• Bulletin of the Korean Chemical Society
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• v.23 no.12
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• pp.1769-1772
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• 2002

Previous $^{19}F\;and\;^{1,2}H$ electron-nuclear double resonance (ENDOR) study of fluorometmyoglobin (MbF) in frozen-solution state provided sensitive tools sensing subtle structural changes of the heme that are not obtainable from X-ray. [Fann et al., J. Am. Chem. Soc. 1995, 117, 6019] Because of the intrinsic inhomogeneouse EPR line broadening effect of MbF in frozen-solution state, detection of the intrinsic inhomogeneouse EPR line broadening effect of MbF in frozen-solution state, detection of the electronic and geometrical changes of the heme ring itself and the proximal histidine by using $^{14}N$ CW ENDOR was interfered. In the present study, hyperfine-sensitive $^{14}N$ Mims ENDOR technique of pulsed-EPR was employed to probe the changes. With two different $\tau$ values of 128 and 196 ns, $^{14}N$ ENDOR signals of the heme and proximal histidine were completely resolved at $g'_{II}(=g_e=2)$. This study present that X-band $^{14}N$ Mims ENDOR sequence can sensitively detect the small changes of the spin densities and p orbital populations of the proximal and the heme nitrogens, caused by ligand and pH variation of the distal site.

• Journal of the Korean Magnetics Society
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• v.15 no.2
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• pp.142-147
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• 2005

The embrittlement of fast neutron-irradiated reactor pressure vessel (RPV) steels was investigated by X-ray diffraction patterns at room temperature and $M\ddot{o}ssbauer$ spectroscopy at room- and liquid nitrogen-temperature. Neutron fluence on the samples were $10^{12},\;10^{13},\;10^{14},\;10^{15},\;10^{16},\;10^{17},\;10^{18}\;n/cm^2$. The X-ray diffraction patterns showed that the structure of the neutron unirradiated sample was bcc type, where as but the neutron irradiated samples with the fluence higher than $10^{17}\;n/{\cal}cm^2$ were so severely damaged, that bcc type structure disappeared. The $M\ddot{o}ssbauer$ spectra of all samples showed superposition of two or more sextets. In this paper all $M\ddot{o}ssbauer$ spectra were fitted by three set of sextet. The isomer shift and quadrupole splitting values were found around zero. At liquid nitrogen temperature, magnetic hyperfine field and absorption area increase rapidly S 1 sextet in the samples of $10^{17}\~10^{18}\;n/{\cal}cm^2$ neutron fluences. And at room temperature, magnetic hyperfine field and absorption increased rapidly at SI sextet in the samples of $10^{17}\~10^{18}\;n/{\cal}cm^2$ neutron fluences. This rapid increase of magnetic hyperfine field and absorption area were inferred to be caused by the change of $^{56}Fe,\;^{55}Mn$ into $^{57}Fe$ due to by neutron irradiation.

• Journal of the Korean Magnetics Society
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• v.12 no.1
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• pp.14-19
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• 2002

The iron-doped perovskite La$_{0.67}$Sr$_{0.33}$Mn$_{0.99}$$^{57}$Fe$_{0.01}$O$_3$compound has been studied by x-ray diffraction, Mossbauer spectroscopy, and vibrating sample magnetometry. The single phase of the polycrystalline La$_{0.67}$Sr$_{0.33}$Mn$_{0.99}$$^{57}$Fe$_{0.01}$O$_3$powder has been prepared by a waterbased solgel method. Crystalline La$_{0.67}$Sr$_{0.33}$Mn$_{0.99}$$^{57}$Fe$_{0.01}$O$_3$was a rombohedral structure with lattice parameters a$_{0}$=5.480 $AA$, $alpha$=60.259$^{circ}$. Mossbauer spectra of La$_{0.67}$Sr$_{0.3}$/Mn$_{0.99}$$^{57}$Fe$_{0.01}$O$_3$have been taken at various temperatures ranging from 20 to 400 K. As the temperature increases toward the Curie temperature, T$_{c}$=375 K, the Mossbauer spectra show line broadening and the difference between the 1,6 and 3,4 linewidths is caused by the anisotropic hyperfine field fluctuation. The anisotropic field fluctuation of +H (P$_{+}$=0.80) is greater than -H (P$_{-}$=0.20). We calculated that the anisotropy energy was 124.01 erg/cm$^3$for T=150 K which is associated with the large line broadening.

• Journal of the Korean Magnetics Society
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• v.7 no.2
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• pp.90-96
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• 1997

We have studied crystallographic and magnetic properties of $NdFe_{10.7}Ti_ {1.2}Mo_{0.1}$ by Mossbauer spectroscopy, X-ray diffraction and vibrating sample magnetometer (VSM). The alloys were prepared by arc-melting under an argon atmosphere. The $NdFe_{10.7}Ti_{1.2}Mo_{0.1}$ has pure a single phase, whereas $NdFe_{10.7}Ti_{1.3}$ contains some $\alpha$-Fe, conformed with X-ray diffractometry and Mossbauer measurements. The $NdFe_{10.7}Ti_ {1.2}Mo_{0.1}$ has a $ThMn_{12}-type$ tetragonal structure with $a_0=8.637{\AA}$ and $c_0=4.807{\AA}$. The Curie temperature ($T_c$) is 600 K from the result of Mossbauer measurement performed at various temperatures ranging from 13 to 800 K. Each spectrum of below $T_c$ is fitted with five subspectra of Fe sites in the structure ($8i_1, 8i_2, 8j_2, 8j_1, 8f$). The area fractions of the subspectra at room temperature are 12.3%, 14.0%, 21.0% 11.8%, 40.9%, respectively. Magnetic hyperfine fields for the Fe sites decrease in the order, $H_{hf}(8i)>H_{hf}(8j)>H_{hf}(8f)$. The abrupt changes in the magnetic hyperfine field, an magnetic moment observed at about 160 K in $NdFe_ {10.7} Ti_{1.2}Mo_{0.1}$ are attributed to spin reorientations. The average hyperfine field of the $NdFe_{10.7}Ti_{1.2}Mo_{0.1}$ shows a temperature dependence of $[H_{hf}(T)-H_{hf}(0)]/H_{hf}(0)=-0.34(T/T_C)^{3/2}-0.14(T/T_C)^{5/2}$ for $T/T_c<0.7$, indicative of spin wave excitation. The Debye temperatures of $NdFe_{10.7}Ti_{1.2}Mo_{0.1}$ is found to be Θ=340$\pm$5 K.