• Title/Summary/Keyword: Solution Heat Treatment

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Development and Evaluation of Natural Hydroxyapatite Ceramics Produced by the Heat Treatment of Pig Bones

  • Lim, Ki-Taek;Kim, Jin-Woo;Kim, Jangho;Chung, Jong Hoon
    • Journal of Biosystems Engineering
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    • v.39 no.3
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    • pp.227-234
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    • 2014
  • Purpose: The aim of this research was to develop and evaluate natural hydroxyapatite (HA) ceramics produced from the heat treatment of pig bones. Methods: The properties of natural HA ceramics produced from pig bones were assessed in two parts. Firstly, the raw materials were characterized. A temperature of $1,200^{\circ}C$ was chosen as the calcination temperature. Fine bone powders (BPs) were produced via calcinations and a milling process. Sintered BPs were then characterized using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR) spectroscopy, and a 2-year in vitro degradability test. Secondly, an indirect cytotoxicity test was conducted on human osteoblast-like cells, MG63, treated with the BPs. Results: The average particle size of the BPs was $20{\pm}5{\mu}m$. FE-SEM showed a non-uniform distribution of the particle size. The phase obtained from XRD analysis confirmed the structure of HA. Elemental analysis using XRF detected phosphorus (P) and calcium (Ca) with the Ca/P ratio of 1.6. Functional groups examined by FTIR detected phosphate ($PO{_4}^{3-}$), hydroxyl ($OH^-$), and carbonate ($CO{_3}^{2-}$). The EDX, XRF, and FTIR analysis of BPs indicated the absence of organic compounds, which were completely removed after annealing at $1,200^{\circ}C$. The BPs were mostly stable in a simulated body fluid (SBF) solution for 2 years. An indirect cytotoxicity test on natural HA ceramics showed no threat to the cells. Conclusions: In conclusion, the sintering temperature of $1,200^{\circ}C$ affected the microstructure, phase, and biological characteristics of natural HA ceramics consisting of calcium phosphate. The Ca-P-based natural ceramics are bioactive materials with good biocompatibility; our results indicate that the prepared HA ceramics have great potential for agricultural and biological applications.

The Growth of Osteoblasts according to the Pretreatment of HA Scaffold Surface (하이드록시아파타이트 지지체의 표면 처리 방법에 따른 골아세포의 성장)

  • Park, Byung-Chan;Kim, Yong-Ha;Kim, Tae-Gon;LeeYoun-Jung, Jun-Ho;Sik-Young, Kim;Choi, Sik-Young
    • Archives of Plastic Surgery
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    • v.37 no.4
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    • pp.340-345
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    • 2010
  • Purpose: Recently, bioceramics have become popular as a substitute graft material for reconstruction of bony defect after trauma or tumor surgery. Among the bioceramic materials, hydroxyapatite (HA) is favored due to its biocompatibility. HA scaffold is composed of the interconnected reticular framework, macropores and micropores. Macropores play an important role in cell migration, nutrients supply and vascular ingrowth. On the other hand, a number of micropores less than $10{\mu}m$ form an irregular surface on HA scaffolds, which prevents the osteoblast from adhering and proliferating on the surface of HA scaffold. Methods: In this study, three different groups were designed for comparison. In the first group (group A), conventional method was used, in which HA pellet was applied without surface pretreatment. The second group (group B) was given a HA pellet that has been coated with crystalline HA solution prior to application. In the third group (group C), the same method was used as the second group, where the pretreated HA pellet was heated ($1250^{\circ}C$, 1 hour) before application. Osteoblast-like cells ($2{\times}10^4$/mL) were scattered onto every pellet, then they were incubated in 5% $CO_2$ incubator at $37^{\circ}C$ for twelve days. During the first three days, osteoblast cells were counted using the hemocytometer daily. ALP activity was measured on the 3, 6, 9 and 12 culture days using the spectrophotometer. Results: Under SEM, group A showed a surface with numerous micropores, and group B revealed more rough crystal surface. Group C revealed a fused crystal appearance and flattened smooth surface. In proliferation and ALP activity of osteoblast cells, group C showed better results compared to group B. Group A which lacks pretreatment of the surface showed less osteoblast proliferation and ALP activity than group C, but showed better results than group B. Conclusion: We found that crystallized HA with heat treatment method enhances the osteoblasts proliferation and differentiation on the surface of HA pellets.

Application of Porous Nanofibers Comprising Hollow α-Fe2O3 Nanospheres Prepared by Applying Both PS Template and Kirkendall Diffusion Effect for Anode Materials in Lithium-ion Batteries (커켄달 효과와 주형법을 통해 합성한 α-Fe2O3 중공입자로 구성된 다공성1차원 구조체의 리튬 이차전지 음극활물질 적용)

  • Lee, Young Kwang;Jeong, Sun Young;Cho, Jung Sang
    • Korean Chemical Engineering Research
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    • v.56 no.6
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    • pp.819-825
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    • 2018
  • Porous nanofibers comprising hollow ${\alpha}-Fe_2O_3$ nanospheres were prepared by applying both template method and Kirkendall diffusion effect to electrospinning process. During heat-treatment processes, the solid Fe nano-metals formed by initial heat-treatment in the carbon matrix were converted into the hollow structured ${\alpha}-Fe_2O_3$ nanospheres. In particular, PS nanobeads added in the spinning solution were decomposed and formed numerous channels in the composite, which served as a good pathway for Kirkendall diffusion gas. The resulting porous nanofibers comprising hollow ${\alpha}-Fe_2O_3$ nanospheres were applied as an anode material for lithium-ion batteries. The discharge capacities of the nanofibers for the 30th cycle at a high current density of $1.0A\;g^{-1}$ was $776mA\;h\;g^{-1}$. The good lithium ion storage property was attributed to the synergetic effects of the hollow ${\alpha}-Fe_2O_3$ nanospheres and the interstitial nanovoids between the nanospheres. The synthetic method proposed in this study could be applied to the preparation of porous nanofibers comprising hollow nanospheres with various composition for various applications, including energy storage.

A Study on the Cobalt and Lithium Recovery from the Production Scraps of Lithium Secondary Battery by High Efficient and Eco-friendly Method (이차전지(二次電池) 제조공정(製造工程)스크랩으로부터 고효율(高效率) 親環境(친환경) 코발트(Co)와 리튬(Li)의 회수(回收)에 관(關)한 연구(硏究))

  • Lee, Jeong-Joo;Chung, Jin-Do
    • Resources Recycling
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    • v.19 no.6
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    • pp.51-60
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    • 2010
  • A study on the recovery of cobalt and lithium from Lithium Ion Battery(LIB) scraps has been carried out by a physical treatment - leaching - solvent extraction process. The cathode scraps of LIB in production were used as a material of this experiment. The best condition for recovering cobalt from the anode scraps was acquired in each process. The cathode scraps are dissolved in 2M sulfuric acid solution with hydrogen peroxide at $95^{\circ}C$, 700 rpm. The cobalt is concentrated from the leaching solution by means of a solvent extraction circuit with bis(2-ethylhexyl) phosphoric acid(D2EHPA) and PC88A in kerosene, and then cobalt and lithium are recovered as cobalt hydroxide and lithium carbonate by precipitation technology. The purity of cobalt oxide powder was over 99.98% and the average particle size after milling was about 10 lim. The over all recoveries are over 95% for cobalt and lithium. The pilot test of mechanical separation was carried out for the recovery of cobalt from the scraps. The $Co_3O_4$ powder was made by the heat treatment of $Co(OH)_2$ and the average particle size was about 10 ${\mu}m$ after grinding. The recovery was over 99% for cobalt and lithium each other and the purity of cobalt oxide was over 99.98%.

Synthesis of Nano TiO2 Coated on Fly Ash Composites by the Precipitation Dropping Method (침전제적하법에 의한 나노 TiO2코팅 석탄회 복합체 제조)

  • 신대용;한상목
    • Journal of the Korean Ceramic Society
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    • v.39 no.6
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    • pp.550-557
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    • 2002
  • TiO$_2$ particles coated on fly ash composites for use in photocatalyst were synthesized by the precipitation dropping method and heated at $700^{\circ}C$ for 2 h. The pH of reaction solution, the addition rate of NH$_4$HCO$_3$, the stirring speed, the reaction temperature and the concentration of TiC1$_4$ had a pronounced effect on the nature of precipitated TiO$_2$ particles on the surface off fly ash and the crystal structure of precipitated TiO$_2$ particles. At an addition rate of NH$_4$HCO$_3$; 1.0 ml/min, the pH of the reaction solution; 6, the stirring speed; 1,000 rpm and the reaction temperature; 8$0^{\circ}C$, about 10 nm of TiO$_2$ particle size and homogeneous precipitated layer on the surface of a fly ash was achieved. On the contrary, at an addition rate of NH$_4$HCO$_3$; 0.3,0.5 ml/min, the pH of the reaction solution; 2 and 11, the stirring speed; 300~500 rpm and the reaction temperature; lower than 5$0^{\circ}C$:, Inhomogeneous precipitated layer was developed on a fly ash. TiO$_2$ particles with anatase phase was formed as-dried precipitation at the low concentration of Tic14, the high addition rate of NH$_4$HCO$_3$ and the high reaction temperature, the crystalline fraction of anatase increased with raising heat-treatment temperature and rutile phase began to formation at 80$0^{\circ}C$. The crystal size of TiO$_2$ particles increased with raising the heat-treatment temperature, the crystal size was showed about 21 m at $700^{\circ}C$. Anatase type of TiO$_2$ coated on the fly ash heated at $700^{\circ}C$ for 2 h showed 1.25 g/cm$^3$of particle density, 82.8% of strength and 69.5 Lab of whiteness and can be used as a photocatalyst.

Pre-treatment effects on softening of carrot during enzyme immersion process (당근의 전처리 조건에 따른 효소의 연화 효과 비교)

  • Kim, Se-rin;Kim, Sun-min;Chang, Jin-Hee;Han, Jung-Ah
    • Korean Journal of Food Science and Technology
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    • v.50 no.3
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    • pp.292-296
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    • 2018
  • Softening effects of enzyme following pre-treatments were examined. Four pre-treatments: raw (R), heat (H), heat and freeze-thawing (HFT), heat and freeze-drying (HFD) were applied to carrot. Subsequently, each treated sample was immersed in 10% celluclast enzyme solution for up to 6 h and then their properties were compared. The minimum and the maximum color change was observed in HFD and H, respectively. R showed no change in hardness after 6 h immersion, indicating that the enzyme did not penetrate the carrot. The number and size of pores were greater in samples undergone HFT or HFD as observed by microstructure analysis using SEM, and HFD caused 99.5% reduction in hardness after 6 h immersion. After 6 h immersion post-HFT or 3 h immersion post-HFD, the hardness was less than $20,000N/m^2$, indicating tongue ingestion was possible, and the samples retained their original shape and easily collapsed by spoon pressing.

Surface Treatment of Al(OH)3 using Dilute Hydrofluoric Acid Aqueous Solution (저농도 HF 수용액을 이용한 Al(OH)3의 표면처리)

  • Kim, Do-Su;Lee, Churl-Kyoung;Yang, Dong-Hyo
    • Journal of the Korean Ceramic Society
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    • v.39 no.3
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    • pp.315-320
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    • 2002
  • Treatment effects of dilute hydrofluoric acid (6 wt% HF) on the surface properties of $Al(OH)_3$ were investigated at the molar ratio of F/Al(fluoride/aluminum)=0.15. Temperature and pH variations in the reaction system were recorded to analyze reaction mechanism between $Al(OH)_3$ and aqueous Hf. The reaction of HF to the surface of $Al(OH)_3$ accompanied with a quantity of heat evolution, resulting in increasing temperature of a reactionsystem. And also the reaction was proceeded as transitional state which metastable ${\alpha}-form\;AlF_3{\cdot}3H_2O$ was transferred to insoluble ${\beta}$-form. The resulting ${\beta}-form\;AlF_3{\cdot}3H_2O$ formed by a surface treatment was identified by FT-IR and X-ray diffractormetry. The formation of ${\beta}$-form aluminum fluoride hydrates with diameter less than $1{\mu}m$ on the surface of $Al(OH)_3$ could be visulaized by SEM imgae, making up a coating layer as precipitate-like. The surface whiteness of $Al(OH)_3$ treated with aqueous HF was furthermore increased approximately 6.6% due to the formation of surface hydrates.

Synthesis of Pt-Bi/Carbon Electrodes by Reduction Method for Direct Methanol Fuel Cell (환원법에 의한 직접 메탄올 연료전지(DMFC)용 Pt-Bi/Carbon 전극제조)

  • Kim, Kwan Sung;Kim, Min Kyung;Noh, Dong Kyun;Tak, Yongsug;Baeck, Sung-Hyeon
    • Applied Chemistry for Engineering
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    • v.22 no.5
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    • pp.479-485
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    • 2011
  • Pt-Bi/C catalysts supported on carbon black with various Pt/Bi ratios were synthesized by a reduction method. Chloroplatinic acid hydrate ($H_2PtCl_6{\cdot}xH_2O$) and bismuth (III) nitrate pentahydrate ($Bi(NO_3)_3{\cdot}5H_2O$) were used as precursors for Pt and Bi, respectively. Before loading metal on carbon, heat treatment and pretreatment of carbon black in an acidic solution was conducted to enhance the degree of dispersion. The physical property of the synthesized catalysts was investigated by X-ray diffraction and X-ray photoelectron spectroscopy. The XRD pattern of untreated Pt-Bi/C catalyst showed BiPt and $Bi_2Pt$ peaks in addition to Pt peaks. These results imply that Bi atoms were incorporated into the Pt crystal lattice by Pt-Bi alloy formation. The catalytic activity for methanol oxidation was measured using cyclic voltammetry in a mixture of 0.5 M $H_2SO_4$ and 0.5 M $CH_3OH$ aqueous solution. The addition of proper amount of Bi was found to significantly improve catalytic activity for methanol oxidation. The catalytic activity for methanol oxidation was closely related to the stability between electrode and electrolyte. In order to investigate the stability of catalysts, chronoamperometry analysis was carried out in the same solution at 0.6 V.

Investigation on the Preparation Method of TiO2-mayenite for NOx Removal (질소산화물 제거를 위한 TiO2-mayenite 제조 방법에 관한 연구)

  • Park, Ji Hye;Park, Jung Jun;Park, Hee Ju;Yi, Kwang Bok
    • Clean Technology
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    • v.26 no.4
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    • pp.304-310
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    • 2020
  • In order to apply a photocatalyst (TiO2) to various building materials, TiO2-mayenite was prepared in this study. The TiO2 was synthesized using the sol-gel method by fixing titanium isopropoxide (TTIP) and urea at a ratio of 1 : 1. Later, they were calcined in a temperature range of 400-700 ℃ to analyze the properties according to temperature. BET, TGA, and XRD were used to analyze the physical and chemical properties of TiO2. The nitrogen oxide removal test was confirmed by measuring the change in the concentration of NO for 1 h according to KS L ISO 22197-1. The prepared TiO2 samples exhibited an anatase crystal structure below 600 ℃, and TiO2 (urea)-400 showed the highest nitrogen oxide removal rate at 2.35 µmol h-1. TiO2-mayenite was prepared using two methods: spraying TiO2 dispersion solution (s/s) and sol-gel solution (g/s). Through BET and XRD analysis, it was found that 5-TiO2 (g/s) prepared by spraying a sol-gel solution has maintained its crystallinity even after heat treatment. Also, 5-TiO2 (g/s)-500 showed the highest removal rate of 0.55 µmol h-1 in the nitrogen oxide removal test. To prepare TiO2-mayenite, it was confirmed that mayenite should be blended with TiO2 in a sol-gel state to maintain the crystal structure and exhibit a high nitrogen oxide removal rate.

Preparation of Halloysite-Based Tubular Media for Enhanced Methylene Blue Adsorption (메틸렌 블루 흡착능 향상을 위한 할로이사이트 기반 튜브형 담체 연구)

  • Jeon, Junyeong;Cho, Yebin;Kim, Jongwook;Shin, Seung Gu;Jeon, Jong-Rok;Lee, Younki
    • Clean Technology
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    • v.27 no.4
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    • pp.359-366
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    • 2021
  • Halloysite nanotubes (HNTs), the multiwalled clay mineral with the composition of Al2Si2O5(OH)4·nH2O, have been highlighted as a low-cost adsorbent for the removal of dyes from wastewater. Although a powder of halloysite presents a high specific surface area, forming media are significantly considered due to sludge-clogging induced by the water-bound agglomeration. However, higher firing temperature to achieve the structural durability of the media and lower utilization rate due to longer penetration depth into the media act as hurdles to increase the dye-adsorption capacity. In this work, the retention of the adsorption capacity of halloysite was evaluated with methylene blue solution after the heat treatment at 750 ℃. In order to improve the utilization rate, tubular media were fabricated by extrusion. The images taken by transmission electron microscopy show that HNTs present excellent structural stability under heat treatment. The HNTs also provide superb capacity retention for MB adsorption (93%, 18.5 mg g-1), while the diatomite and Magnesol® XL show 22% (7.65 mg g-1) and 6% (11.7 mg g-1), respectively. Additionally, compositing with lignin enhances adsorption capacity, and the heat treatment under the hydrogen atmosphere accelerates the adsorption in the early stage. Compared to the rod-type, the tubular halloysite media rapidly increases methylene blue adsorption capacity.