계 화합물을 제조하였다. 산성분위기(pH=5.21)에서는 ${\beta}-TCP({\beta}-tricalcium phosphate)$가, pH>7.62에서는 HAp(hydroxyapatite)가 주 결정상으로 관찰되었다. XRD 분석결과, $Ca(OH)_2$와 $H_{3}PO_4$는 빠르게 반응(5분이내)하여 HAp를 생성하였고, 반응 16시간까지 안정적으로 구조를 유지하였다. 우수한 결정성을 나타내는 소성온도는 $1200^{\circ}C$로 관찰되었다. 주사전자현미경(SEM)에 의한 미세구조 관찰 결과, pH가 5.21일 경우 침상 형태의 ${\beta}-TCP$ 입자가, pH 7.62에서는 침상 형태의 HAp가 합성되었다. 그러나 pH 9.16에서는 매우 작고 균일한 구형의 HAp 입자들이 생성되었고, 다시 작은 입자들이 침상으로 재배열된 형상을 관찰할 수 있었다. 합성된 HAp(pH 9.16)를 본차이나 소지에 일정량 혼합하여 본차이나 물성, 즉 결정성, 흡수율, 색도, 파단면의 형상을 측정${\cdot}$분석하였다.

• 한국결정성장학회지
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• 제29권5호
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• pp.203-207
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• 2019

인산칼슘(hydroxyapatite(HAp), ${\beta}$-tricalcium phosphate(${\beta}$-TCP) 및 HAp와 ${\beta}$-TCP가 혼합된 2상 인산칼슘(BCP, HA/${\beta}$-TCP))들을 수열합성법을 통해 합성하였다. 여러 수열합성 조건(최고온도 $150^{\circ}C$ 및 pH 12 이하)에서 수산화칼슘($Ca(OH)_2$) 수용액과 인산($H_3PO_4$) 용액을 반응시켜 얻은 침전물을 수열합성에 이용하였다. 초기 전구체 Ca/P 비율을 1.30, 1.50 및 1.67로 조절하였으며 이 조성비와 합성 후 열처리가 분말 및 소결체의 상합성에 미치는 영향에 대해 조사하였다. 초기 전구체 Ca/P 비율을 조절함으로써 분말 및 소결체의 상의 조절이 가능하였다. Ca/P 비율이 1.67일 경우 모든 열처리 온도에서 분말 및 소결체 모두에서 HAp 단일 상이 합성되었다. Ca/P 비율이 1.30과 1.50에서 $900^{\circ}C$ 이상 열처리 할 경우 각각 순수한 ${\beta}$-TCP와 BCP(HAp/${\beta}$-TCP)가 합성되었다. 반응성 높은 미세한 분말을 이용하여 소결함으로써 미세한 입경을 가지며 투광성을 가지는 소결체들을 저온에서 얻을 수 있었다.

• 한국토양비료학회지
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• 제40권5호
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• pp.405-411
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• 2007

본 연구는 감귤원 토양유형별로 고정되어 있는 난용성 인산염함량을 파악하고 이를 생물학적으로 이용하고자 인산가용화 우수미생물을 선발하여 특성을 조사하였다. 토양중 난용성 인산염의 형태별 분포는 Al-P>Ca-P>Fe-P 순으로 화산회토 토양이 비화산회토 보다 많았다. PDA-P배지를 이용하여 인산염 가용화능이 우수한 Bacillus sphaericus를 분리하였으며 pH 4~5와 $30^{\circ}C$에서 생육이 제일 좋았다. Bacillus sphaericus은 $AlPO_4$에서 324.5 ppm, $Ca_{10}(PO_4)_6(OH)_2$에서 334.8 ppm, $Ca_3(PO_4)_2$에서 207.0 ppm의 유리인산을 생성하였으며 인산효소활성은 $35^{\circ}C$에서 배양할 때 높았다. Bacillus sphaericus를 Bentonite 등 담체에 고정 후 온도를 달리하여 7개월 보존기간 동안 밀도변화를 조사한 결과 $10^5c.f.u.\;g^{-1}$ 수준과 인산가용화능을 유지하여 추후 생물비료로 이용이 가능할 것으로 기대된다.