• Journal of the Korean Chemical Society
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• v.61 no.1
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• pp.29-33
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• 2017

Formation of Au particles in nonstoichiometric $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxide from aniline + hydrochloric acid mixtures and chloroauric acid in the ratios 30 : 1; 60 : 1; 90 : 1 (S1-S3) by volume and 0.01 mol of copper acetate, $Cu(OCOCH_3)_2.H_2O$, in each case is performed by sol-gel growth. Powder x-ray diffraction (XRD) results show Au particles are dispersed in tetragonal nonstoichiometric dicopper (I) dicopper (II) oxides, $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$). Average crystallite sizes of Au particles determined using Scherrer equation are found to be in the approximate ranges ${\sim}85-140{\AA}$, ${\sim}85-150{\AA}$ and ${\sim}80-150{\AA}$ in S1-S3, respectively which indicate the formation of Au nano-micro size particles in $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxides. Hysteresis behaviour at 300 K having low loop areas and magnetic susceptibility values ${\sim}5.835{\times}10^{-6}-9.889{\times}10^{-6}emu/gG$ in S1-S3 show weakly ferromagnetic nature of the samples. Broad and isotropic electron paramagnetic resonance (EPR) lineshapes of S1-S4 at 300, 77 and 8 K having $g_{iso}$-values ${\sim}2.053{\pm}0.008-2.304{\pm}0.008$ show rapid spin-lattice relaxation process in magnetic $Cu^{2+}$ ($3d^9$) sites as well as delocalized electrons in Au ($6s^1$) nano-micro size particles in the $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxides. Broad and weak UV-Vis diffuse reflectance optical absorption band ~725 nm is assigned to $^2B_{1g}{\rightarrow}^2A_{1g}$ transitions, and the weak band ~470 nm is due to $^2B_{1g}{\rightarrow}^2E_g$ transitions from the ground state $^2B_{1g}$(${\mid}d_{x^2-y^2}$>) of $Cu^{2+}$ ($3d^9$) ions in octahedral coordination having tetragonal distortion.

• Journal of the Korean Chemical Society
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• v.56 no.1
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• pp.62-67
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• 2012

A series of homo binuclear complexs of the type $[M_2(L/L^')(NO_3)n].mH_2O$, [where $M=U{O_2}^{2+},\;Th^{4+},\;ZrO^{2+}$] and $[(VO)_2(L/L^')(SO_4)_2]{\cdot}2H_2O$, L=1,5,6,9,12,15,16,20 octaaza-7,813,14-tetraphenyl-2,4,17,19-tetramethyl-1,4,6,8,12,14,16,19-docosaoctene (OTTDO) or L'=10:11;21:22-dibenzo-1,5,6,9,12,15,16,20-octaaza-7,813,14-tetraphenyl-2,4,17,19-tetramethyl-1,4,6,8,12,14,16,19-docosaoctene (DOTTOT), n=4 for $U{O_2}^{2+}$, $ZrO^{2+}$ n=8 for $Th^{4+}$ m=1,2,3 respectively, have been synthesized in template method from ethylenediamine/orthophenylene diamine, benzil monohydrazone and acetyl acetone and characterized on the basis of elemental analysis, thermal analysis, molar conductivity, magnetic moment, electronic, infrared, $^1H$-NMR studies. The results indicate that the VO(IV) ion is penta co-ordinated yielding paramagnetic complexes; $UO_2(VI)$, ZrO(IV) ions are hexa co-ordinated where as Th(IV) ion is octa co-ordinated yielding diamagnetic complexes of above composition. The fungi toxicity of the ZrO(IV) and VO(IV) complexes against some fungal pathogen has been studied.

• Journal of the Korean Magnetics Society
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• v.10 no.2
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• pp.81-85
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• 2000

Crystallographic and magnetic properties of the Mn-doped orthoferrite LaFe$_{1-x}$Mn$_{x}$ O$_3$(0.0$\leq$x$\leq$O.4) system have been investigated by means of x-ray diffractometry, M ssbauer spectroscopy, vibrating sample magnetometer and super-conducting quantum interference device. The structure of the system was found to be orthorhombic distorted perovskite structure. At room temperature, the M ssbauer spectra for x=0.0 consists of one Zeeman sextets from Fe$^{3+}$ ions at octahedral sites. The M ssbauer spectra of two Zeeman sextets (x$\leq$0.1) change one Zeeman sextets and a paramagnetic doublet (x=0.4). The saturation magnetization increases but the coercivity decreases with increasing x in LaFe$_{1-x}$Mn$_{x}$ O$_3$.

• Korean Chemical Engineering Research
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• v.44 no.4
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• pp.369-374
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• 2006

A solid-state reaction of $V_2O_5$ with AlMCM-48 followed by calcination generated very weak paramagnetic $VO^{2+}$ species in the mesoporous material. Dehydration and subsequent reduction with CO result in the formation of vanadyl $VO^{2+}$ species that can be characterized by EPR. The chemical environment of vanadium centers in $VO^{2+}-AlMCM-48$ was investigated by XRD, EDX, DR-UV-Vis, EPR,$^{29}Si$ and $^{27}Al$ and $^{51}V$ NMR. Vanadium species in MCM-48 are existed as pseudotetrahedral $VO^{2+}$ state when they were dehydrated or reduced with CO. The coordination of water on vanadyl ions transformed their structure to distorted octahedral.

• Journal of the Korean Magnetics Society
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• v.15 no.2
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• pp.106-108
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• 2005

The rutile polycrystal $Ti_{0.99}\;^{57}Fe_{0.01}O_2$ prepared with $^{57}Fe$ enriched iron have been studied by $M\ddot{o}ssbauer$ spectroscopy, X-ray diffraction and VSM. The $M\ddot{o}ssbauer$ spectrum of $Ti_{0.99}\;^{57}Fe_{0.01}O_2$ consists of a ferromagnetic and a paramagnetic phase over all temperature ranging from 4 to 300 K. Isomer shifts indicate $Fe^{2+}$ for the ferromagnetic phase, but $Fe^{3+}$ for the paramagneic phase of $Ti_{0.99}\;^{57}Fe_{0.01}O_2$ sample. It is noted that the magnetic hyperfine field of ferromagnetic phase had the value about 1.48 times as large as that of $\alpha$-Fe. The XRD data for $Ti_{0.99}\;^{57}Fe_{0.01}O_2$ showed a pure rutile phase with tetragonal structures without any segregation of Fe into particulates within the instrumental resolution limit The magnetic hysteresis (M-H) curve at room temperature showed an obvious ferromagnetic behavior and the magnetic moment per Fe atom under the applied field of 1 T was estimated to be about $0.71{\mu}_B$, suggesting a low spin configuration of Fe ions.

• Journal of the Korean Magnetics Society
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• v.20 no.6
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• pp.216-221
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• 2010

Magnetic nanocomposites contained iron oxide were synthesized by through cross-linking polymerization of dimethylacetamide (DMAc) solution and toluen solution on the amphiphilic polymer networks based on urethan acrylate nonionomer (UAN) precursor chains. For the study on microscopic structures and magnetic properties of the magnetic nanoparticles, FESEM and XRD and Mossbauer spectroscopy were used. The results investigated show that there are magnetic nanoparticles of $Fe_2O_3$ in samples and the magnetic nanocomposites contained iron oxide in polymer networks of UAN using DMAc solution are more smaller than using toluen solution. All of the Fe ions in the samples present $Fe^{3+}$ and the magnetic property of samples are paramagnetic by superparamagnetic effect at room temperature.

• Journal of the Korean Magnetics Society
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• v.16 no.1
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• pp.11-13
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• 2006

[ $M\"{o}ssbauer$ ] spectra of $Ti_{1-x-y}Co_xFe_yO_2(0.01{\leq}x,\;y{\leq}0.05)$ prepared with $^{57}Fe$ enriched iron have been taken at various temperatures ranging from 80 to 300K. The Mossbauer spectrum of $Ti0.94Co_{0.03}Fe_{0.03}O_2$ consists of a ferromagnetic (six-Lorentzian), a paramagnetic phase (doublet) and armorphous phase over all temperature ranges. Isomer shifts indicate $Fe^{3+}$ for the ferromagnetic phase and the paramagneic phase of $Ti_{1-x-y}Co_xFe_yO_2$ samples. It is noted that the magnetic hyperfine field of ferromagnetic phase had the value about 1.5 times as large as that of u-fe. The XRB data for $Ti_{1-x-y}Co_xFe_yO_2$ showed mainly rutile phase with tetragonal structures without any segregation of Co and Fe into particulates within the instrumental resolution limit. The magnetic moment per (Co+Fe) atom in $Ti0.94Co_{0.03}Fe_{0.03}O_2$, under the applied field of 1T was estimated to be about $0.332{\mu}_B$ which is ten times as large as that of $Ti0.97Co_{0.03}Fe_{0.03}O_2,\;0.024{\mu}_B$ per Co atom, suggesting a high spin configuration of Co and fe ions.

• Journal of Magnetics
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• v.10 no.1
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• pp.5-9
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• 2005

Nanoparticles $Ni_{0.9}Zn_{0.1}Fe_2O_4$ is fabricated by a sol-gel method. The magnetic and structural properties of powders were investigated with XRD, SEM, Mossbauer spectroscopy, and VSM. $Ni_{0.9}Zn_{0.1}Fe_2O_4$ powders annealed at $300{^{\circ}C}$ have a spinel structure and behaved superparamagnetically. The estimated size of $Ni_{0.9}Zn_{0.1}Fe_2O_4$ nanoparticle is about 10 nm. The hyperfine fields at 13 K for the A and B patterns are found to be 533 and 507 kOe, respectively. The ZFC curves are rounded at the blocking temperature ($T_B$)and show a paramagnetic-like behavior above $T_B$. $T_B$ of $Ni_{0.9}Zn_{0.1}Fe_2O_4$ nanoparticle is about 250 K. Nanoparticles $Ni_{0.9}Zn_{0.1}Fe_2O_4$ annealed at 400 and $500{^{\circ}C}$ have a typical spinel structure and is ferrimagnetic in nature. The isomer shifts indicate that the iron ions were ferric at the tetrahedral (A) and the octahedral (B). The saturation magnetization of nanoparticles $Ni_{0.9}Zn_{0.1}Fe_2O_4$ annealed at 400 and $500{^{\circ}C}$ are 40 and 43 emu/g, respectively. The magnetic anisotropy constant of $Ni_{0.9}Zn_{0.1}Fe_2O_4$ annealed at $300{^{\circ}C}$ were calculated to be 1.6 ${\times}$ $10^6$ ergs/$cm^3$.

• Journal of Magnetics
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• v.18 no.1
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• pp.21-25
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• 2013

Nickel substituted manganese ferrites, $Mn_{1-x}Ni_xFe_2O_4$ ($0.0{\leq}x{\leq}0.6$), were fabricated by sol-gel method. The effects of sintering and substitution on their crystallographic and magnetic properties were studied. X-ray diffractometry of $Mn_{0.6}Ni_{0.4}Fe_2O_4$ ferrite sintered above 523 K indicated a spinel structure; particles increased in size with hotter sintering. The M$\ddot{o}$ssbauer spectrum of this ferrite sintered at 523 K could be fitted as a single quadrupole doublet, indicative of a superparamagnetic phase. Sintering at 573 K led to spectrum fitted as the superposition of two Zeeman sextets and a single quadrupole doublet, indicating both ferrimagnetic and paramagnetic phase. Sintering at 673 K and at 773 K led to spectra fitted as two Zeeman sextets due to a ferrimagnetic phase. The saturation magnetization and the coercivity of $Mn_{0.6}Ni_{0.4}Fe_2O_4$ ferrite sintered at 773 K were 53.05 emu/g and 142.08 Oe. In $Mn_{1-x}Ni_xFe_2O_4$ ($0.0{\leq}x{\leq}0.6$) ferrites, sintering of any composition at 773 K led to a single spinel structure. Increased Ni substitution decreased the ferrites' lattice constants and increased their particle sizes. The M$\ddot{o}$ssbauer spectra could be fitted as the superposition of two Zeeman sextets due to the tetrahedral and the octahedral sites of the $Fe^{3+}$ ions. The variations of saturation magnetization and coercivity with changing Ni content could be explained using the changes of particle size.

• Journal of Magnetics
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• v.21 no.3
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• pp.308-314
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• 2016

Cobalt-, zinc-, and nickel-zinc-substituted nano-size manganese ferrite powders, $MnFe_2O_4$, $Mn_{0.8}Co_{0.2}Fe_2O_4$, $Mn_{0.8}Zn_{0.2}Fe_2O_4$ and $Mn_{0.8}Ni_{0.1}Zn_{0.1}Fe_2O_4$, were fabricated using a sol-gel method, and their crystallographic and magnetic properties were subsequently studied. The $MnFe_2O_4$ ferrite powder annealed at temperatures above 523 K exhibited a spinel structure, and the particle size increased as the annealing temperature increased. All ferrites annealed at 773 K showed a single spinel structure, and the lattice constants and particle size decreased with the substitution of Co, Zn, and Ni-Zn. The $M{\ddot{o}}ssbauer$ spectrum of the $MnFe_2O_4$ ferrite powder annealed at 523 K only showed a doublet due to its superparamagnetic phase, and the $M{\ddot{o}}ssbauer$ spectra of the $MnFe_2O_4$, $Mn_{0.8}Co_{0.2}Fe_2O_4$, and $Mn_{0.8}Zn_{0.2}Fe_2O_4$ ferrite powders annealed at 773 K could be fitted as the superposition of two Zeeman sextets due to the tetrahedral and octahedral sites of the $Fe^{3+}$ ions. However, the $M{\ddot{o}}ssbauer$ spectrum of the $Mn_{0.8}Ni_{0.1}Zn_{0.1}Fe_2O_4$ ferrite powder annealed at 773 K consisted of two Zeeman sextets and one quadrupole doublet due to its ferrimagnetic and paramagnetic behavior. The area ratio of the $M{\ddot{o}}ssbauer$ spectra could be used to determine the cation distribution equation, and we also explained the variation in the $M{\ddot{o}}ssbauer$ parameters by using this cation distribution equation, the superexchange interaction and the particle size. Relative to pure $MnFe_2O_4$, the saturation magnetizations and coercivities were larger in $Mn_{0.8}Co_{0.2}Fe_2O_4$ and smaller in $Mn_{0.8}Zn_{0.2}Fe_2O_4$, and $Mn_{0.8}Ni_{0.1}Zn_{0.1}Fe_2O_4$. These variations could be explained using the site distribution equations, particle sizes and magnetic moments of the substituted ions.