• Title/Summary/Keyword: Ca$^{2+}$-phosphate precipitation

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Precipitation of Calcium Phosphate at pH 5.0 for the β Tri-calcium Phosphate Cement

  • Chang, Myung Chul
    • Journal of the Korean Ceramic Society
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    • v.50 no.4
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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.

Synthesis of Hydroxyapatite Powders by Homogeneous Precipitation Method and Their Thermal Changes (균일침전법을 이용항 Hydroxyapatite 분말의 제조 및 가열변화)

  • Lee, Jin-Ho;Park, Hoon;Kim, Chang-Eun
    • Journal of the Korean Ceramic Society
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    • v.33 no.1
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    • pp.7-16
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    • 1996
  • ${CO_3}^{2-}$ containing whisker-like hydroxyapatite powders were synthesized byhomogeneous precipitation method using urea, Dicalcium phosphate anhdrate[DCPA; $CaHPO_4$] and octacalcium phosphate [OCP; $Ca_8H_2(PO_4_)6\cdot5H_20$]were obtained as precursors and they transformed to high crystalline hydroxyapatites at pH 5.62, and 6.54 respectively. According to the condition of the final pH in the solutions for the solution products and urea contents OCP was remained. When the solution product of $Ca^{2-}$ and ${PO_4}^{3-}$ was $1.5\times 10^4$[$mM^2$] and the content of urea was 0.25 mol.$dm^{-3}$ well crystallized whisker-like hydroxyapatite tens of micrometer in length was obtained. By heat treatment DCPA and OCP were decomposed into $\beta$-tricalcium phosphate [$\beta$-TCP ; $\beta$-$Ca_3{PO_4}_2$] and $\beta$-dicalcium phosphate [$\beta$-DCP ;$\beta$-$Ca_2P_2O_4}_2$]. And well-crystallized hydroxyapatite was partially decomposed into $\beta$-TCP at $800^{\circ}C$.

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Synthesis of calcium phosphates from abalone shells via precipitation (전복패각을 침전법의 원료로 이용한 calcium phosphates의 합성)

  • Moon, Sung Wook;Lee, Byeong Woo
    • 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.

Bioactivity behavior of biphasic calcium phosphate powders prepared by co-precipitation method (공침법으로 합성된 biphasic calcium phosphate 분말의 생체활성 거동)

  • Kim, Tae-Wan;Kim, Dong-Hyun;Jin, Hyeong-Ho;Lee, Heon-Soo;Park, Hong-Chae;Yoon, Seog-Young
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.22 no.2
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    • pp.99-104
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    • 2012
  • The co-precipitation technique has been applied to synthesize biphasic calcium phosphate (BCP). $Ca(NO_3)_2{\cdot}4H_2O$ and $(NH_4)_2HPO_4$ as the starting materials was used. X-ray diffraction (XRD) and Fourier transformed infrared (FT-IR) spectroscopy were used to characterize the structure of as-synthesized and calcined BCP powders. After immersion in Hanks' Balanced Salt Solution (HBSS), for 1 week a precipitation started to be formed with individual small granules on the specimen surface. An MTT assay indicated that BCP powders have no cytotoxic effects on MG-63 cells, and that they have good biocompatibility.

Hydration Properties of $\alpha$-Tricalcium Phosphate in Tris. Solution ($\alpha$-Tricalcium Phosphate의 Tris. Solution에서의 수화특성)

  • 인경필;최상흘
    • Journal of the Korean Ceramic Society
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    • v.30 no.11
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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-.

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The effect of organic matter on the removal of phosphorus through precipitation as struvite and calcium phosphate in synthetic dairy wastewater

  • Aleta, Prince;Parikh, Sanjai J.;Silchuk, Amy P.;Scow, Kate M.;Park, Minseung;Kim, Sungpyo
    • Membrane and Water Treatment
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    • v.9 no.3
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    • pp.163-172
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    • 2018
  • This study investigated the effect of organic matter on the precipitation of struvite and calcium phosphate for phosphorus recovery from synthetic dairy wastewater. Batch precipitation experiments were performed to precipitate phosphorus from solutions containing $PO_4{^{3-}}$ and $NH_4{^+}$ by the addition of $Mg^{2+}$ and $Ca^{2+}$, separately, at varying pH, Mg/P and Ca/P molar ratios, and organic matter concentrations. Soluble total organic solids exhibited more inhibition to precipitation due to potential interaction with other dissolved ionic species involved in phosphorus precipitation. Xylan with low total acidity only exhibited significant inhibition at very high concentrations in synthetic wastewater (at up to 100 g/L). No significant inhibition was observed for Mg and Ca precipitation at relatively lower concentrations (at up to 1.2 g/L). MINTEQ simulations show that dissolved organic matter (DOM) as humic substances (HS) can cause significant inhibition even at relatively low concentrations of 0.165 g/L fulvic acid. However, scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis suggested that xylan altered the crystal structure of both precipitates and had caused the formation of smaller sized struvite crystals with slightly rougher surfaces This could be due to xylan molecules adhering on the surface of the crystal potentially blocking active sites and limit further crystal growth. Smaller particle sizes will have negative practical impact because of poorer settleability.

Calcium Phosphate Bone Cement Based on Wet Prepared Dicalcium Phosphate

  • Chang, Myung Chul
    • Journal of the Korean Ceramic Society
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    • v.55 no.5
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    • pp.480-491
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    • 2018
  • Calcium phosphates (CaP) were prepared by a wet chemical method. Micro-crystalline dicalcium phosphate (DCPD) was precipitated at $37^{\circ}C$ and pH 5.0 using $Ca(OH)_2$ and $H_3PO_4$. The precipitated DCPD solution was kept at $37^{\circ}C$ for 96 h. Artificial bone cement was composed of DCPD, $Ca(H_2PO_4)_2{\cdot}H_2O$ (MCPM), and $CaSO_4{\cdot}1/2H_2O$, $H_2O$ and aqueous poly-phosphoric acid solution. The wet prepared CaP powder was used as a matrix for the bone cement recipe. With the addition of aqueous poly-phosphoric acid, the cement hardening reaction was started and the CaP bone cement blocks were fabricated for the mechanical strength measurement. For the tested blocks, the mechanical strength was measured using a universal testing machine, and the microstructure phase analysis was done by field emission scanning electron microscopy and X-ray diffraction. The cement hardening reaction occurred through the decomposition and recrystallization of MCPM and $CaSO_4{\cdot}1/2H_2O$ added on the surface of the wet prepared CaP, and this resulted in grain growth in the bone cement block.

Wet preparation of calcium phosphates from aqueous solutions

  • Lee, Byeong Woo;Hong, Il Gok
    • Journal of Ceramic Processing Research
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    • v.20 no.6
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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.

Use of Wet Chemical Method to Prepare β Tri-Calcium Phosphates having Macro- and Nano-crystallites for Artificial Bone

  • Chang, Myung Chul
    • Journal of the Korean Ceramic Society
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    • v.53 no.6
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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 ${\beta}-TCP$.

Adsorption Removal of Phosphate from Aqueous Solution by Olivine (감람석을 이용한 인의 흡착제거 특성)

  • Lee, Yong-Hwan;Yim, Soo-Bin
    • Journal of Korean Society on Water Environment
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    • v.27 no.4
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    • pp.516-522
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    • 2011
  • This study was performed to investigate the removal characteristics of phosphate by adsorption on olivine, which is generated as industrial by-products from quarry. The adsorption of phosphate on olivine was significantly achieved within 1 hour and equilibrated after 3 hours. The adsorption capacity of phosphate was enhanced with decreasing pH. The maximum adsorption capacity was observed to be 0.463 mg/g in the condition of pH 3. The $Ca^{2+}$ and $Mg^{2+}$ ion amount per adsorbent eluted from olivine was increased with decreasing pH. The precipitation test showed that phosphate in aqueous phase under the condition of pH 3 ~ 9 could be eliminated largely by adsorption on olivine, not precipitation. Freundlich adsorption model were successfully applied to describe the adsorption behavior of phosphate on olivine. The $q_m$ of Langmuir adsorption model were 1.3369 mg/g, 1.0544 mg/g, 1.0288 mg/g at pH 3, 6 and 9, respectively. The $K_F$ of Freundlich adsorption model were 0.4247 mg/g, 0.3399 mg/g, 0.2942 mg/g at pH 3, 6 and 9, respectively. The olivine showed high feasibility as a adsorbent for the removal of $PO_4$-P.