• Journal of the Korean Magnetics Society
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• v.16 no.1
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• pp.60-65
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• 2006

In order to investigate the dependence of the particle size on the cation distribution in the spinel structure, Mossbauer spectra were taken in the presence of an external magnetic field f3r the magnetic nanoparticles prepared by using a microemulsion method. The crystals are found to have a cubic structure. The results show that as the particle sizes decrease, $Fe^{3+}$ ions migrate from the octahedral site to tetrahedral site.

• Metals and materials international
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• v.24 no.6
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• pp.1285-1292
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• 2018

Microstructural properties of as-grown and annealed CoCrFeMnNi high entropy alloy (HEA) oxynitride thin films were investigated. The CoCrFeMnNi HEA oxynitride thin film was grown by magnetron sputtering method using an air gas, and annealed under the argon plus air flow for 5 h at $800^{\circ}C$. The as-grown film was homogeneous and uniform composed of nanometer-sized crystalline regions mixed with amorphous-like phase. The crystalline phase in the as-grown film was face centered cubic structure with the lattice constant of 0.4242 nm. Significant microstructural changes were observed after the annealing process. First, it was fully recrystallized and grain growth happened. Second, Ni-rich region was observed in nanometer-scale range. Third, phase change happened and it was determined to be $Fe_3O_4$ spinel structure with the lattice constant of 0.8326 nm. Hardness and Young's modulus of the as-grown film were 4.1 and 150.5 GPa, while those were 9.4 and 156.4 GPa for the annealed film, respectively.

• Journal of the Korean Ceramic Society
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• v.44 no.11
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• pp.639-644
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• 2007

Spinel pigments, developing black color in high temperature glazes at oxidation or reduction atmosphere, without CoO because of its high price were synthesized by solid solution method. Ten mixed compositions consisted of NiO, MnO, $Fe_2O_3 and $Mn_2O_3$ were fired at $1250^{\circ}C$ for 1h. The resulting pigments were characterized by using XRD, FT-IR, SEM and UV-vis spectrometer. Structure of the pigments are spinel and particles' shape are spherical or cubic. Glazed tiles containing 5 wt% pigments were fired at $1260^{\circ}C$ and $1240^{\circ}C$ in reduction atmosphere. Color in glazes were analyzed by UV-vis spectrometer. Colors of NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.4875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0125 mole% and NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.3875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.1125 mole% in lime glaze showed black in oxidation, in reduction NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.4875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0125 mole% and NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.55{\cdot}Mn_2O_3$ 0.0125 mole% showed black. In case of lime-barium glaze, NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.3875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.1125 mole%, NiO 0.975 MnO $0.075{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0625 mole% and NiO 0.925 MnO $0.075{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0625 mole% showed black color in oxidation and NiO 0.875 MnO $0.125{\cdot}Fe_2O_3$ $0.3875{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.1125 mole%, NiO 0.925 MnO $0.075{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0625 mole% and NiO 0.725 MnO $0.275{\cdot}Fe_2O_3$ $0.4375{\cdot}Cr_2O_3$ $0.50{\cdot}Mn_2O_3$ 0.0625 mole% showed black one in reduction.

• Journal of the Korean Applied Science and Technology
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• v.20 no.1
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• pp.33-43
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• 2003

$LiMn_2O_4$ catalyst for $CO_2$ decomposition was synthesized by oxidation method for 30 min at 600$^{\circ}C$ in an electric furnace under air condition using manganese(II) nitrate $(Mn(NO_3)_2{\cdot}6H_2O)$, Lithium nitrate ($LiNO_3$) and Urea $(CO(NH_2)_2)$. The synthesized catalyst was reduced by $H_2$ at various temperatures for 3 hr. The reduction degree of the reduced catalysts were measured using the TGA. And then $CO_2$ decomposition rate was measured using the reduced catalysts. Phase-transitions of the catalysts were observed after $CO_2$ decomposition reaction at an optimal decomposition temperature. As the result of X-ray powder diffraction analysis, the synthesized catalyst was confirmed that the catalyst has the spinel structure, and also confirmed that when it was reduced by $H_2$, the phase of $LiMn_2O_4$ catalyst was transformed into $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase. After $CO_2$ decomposition reaction, it was confirmed that the peak of $LiMn_2O_4$ of spinel phase. The optimal reduction temperature of the catalyst with $H_2$ was confirmed to be 450$^{\circ}C$(maximum weight-increasing ratio 9.47%) in the case of $LiMn_2O_4$ through the TGA analysis. Decomposition rate(%) using the $LiMn_2O_4$ catalyst showed the 67%. The crystal structure of the synthesized $LiMn_2O_4$ observed with a scanning electron microscope(SEM) shows cubic form. After reduction, $LiMn_2O_4$ catalyst became condensed each other to form interface. It was confirmed that after $CO_2$ decomposition, crystal structure of $LiMn_2O_4$ catalyst showed that its particle grew up more than that of reduction. Phase-transition by reduction and $CO_2$ decomposition ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase at the first time of $CO_2$ decomposition appear like the same as the above contents. Phase-transition at $2{\sim}5$ time ; $Li_2MnO_3$ and $Li_{1-2{\delta}}Mn_{2-{\delta}}O_{4-3{\delta}-{\delta}'}$ of tetragonal spinel phase by reduction and $LiMn_2O_4$ of spinel phase after $CO_2$ decomposition appear like the same as the first time case. The result of the TGA analysis by catalyst reduction ; The first time, weight of reduced catalyst increased by 9.47%, for 2${\sim}$5 times, weight of reduced catalyst increased by average 2.3% But, in any time, there is little difference in the decomposition ratio of $CO_2$. That is to say, at the first time, it showed 67% in $CO_2$ decomposition rate and after 5 times reaction of $CO_2$ decomposition, it showed 67% nearly the same as the first time.

• Journal of the Korean Magnetics Society
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• v.7 no.2
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• pp.76-81
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• 1997

$Cu_{0.9}Ni_{0.1}Fe_2O_4$ has been studied with Mossbauer spectroscopy and X-ray diffraction. The crystal structure is found to be a cubic spinel with the lattice constant $a_0=8.386{\AA}$. The Curie temperature is determined to be $T_c=755K$ for a heating rate of 5 K/ min. The Mossbauer spectra consist of two six-line patterns corresponding to $Fe^{3+}$ at the tetrahedral(A) and octahedral(B) sites. Debye temperatures for A and B sites are found to be 568 k and 194 K, respectively. Atomic migration of $Cu_{0.9}Ni_{0.1}Fe_2O_4$ begins near 350 K and increases rapidly with increasing temperature such a degree that 71% of the ferric ions as A sites have moved over to the B sites at 550 K.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.27 no.4
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• pp.226-231
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• 2014

Thin thermistor films of solutions with nickel and manganese oxides were prepared by metal-organic decomposition (MOD). The structural properties of the thin films were investigated as a function of annealing temperature. Field emission scanning electron microscope (FE-SEM) results indicated that the thin films had a thin thickness, smooth and dense surface. The crystallization temperature of $414.9^{\circ}C$ was confirmed from thermogavimetric-differential thermal analysis (TG-DTA) curve. A single phase of cubic spinel structure was obtained for the thin film annealed from $700^{\circ}C$ to $800^{\circ}C$, which was confirmed from the X-ray diffraction (XRD). From the selected area electron diffraction (SAED) in high resolution transmission electron microscope (HRTEM), the nano grains (2~3 nm) of spinel phase with (311) and (222) planes were detected for the thin film annealed at $500^{\circ}C$, which could be applicable to read-out integrated circuit (ROIC) substrate of the uncooled microbolometer with low processing temperature.

• Journal of the Korean Magnetics Society
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• v.15 no.2
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• pp.137-141
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• 2005

The CMR properties and magnetic properties of sulphospinels $Zn_xFe_{1-x}Cr_2S_4$ have been explored by X-ray diffraction, magnetoresistance measurement, and $M\ddot{o}ssbauer$ spectroscopy. The crystal structures in the range of x=0.05, 0.1, 0.2 are cubic at room temperature. Magnetoresistance measurement indicates that these system is semiconducting below about 160 K. The temperature of maximum magnetoresistance is almost consistent with Curie temperature. The Zn substitutions for Fe occur to increase the Jahn-Teller relaxation and the electric quadrupole shift. CMR properties could be explained with Jahn-Teller effect, and half-metallic electronic structure, which is different from both the double exchange interactions of manganite La-Ca-Mn-O system and the triple exchange interactions of chalcogenide $Cu_xFe_{1-x}Cr_2S_4$.

• Journal of the Korean Magnetics Society
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• v.10 no.2
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• pp.74-80
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• 2000

CoCr$_{x}$ Fe$_{2-x}$O$_4$(0.0$\leq$x$\leq$1.0) ferrites have been fabricated by sol-gel method. The crystallographic and magnetic properties of the samples were investigated by means of x-ray diffraction, scanning electron microscophy, Mossbauer spectroscopy and vibrating sample magnetometry. The structure of all the samples is cubic spinel type and the lattice constant decrease with increasing Cr content. The substituted Cr ions were located only in the B-site. The particle size also decreases with increasing Cr content. The Mossbauer spectra consist of two sextets due to Fe$^{3+}$ions at A- and B sites for 0.0$\leq$x$\leq$0.6, while, a paramagnetic doublet appears for 0.8$\leq$x$\leq$1.0. The magnetic hyperfine field decreases with increasing Cr content. The relaxation spectra was shown at 0.8$\leq$x$\leq$1.0 in CoCr$_{x}$ Fe$_{2-x}$O$_4$. The coercivity decreases drastically, while, the saturation magnetization decreases linearly with increasing x.ing x.

• Journal of the Korean Magnetics Society
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• v.16 no.1
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• pp.18-22
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• 2006

Effects of V substitution of Fe on the magnetic properties of $Fe_3O_4$ have been investigated by x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), conversion electron Mossbauer spectroscopy (CEMS), and vibrating sample magnetometry (VSM) measurements on sol-gel-grown films. XRD data indicates that the $V_xFe_{3-x}O_4$ films maintain cubic structure up to x=1.0 with little change of the lattice constant. Analyses on V 2p and Fe 2p levels of the XPS data indicate that V exist as $V^{3+}$ mostly in the $V_xFe_{3-x}O_4$ films with the density of $V^{2+}$ ions increasing with increasing V content. Analyses on the CEMS data indicate that $V^{3+}$ ions substitute tetrahedral $Fe^{3+}$ sites mostly, while $V^{2+}$ ions octahedral $Fe^{2+}$ sites. Results of room-temperature VSM measurements on the films reveal that the saturation magnetization for the x=0.14 sample is larger than that of $Fe_3O_4$, while it becomes smaller than that of $Fe_3O_4$ for $x{\geq}0.5$. The coercivity of the $V_xFe_{3-x}O_4$ films is found to increase with x, attributed to the increase of anisotropy by the substitution of $V^{2+}(d^3)$ ions into the octahedral sites.

• Journal of the Korean Magnetics Society
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• v.24 no.2
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• pp.51-55
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• 2014

The $Fe_3O_4$ nanoparticle was synthesized by the hot-injection method while varying the injection time of the precursor solution. The crystal structure was determined to be cubic inverse spinel with space group of Fd-3m based on X-ray diffraction (XRD) measurements and the morphology of the prepared $Fe_3O_4$ nanoparticle was studied with a high-resolution transmission electron microscope (HR-TEM). When the precursor solution was injected for 0.5 min, the size of the $Fe_3O_4$ nanoparticle was 7.63 nm, while the size of the obtained particle was 21.27 nm with the injection time of 60 min. The magnetic properties of the prepared $Fe_3O_4$ nanoparticle were investigated by both vibrating sample magnetometer (VSM) and $^{57}Co$ M$\ddot{o}$ssbauer spectroscopy at various temperatures. From the hyperthermia measurement, we observed that the temperature of the $Fe_3O_4$ nanoparticle powder reached around $120^{\circ}C$ under 250 Oe at 50 kHz, when the injection time of the precursor solution was 60 min.