• Title/Summary/Keyword: Annealing Process

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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.

High Tc Superconductor Fiber $YBa_2Cu_3O_{7-{\sigma}}$ Synthesized by the Sol-gel Process (Sol-gel 법에 의한 고온 초전도체 $YBa_2Cu_3O_{7-{\sigma}}$ 선재 합성에 관한 연구)

  • Jin Ho Choy;Jong Seok Yoo;Bae Whan Kim;Seung Tae Hong
    • Journal of the Korean Chemical Society
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    • v.33 no.3
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    • pp.326-331
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    • 1989
  • Superconducting fiber of high Tc $YBa_2Cu_3O_{7-{\sigma}}$ was successfully prepared by the sol-gel method. The stoichiometric mixture of Y, Ba and Cu nitrates was dissolved in water, to which citric acid solution was added. Then ammonium hydroxide was added to the mixture in order to increase the pH to a value between 5.8 and 6.2. The mixture was heated carefully to form a homogeneous colloid sol at 358 K. The solution was viscous enough to draw a long gel fiber, which was then heated at 1223K for 8 hrs. under oxygen partial pressure of $Po_2$ = 1 atm., cooled slowly and annealed at 723K for 13 hrs.. The reacted superconducting sample maintained a fiber form with some shrinkage of its volume. The superconducting transition temperatures (Tc, onset and Tc, offset) of $YBa_2Cu_3O_{7-{\sigma}}$ have been determined to be approximately 95K and 82K, respectively. The superconducting phase was also confirmed by Meissner effect at liquid nitrogen boiling temperature.

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Fabrication and loss measurement of $P_2O_5-SiO_2$ optical waveguides on Si (Si을 기판으로한 $P_2O_5-SiO_2$ 광도파로의 제작 및 손실측정)

  • 이형종;임기건;정창섭;정환재;김진승
    • Korean Journal of Optics and Photonics
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    • v.3 no.4
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    • pp.258-265
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    • 1992
  • A low loss optical waveguide of $P_{2}O_{5}-SiO_{2}$on Si substrate is produced by using the chemical vapour deposition method of $SiO_2$ thin films used in Si technology. Propagation loss of the waveguide layer was 1.65 dB/cm as produced and reduced down to 0.1 dB/cm after heat treatment at $1100^{\circ}C$. By using laser lithography and reactive ion etching method $P_{2}O_{5}-SiO_{2}$ waveguide was produced and subsequently annealed at $1100^{\circ}C$.As a result of this annealing the shape of the waveguide core was changed from rectangular to semi-circular form, and the propagation loss was reduced as down to 0.03 dB/cm at 0.6328$\mu$m and 0.04dB/cm at 1.53$\mu$m. We think that the mechanism of the reduction in propagation loss during the heat treatment is the following: 1) The hydrogen bonding in waveguide layer, which causes absorption loss, is dissociated and diffused out. 2) The roughness of the interface and the micro-structure of the waveguide layer is removed. 3) The irregularities in the cross-sectional shape of the waveguide which was induced during the lithographic process were disappeared by flowing of the waveguide core.

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Determination of the complex refractive index of $Ge_2Sb_2Te_5$ using spectroscopic ellipsometry (분광타원해석법을 이용한 $Ge_2Sb_2Te_5$ 의 복소굴절율 결정)

  • Kim, S. J.;Kim, S. Y.;Seo, H.;Park, J. W.;Chung, T. H.
    • Korean Journal of Optics and Photonics
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    • v.8 no.6
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    • pp.445-449
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    • 1997
  • The complex refractive indices of $Ge_2Se_2Te_5$ which show reversible phase change between the crystalline phase and an amorphous one depending upon the annealing process have been determined in the spectral range of 0.7-4.5 eV. The $Ge_2Se_2Te_5$ films were DC sputter deposited on the crystalline silicon substrate. The spectro-ellipsometry data of a thick film were analyzed following the modelling procedure where the quantum mechanical dispersion relation were used for the complex refractive indices of both the cryastalline phase $Ge_2Se_2Te_5$ and and amorphous phase $Ge_2Se_2Te_5$, respectively. On the other hand, with the surface micro-roughness layer whose effective thickness was determined from AFM analysis, the spectro-ellipsometry data were numerically inverted to yield the complex refractive index of $Ge_2Se_2Te_5$ at each wavelength. With these set of complex refractive indices, the reflectance spectra were calculated and those spectra obtained from the numerical inversion showed better agreement with the experimental reflection spectra for both the cryastalline phase and an amorphous phase. Finally, the thin $Ge_2Se_2Te_5$ film which has the optimum thickness of 26 nm as the medium for optical recording was also analyzed and the quantitative result of the film thickness and the surface microroughness has been reported.

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New Magnetic Phases of Fe-N and Mn-Al Alloys Produced by Mechanochemical Milling (기계적 밀링 및 화학적 추출법에 의해 제조한 Fe-N 및 Mn-Al계의 새로운 자성재료)

  • Kyu-Jin Kim;Tae-Hwan Noh;Kenji Suzuki
    • Journal of the Korean Magnetics Society
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    • v.4 no.4
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    • pp.347-354
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    • 1994
  • The structural change and magnetic properties of mechanically milled Fe-N and Mn-Al alloy powders have been investigated by XRD, TEM, VSM, $M\"{o}ssbauer$ spectroscopy and inelastic neutron scattering measurements. During milling of ${\gamma}'-Fe_{4}N$ powders, and fcc ${\gamma}'-Fe_{4}N$ phase is transformed to a bct ${\alpha}'-Fe(N)$ phase by stress-induced martensitic transformation, being accompanied by an initial increase in saturation magnetization. During annealing the bct ${\alpha}'-Fe(N)$ nanocrystalline phase which is obtained by mechanical grinding for a long time, an ${\alpha}'-Fe_{16}N_{2}$ phase partially appears as an intermediate phase at 673~773 K, causing an increase in saturation magnetization. During milling of Mn-45, 70 and 85 at.% Al mixed powders, Al atoms are partially solubilized into an ${\alpha}-Mn$ phase. The Al supersaturated ${\alpha}-Mn-type$ phases change from paramagnetic to ferromagnetic : the saturation magnetization is 11 emu/g for the as-milled Mn-70 at.% Al powders. Moreover, by removing almost all Al atoms from the as-milled Mn-85 at.% Al powders using chemical leaching, the saturation magnetization increases up to 36 emu/g. The above bct ${\alpha}'-Fe(N)$ and ferromagnetic ${\alpha}-Mn$ type alloys are the magnetic materials found for the first time, by using the present mechanochemical process.

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Effects of Temperature and Mechanical Deformation on the Microhardness of Lead free and Composite Solders (무연 복합 솔더의 미소경도에 미치는 기계적 변형과 온도의 영향)

  • Lee Joo Won;Kang Sung K.;Lee Hyuck Mo
    • Journal of the Microelectronics and Packaging Society
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    • v.12 no.2 s.35
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    • pp.121-128
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    • 2005
  • Solder joints in microelectronic devices are frequently operated at an elevated temperature in service. They also experience plastic deformation caused by temperature excursion and difference in thermal expansion coefficients. Deformed solders can go through a recovery and recrystallization process at an elevated temperature, which would alter their microstructure and mechanical properties. In this study, to predict the changes in mechanical properties of Pb-free solder joints at high temperatures, the high temperature microhardness of several Pb-free and composite solders was measured as a function of temperature, deformation, and annealing condition. Solder alleys investigated include pure Sn, Sn-0.7Cu, Sn-3.5Ag, Sn-3.8Ag-0.7Cu, Sn-2.8Ag-7.0Cu (composite), and Sn-2.7Ag-4.9Cu-2.9Ni (composite). Numbers are all in wt.$\%$ unless specified otherwise. Solder pellets were cast at two cooling rates (0.4 and $7^{\circ}C$/s). The pellets were compressively deformed by $30\%$ and $50\%$ and annealed at $150^{\circ}C$ for 2 days. The microhardness was measured as a function of indentation temperature from 25 to $130^{\circ}C$. Their microstructure was also evaluated to correlate with the changes in microhardness.

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Ferroelectric domain inversion in $LiNbO_3$ crystal plate during heat treatment for Ti in-diffusion ($Ti:LiNbO_3$ 도파로 제작을 위한 열처리 과정 동안 강유전 도메인 특성에 미치는 영향)

  • Yang, W.S.;Lee, H.Y.;Kwon, S.W.;Kim, W.K.;Lee, H.Y.;Yoon, D.H.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.15 no.3
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    • pp.124-127
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    • 2005
  • It is demonstrated that the annealing process for Ti in-diffusion to z-cut $LiNbO_3$ at temperature lower than the curie temperature in a platinum (Pt) box can cause a ferroelectric micro-domain inversion at the +z surface and Li out-diffusion, therefore which should be avoided or suppressed for waveguide type periodically poled lithium niobate (PPLN) devices. The depth of the inversion layer depends on the Ti-diffusion conditions such as temperature, atmosphere, the sealing method of $LiNbO_3$ in the Pt box and crystal orientation is experimentally examined. The result shows that the polarization-inverted domain boundary appears at the only +z surface and its thickness is about $1.6{\mu}m$. Also, for the etched $LiNbO_3$, surface the domain shape was observed by the optical microscope and atomic force microscopy (AEM), and distribution of the cation concentrations in the $LiNbO_3$ crystal by the secondary ion mass spectrometry (SIMS).

Effect of magnetic separation in removal of Cr and Ni from municipal solid waste incineration (MSWI) bottom ash (생활폐기물(生活廢棄物) 소각(燒却) 바닥재의 자력선별(磁力選別)에 따른 크롬과 니켈의 거동(擧動))

  • Ahn, Ji-Whan;Um, Nam-Il;Cho, Kye-Hong;Oh, Myung-Hwan;You, Kwang-Suk;Han, Gi-Chun;Cho, Hee-Chan;Han, Choon;Kim, Byong-Gon
    • Resources Recycling
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    • v.16 no.6
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    • pp.3-9
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    • 2007
  • Although the ferrous material was separated by the magnetic separation before the incineration process, the municipal solid waste incineration bottom ash generated during incinerator in metropolitan area consists of many iron products which account for about $3{\sim}11%$ as well as ceramics and glasses. The formation of $NiFe_2O_4$ and $FeCr_2O_4$ with a $Fe_3O_4-Fe_2O_3$ (similar to pure Fe) on the surface of iron product was found during air-annealing in the incinerator at $1000^{\circ}C$, because Ni and Cr has a chemical attraction about iron is using to coat with Ni and Cr metals for poish or to prevent corrosion. Therefore, Fe-Ni Cr oxide can be formed on durface of the iron product and it can be separated from bottom ash through the magnetic separation. So, in this study, the separation ratio of heavy metals as magnetic separation and mineralogical formation of Fe-ion(heavy metal) in ferrous metals corroded were investigated. As the result, the separation ratio of Ni and Cr based on particle sizes accounted for about $45{\sim}50%$, and Cu and Pb accounted for below 20%. Also, the leaching concentration of Ni and Cr in bottom ash separated by magnetic separation was lower than that in fresh bottom ash.

Removal of Fe Impurities on Silicon Surfaces using Remote Hydrogen Plasma (리모트 수소 플라즈마를 이용한 Si 표면 위의 Fe 불순물 제거)

  • Lee, C.;Park, W.;Jeon, B.Y.;Jeon, H.T.;Ahn, T.H.;Back, J.T.;Shin, K.S.;Lee, D.H.
    • Korean Journal of Materials Research
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    • v.8 no.8
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    • pp.751-756
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    • 1998
  • Effects of remote hydrogen plasma cleaning process parameters on the removal of Fe impurities on Si surfaces and the Fe removal mechanism were investigated. Fe removal efficiency is enhanced with decreasing the plasma exposure time and increasing the rf-power. The optimum plasma exposure time and rf-power are 1 min and 100W. respectively, in the range below 10 min and 100W. Fe removal efficiency is better under lower pressures than higher pressures, and the optimum $\textrm{H}_2$ flow rate was found to be 20 and 60sccm, respectively, under a low and a high pressure. The post-RHP(remote hydrogen plasma) annealing enhanced metallic contaminants removal efficiency, and the highest efficiency was achieved at $600^{\circ}C$. According to the AFM analysis results Si surface roughness was improved by 30-50%, which seems to be due to the removal of particles by the plasma cleaning. Also. Fe impurities removal mechanisms by remote hydrogen plasma are discussed.

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Ferroelectric Properties of ErMnO3 Thin Film Prepared by Sol-gel Method (졸겔법으로 제조한 ErMnO3 박막의 강유전 특성)

  • Kim, Yoo-Taek;Kim, Eung-Soo;Chae, Jung-Hoon;Ryu, Jae-Ho
    • Journal of the Korean Ceramic Society
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    • v.39 no.9
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    • pp.829-834
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    • 2002
  • Ferroelectric properties of $ErMnO_3$ thin films deposited on Si(100) substrate using Sol-gel process with metal salts were investigated. $ErMnO_3$ thin films with a (001) preferred orientation were crystallized at 800$^{\circ}C$. The $ErMnO_3$ thin film post-annealed at 800$^{\circ}C$ for 1 h showed the dielectric constant(k) of 26 and the dielectric loss(tan ${\delta}$) of 0.032 at the frequency range from 1 to 100 KHz. The grain size of $ErMnO_3$ thin film post-annealed at 800 for 1 h was 10∼30 nm. The remanent polarization($P_r$) of the $ErMnO_3$ thin films increased with increasing (001) preferred orientation. The $ErMnO_3$ thin films post-annealed at 800$^{\circ}C$ for 1 h showed the remanent polarization($P_r$) of 400 nC/$cm^2$, with the increase of post-annealing time at 800$^{\circ}C$, the coercive field($E_c$) of thin films was lowered because the dense and homogeneous thin films were obtained.