• Title/Summary/Keyword: crystal structure analysis

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A study on the preparation and analysis of cordierite by sol-gel method (졸-겔법에 의한 코디어라이트 제조와 분석에 관한 연구)

  • Chun, Kyung Soo;Lee, Young Hwan
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.123-128
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    • 2008
  • The golden turbid solution of cordierite precursor was obtained by using magnesium ethoxide in sol-gel method, while the clear solution of cordierite precursor was obtained when 5%-$Zr(OC_3H_7)_4$ solution was used in the sol-gel reaction. $SiO_2$ component was confirmed by infrared spectra showing $1045cm^{-1}$ and the stretching vibration of gelish $SiO_4$ showed $1140cm^{-1}$ and $940cm^{-1}$. The component of $Al_2O_3$ showed at $580cm^{-1}$ and network structure of $Al_2O_6$ showed at $680cm^{-1}$. The component of MgO was confirmed at $575cm^{-1}$ as the stretching vibration. X-ray diffraction analysis showed ${\mu}$-cordierite crystal was showed up at temperature above $1000^{\circ}C$ at the mole ratio of cordierite precursor and water (1:5). ${\mu}$-Cordierite and ${\alpha}$-cordierite were coexisted at $1050^{\circ}C$ for the mole ratio of cordierite precursor and ammonia (1:5) while ${\alpha}$-cordierite was only existed at $1100^{\circ}C$ for the same mole ratio as mentioned above.

Alice Springs Orogeny (ASO) Footprints Tracing in Fresh Rocks in Arunta Region, Central Australia, Using Uranium/Lead (U-Pb) Geochronology

  • Kouame Yao;Mohammed O. Idrees;Abdul-Lateef Balogun;Mohamed Barakat A. Gibril
    • Economic and Environmental Geology
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    • v.56 no.6
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    • pp.817-830
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    • 2023
  • This study investigates the age of the surficial rocks in the Arunta region using Uranium-Lead (U-Pb) geochronological dating. Rock samples were collected at four locations, Cattle-Water Pass (CP 1610), Gough Dam (GD 1622 and GD 1610), and London-Eye (LE 1601), within the Strangways Metamorphic Complex and crushed by selFragging. Subsequently, the zircon grains were imaged using Cathodoluminescence (CL) analysis and the U-Pb (uranium and lead) isotope ratios and the chrono-stratigraphy were measured. The imaged zircon revealed an anomalous heterogeneous crystal structure. Ellipses of the samples at locations GD1601, CP1610, and GD1622 fall below the intercept indicating the ages produced discordant patterns, whereas LE1601 intersects the Concordia curve at two points, implying the occurrence of an event of significant impact. For the rock sample at CP1610, the estimated mean age is 1742.2 ± 9.2 Ma with mean squared weighted deviation (MSWD) = 0.49 and probability of equivalence of 0.90; 1748 ± 15 Ma - MSWD = 1.02 and probability of equivalence of 0.40 for GD1622; and 1784.4 ± 9.1 Ma with MSWD of 1.09 and probability of equivalence of 0.37 for LE1601. But for samples at GD1601, two different age groups with different means occurred: 1) below the global mean (1792.2 ± 32 Ma) estimated at 1738.2 ± 14 Ma with MSWD of 0.109 and probability of equivalence of 0.95 and 2) above it with mean of 1838.22 ± 14 Ma, MSWD of 1.6 and probability of equivalence of 0.95. Analysis of the zircon grains has shown a discrepancy in the age range between 1700 Ma and 1800 Ma compared to the ASO dated to have occurred between 440 and 300 Ma. Moreover, apparent similarity in age of the core and rim means that the mineral crystallized relatively quickly without significant interruptions and effect on the isotopic system. This may have constraint the timing and extent of geological events that might have affected the mineral, such as metamorphism or hydrothermal alteration.

Sol-Gel Synthesis, Crystal Structure, Magnetic and Optical Properties in ZnCo2O3 Oxide

  • Das, Bidhu Bhusan;Barman, Bittesh
    • Journal of the Korean Chemical Society
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    • v.63 no.6
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    • pp.453-458
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    • 2019
  • Synthesis of ZnCo2O3 oxide is performed by sol-gel method via nitrate-citrate route. Powder X-ray diffraction (XRD) study shows monoclinic unit cell having lattice parameters: a = 5.721(1) Å, b = 8.073(2) Å, c = 5.670(1) Å, β = 93.221(8)°, space group P2/m and Z = 4. Average crystallite sizes determined by Scherrer equation are the range ~14-32 nm, whereas SEM micrographs show nano-micro meter size particles formed in ZnCo2O3. Endothermic peak at ~798 K in the Differential scanning calorimetric (DSC) trace without weight loss could be due to structural transformation and the endothermic peak ~1143 K with weight loss is due to reversible loss of O2 in air atmosphere. Energy Dispersive X-ray (EDX) analysis profile shows the presence of elements Zn, Co and O which indicates the purity of the sample. Magnetic measurements in the range of +12 kOe to -12 kOe at 10 K, 77 K, 120 K and at 300 K by PPMS-II Physical Property Measurement System (PPMS) shows hysteresis loops having very low values of the coercivity and retentivity which indicates the weakly ferromagnetic nature of the oxide. Observed X-band EPR isotropic lineshapes at 300 K and 77 K show positive g-shift at giso ~2.230 and giso ~2.217, respectively which is in agreement with the presence of paramagnetic site Co2+(3d7) in the oxide. DC conductivity value of 2.875 ×10-8 S/cm indicates very weakly semiconducting nature of ZnCo2O3 at 300 K. DRS absorption bands ~357 nm, ~572 nm, ~619 nm and ~654 nm are due to the d-d transitions 4T1g(4F)→2Eg(2G), 4T1g(4F)→4T1g(4P), 4T1g(4F)→4A2g(4F), 4T1g(4F)→4T2g(4F), respectively in octahedral ligand field around Co2+ ions. Direct band gap energy, Eg~ 1.5 eV in the oxide is obtained by extrapolating the linear part of the Tauc plot to the energy axis indicates fairly strong semiconducting nature of ZnCo2O3.

SURFACE CHARACTERISTICS AND BIOLOGICAL RESPONSES OF HYDROXYAPATITE COATING ON TITANIUM BY HYDROTHERMAL METHOD: AN IN VITRO STUDY

  • Kim, Dong-Seok;Kim, Chang-Whe;Jang, Kyung-Soo;Lim, Young-Jun
    • The Journal of Korean Academy of Prosthodontics
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    • v.43 no.3
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    • pp.363-378
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    • 2005
  • Statement of problem. Hydroxyapatite(HA) coated titanium surfaces have not yet showed the reliable osseointegration in various conditions. Purpose. This study was aimed to investigate microstructures, chemical composition, and surface roughness of the surface coated by the hydrothermal method and to evaluate the effect of hydrothermal coating on the cell attachment, as well as cell proliferation. Material and Methods. Commercially pure(c.p.) titanium discs were used as substrates. The HA coating on c.p. titanium discs by hydrothermal method was performed in 0.12M HCl solution mixed with HA(group I) and 0.1M NaOH solution mixed with HA(group II). GroupⅠ was heated at 180 $^{\circ}C$ for 24, 48, and 72 hours. GroupⅡ was heated at 180 $^{\circ}C$ for 12, 24, and 36 hours. And the treated surfaces were evaluated by Scanning electron microscopy(SEM), Energy dispersive X-ray spectroscopy(EDS), X-ray photoelectron spectroscopy(XPS), X-ray diffraction method(XRD), Confocal laser scanning microscopy(CLSM). And SEM of fibroblast and 3-(4,5- dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide(MTT) assay were used for cellular responses of the treated surfaces. Results. The color of surface changed in both groups after the hydrothermal process. SEM images showed that coating pattern was homogeneous in group II, while inhomogeneous in group I. H72 had rosette-like precipitates. The crystalline structure grew gradually in group II, according to extending treatment period. The long needle-like crystals were prominent in N36. Calcium(Ca) and phosphorus(P) were not detected in H24 and H48 in EDS. In all specimens of group II and H72, Ca was found. Ca and P were identified in all treated groups through the analysis of XPS, but they were amorphous. Surface roughness did not increase in both groups after hydrothermal treatment. The values of surface roughness were not significantly different between groups I and II. According to the SEM images of fibroblasts, cell attachments were oriented and spread well in both treated groups, while they were not in the control group. However, no substantial amount of difference was found between groups I and II. Conclusions. In this study during the hydrothermal process procedure, coating characteristics, including the HA precipitates, crystal growth, and crystalline phases, were more satisfactory in NaOH treated group than in HCl treated group. Still, the biological responses of the modified surface by this method were not fully understood for the two tested groups did not differ significantly. Therefore, more continuous research on the relationship between the surface features and cellular responses seems to be in need.

Synthesis and Characterization of The Electrolessly Deposited Co(Re,P) Film for Cu Capping Layer (무전해 도금법으로 제조된 Co(Re,P) capping layer제조 및 특성 평가)

  • Han, Won-Kyu;Kim, So-Jin;Ju, Jeong-Woon;Cho, Jin-Ki;Kim, Jae-Hong;Yeom, Seung-Jin;Kwak, Noh-Jung;Kim, Jin-Woong;Kang, Sung-Goon
    • Korean Journal of Materials Research
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    • v.19 no.2
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    • pp.61-67
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    • 2009
  • Electrolessly deposited Co (Re,P) was investigated as a possible capping layer for Cu wires. 50 nm Co (Re,P) films were deposited on Cu/Ti-coated silicon wafers which acted as a catalytic seed and an adhesion layer, respectively. To obtain the optimized bath composition, electroless deposition was studied through an electrochemical approach via a linear sweep voltammetry analysis. The results of using this method showed that the best deposition conditions were a $CoSO_4$ concentration of 0.082 mol/l, a solution pH of 9, a $KReO_4$ concentration of 0.0003 mol/l and sodium hypophosphite concentration of 0.1 mol/L at $80^{\circ}C$. The thermal stability of the Co (Re,P) layer as a barrier preventing Cu was evaluated using Auger electron spectroscopy and a Scanning calorimeter. The measurement results showed that Re impurities stabilized the h.c.p. phase up to $550^{\circ}C$ and that the Co (Re,P) film efficiently blocked Cu diffusion under an annealing temperature of $400^{\circ}C$ for 1hr. The good barrier properties that were observed can be explained by the nano-sized grains along with the blocking effect of the impurities at the fast diffusion path of the grain boundaries. The transformation temperature from the amorphous to crystal structure is increased by doping the Re.

The Defect Characterization of Luminescence Thin Film by the Positron Annihilation Spectroscopy (양전자 소멸 측정을 이용한 발광 박막 구조 결함 특성)

  • Lee, Kwon Hee;Bae, Suk Hwan;Lee, Chong Yong
    • Journal of the Korean Vacuum Society
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    • v.22 no.5
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    • pp.250-256
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    • 2013
  • It is described that the proton beam induces micro-size defects and electronic deep levels in luminescence Thin Film. Coincidence Doppler Broadening Positron Annihilation Spectroscopy (CDBPAS) and Positron lifetime Spectroscopy were applied to study of characteristics of a poly crystal samples. In this investigation the numerical analysis of the Doppler spectra was employed to the determination of the shape parameter, S-parameter value. The samples were exposed by 3.0 MeV proton beams with the intensities ranging between 0 to ${\sim}10^{14}$ particles. The S-parameter values decreased as increased the proton beam, that indicates the protons trapped in vacancies. Lifetime ${\tau}_1$ shows that positrons are trapped in mono vacancies. Lifetime ${\tau}_2$ is not changed according to proton irradiation that indicate the cluster vacancies of the grain structure.

Photoluminescent Properties of $\textrm{Zn}_2\textrm{SiO}_4$:Mn Green Phosphors Prepared by the Solution Reaction Method (액상반응법으로 제조한 $\textrm{Zn}_2\textrm{SiO}_4$:Mn 녹색 형광체의 발광특성)

  • Park, Eung-Seok;Jang, Ho-Jeong;Jo, Tae-Hwan
    • Korean Journal of Materials Research
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    • v.9 no.1
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    • pp.46-50
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    • 1999
  • $\textrm{Zn}_{2-x}\textrm{Mn}_{x}\textrm{SiO}_{4}$ green phosphors have been prepared by the solution reaction method and the photoluminescence and crystalline properties were studied as a function of both the firing temperature ($900^{\circ}C$~$1200^{\circ}C$) and the concentration of Mn activator (x=0.01~0.20). Under 147 nm and 254nm and excitation sources, the emission intensity of the phosphors was increased about 4 times increasing firing temperatures from $900^{\circ}C$ to $1200^{\circ}C$. From the XRD analysis, $\textrm{Zn}_{2}\textrm{SiO}_{4}$:Mn phosphors fired above $1100^{\circ}C$ showed willemite crystal structure. Under 147nm excitation, the maximum emission intensity was obtained at the Mn concentration of x=0.02 for $\textrm{Zn}_{2-x}\textrm{Mn}_{x}\textrm{SiO}_{4}$ phosphors fired at $1200^{\circ}C$ and the concentration quenching was occurred at the Mn concentration above x=0.10. The phosphor particles showed almost spherical shapes with the average size of around 2~3$\mu\textrm{m}$ by the SEM morphology.

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A Study on Characteristics of Leachability and Compressive Strength of Incinerator Fly Ash, Cement and Waste Stone Powder by Solidification (산업폐기물 소각장 비산재의 시멘트 및 폐석분 고형화시 압축강도 및 용출특성)

  • Jung, Ho-Young;Kim, Young-Ju;Kim, Ji-Hoon
    • Journal of Korean Society of Environmental Engineers
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    • v.30 no.5
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    • pp.560-566
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    • 2008
  • In this paper, the solidification behaviour and compressive strength of fly ash, cement, and waste stone powder were studied each separately and with addition of each in different proportions. And also, we assessed stabilizing ability of waste stone powder in cement which was added in fly ash. The particle size of waste stone powder was found smaller than the fly ash and cement particle sizes. Moreover, when mixing all(fly ash, cement, and waste stone powder) showed distinctive crystal structure, and improved stiffness. In case of mixing fly ash, cement and waste stone powder in different proportions, the compressive strength was exceeded to the predicted compressive strength of 10 kgf/cm$^2$. The XRD analysis showed high contents of CaO in fly ash and SiO$_2$ in case of waste stone powder sample. Heavy metal emission experiment showed the 3mg/L of Pb after 14 days of mixing 150 kg/m$^3$ of cement with the 80$\sim$100 kg/m$^3$ of waste stone powder, which is fulfilling the National Waste Management Policy.

Optical properties of Nb2O5 thin films prepared by ion beam assisted deposition (이온빔 보조 증착 Nb2O5 박막의 광학적 특성)

  • 우석훈;남성림;정부영;황보창권;문일춘
    • Korean Journal of Optics and Photonics
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    • v.13 no.2
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    • pp.105-112
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    • 2002
  • We studied the optical and structural properties of conventional and ion-beam-assisted-deposition (IBAD) Nb$_2$O$_{5}$ films which were evaporated by an electron beam gun. The vacuum-to-air spectral shift and the cross sectional SEM images of the Nb$_2$O$_{5}$ films were investigated. The results show that the IBAD Nb$_2$O$_{5}$ films have a higher packing density than the conventional Nb$_2$O$_{5}$ films. The average refractive index of IBAD Nb$_2$O$_{5}$ films was increased, while the extinction coefficient was decreased compared with the conventional films. As the oxygen flow was increased, the average refractive index and extinction coefficient of the conventional and IBAD films decreased. Both the conventional and IBAD Nb$_2$O$_{5}$ films showed inhomogeneity in refractive index, and the degree of inhomogeneity of the IBAD Nb$_2$O$_{5}$ films became larger as the ion current density was increased. All Nb$_2$O$_{5}$ films were found to be amorphous by x-ray diffraction (XRD) analysis, and hence the crystal structure of Nb$_2$O$_{5}$ films was not changed by IBAD.

Adsoptive Properties of Cellulose Thermally Treated at Low Temperature and Its Solubility to Water (저온 열처리 셀룰로오스의 염기성가스 흡착과 용해특성)

  • Jo, Tae-Su;Ahn, Byung-Jun;Choi, Don-Ha;Akihiko, Miyakoshi
    • Journal of the Korean Wood Science and Technology
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    • v.33 no.6 s.134
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    • pp.63-70
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    • 2005
  • The purpose of this study was to investigate how to modify the physical properties of cellulose after thermal treatment. Cellulose was treated between $225^{\circ}C$ and $325^{\circ}C$ for 3 hrs under air flow, and then the thermally treated cellulose was measured to specific surface area, constitute elements, consumption ofacid and base, as well as the adsorption capacity of ethylamine vapor. The higher was the treating temperature from $225^{\circ}C$ to $325^{\circ}C$, the lower was the total yield of cellulose. Elemental analysis revealed that carbon content in thermally treated cellulose was gradually increased in proportion to temperature increment. The amount of acidic functional groups tended to increase up to $300^{\circ}C$, after then to be lowered slightly. In principle, no alkaline functional groups were found in thermally treated cellulose. In case of treatment with $325^{\circ}C$, only a few amount of alkaline functional groups were detectable. Specific surface area of thermally treated cellulose are determined to $1.9m^2/g$, which value can become higher when the treated temperature rises. The thermally treated cellulose at $275^{\circ}C$ shows the highest adsorption capacity of ethylamine at $40^{\circ}C$ for 4 hrs. Solubility of those two celluloses with WPG (Weight Percent Gain) value of 113% and 108%, respectively, was determined to almost 100%. X-ray diffractogram of thermally treated cellulose suggested that the crystalline structure of cellulose began to be destroyed at the temperature of $275^{\circ}C$. As a conclusion, changes of such a physical properties make it possible to weaken inter and/or intra hydrogen bond in crystal region of cellulose macromolecules. When thermally treated cellulose adsorbs ethylamine, it turns to be well soluble to water.