Mössbauer spectroscopy, X-ray spectroscopy, SEM, EDX, heat capacity and SQUID measurement were carried out in conjunction with a catalytic study on mixed Fe-Mo oxides, some of which have been used in selective oxidation of certain hydrocarbons. With the specific activity being sensitive to the catalytic particle size and morphology, an aerogel process was employed to prepare seven samples covering Fe/Mo ratios from 1/2 to 2/1and some of the samples were annealed at 300oC and 500oC . Mössbauer data have been analyzed, with each set well fitted to reflect one Fe3+ and two or more non-equivalent Fe2+ sites. There isomer shift, quadruple splitting and molar fraction are analyzed in terms of temperature and Fe/Mo-ratio dependence. The Fe-rich samples exhibit magnetic ordering at low temperatures, revealing multiple sextets corresponding to different magnetic hyperfine fields. Two samples with the Fe:Mo ratio 1:1 and 2:3 were study in more detail their X-ray diffraction pattern reveal that they crystallize with the β-FeMoO4 structure. SEM gives unusual morphology and the material form into hallow sphere with 2um in diameter. EDS confirms that the metal ion is fairly uniformly distributed and close to the nominal values. Finally heat capacity and SQUID measurements confirm the antiferromagnetic phase transition near 13K for the heat treated samples. / "December 2006."

No description available.

No description available.

In this thesis the result x-ray diffraction, magnetic susceptibility, magnetization, and Mössbauer spectroscopy measurements of EuPdGe3, Al13Fe4, and FeNiSn are reported. The compound EuPdGe3 crystallizes in the BaNiSn3-type tetragonal structure (space group I4mm) with the lattice constants a = 4.4457(1) Å and c = 10.1703(2) Å. The results are consistent with EuPdGe3 being an antiferromagnet with the Néel temperature TN = 12.16(1) K and with the Eu spins S = 7/2 in the ab plane. The temperature dependence of the magnetic susceptibility above TN follows the modified Curie-Weiss law with the effective magnetic moment of 7.82(1) 𝜇𝐵 per Eu atom and the paramagnetic Curie temperature of −5.3(1) K indicative of dominant antiferromagnetic interactions. The M(H) isotherms for temperatures approaching TN from above are indicative of dynamical short-range antiferromagnetic ordering in the sample. The temperature dependence of the hyperfine magnetic field follows a S = 7/2 Brillouin function. The principal component of the electric field gradient tensor is shown to increase with decreasing temperature and is well described by a 𝑇32⁄ power-law relation. The Debye temperature of EuPdGe3 determined from the Mössbauer data is 199(2) K. The compound Al13Fe4 crystallizes in the monoclinic space group C2/m, in which Fe atoms are located at five inequivalent crystallographic sites, with the lattice parameters a = 15.503(2) Å, b = 8.063(2) Å, c = 12.464(2) Å, and β = 107.71(2)°. It is demonstrated that zero-field Mössbauer spectra can be decomposed into three quadrupole doublets. With the aid of the calculated electric field gradient (EFG) parameters we show that the first doublet results from one Fe site, the second doublet is due to two other Fe sites, and the third doublet originates from the last two Fe sites. We find that the shape of the Mössbauer spectrum of Al13Fe4 measured in an external magnetic field of 90 kOe can be accounted for with five component subspectra generated using the calculated II EFG parameters at five inequivalent Fe sites. The quadrupole splittings corresponding to three component doublets are shown to increase with decreasing temperature and are well described by a 𝑇32⁄ power-law relation. The Debye temperature of Al13Fe4 is found to be 383(3) K. We find a pseudogap in the density of states (DOS), with a width of ∼ 0.2 eV, that is centered 0.1 eV above the Fermi energy. The finite DOS at the Fermi energy confirms good metallicity of Al13Fe4. The 1/T-like dependence of the magnetic susceptibility shows that Al13Fe4 is a paramagnet. The compound FeNiSn crystallizes in the ZrBeSi-type crystal structure (space group P63/mmc) with the lattice constants a = 4.1329(1) Å and c = 5.1912(2) Å. It is a ferromagnet with the Curie temperature TC = 1024(10) K. Evidence is provided for a possible phase separation in the studied compound, into a majority magnetic phase and a minority, nanoscale, disordered phase with the corresponding iron magnetic moments at 4.6 K of 2.39(1) and 1.17(1) 𝜇𝐵. It is demonstrated that FeNiSn decomposes at a temperature significantly below TC when it is annealed in vacuum for about 30 hours. The Debye temperature of FeNiSn is found to be 445(6) K.

Este trabalho tem como objetivo a síntese da liga Fe IND.78-X Al IND.X Si IND.9 B IND.13, com o X=0, 10, 20, 30 e 50, através da moagem utilizando para isto um moinho de bolas de alta energia. As técnicas de difração de raios-X, microscopia eletrônica de varredura, SQUID, análise térmica diferencial (DTA) e espectroscopia Mössbauer são utilizadas na verificação da dependência da estrutura e propriedades magnéticas com o tempo de moagem e diferentes concentrações de Al. Com a moagem uma solução sólida com estrutura BCC é formada, com os átomos sendo distribuídos de forma aleatória na rede. O tamanho de grãos descresce rapidamente nos primeiros estágios de moagem e depois, com a continuação da moagem, permanece aproximadamente constante. Os espectros Mössbauer apresentam linhas alargadas, uma característica dos materiais submetidos a moagem, e forma ajustados considerando sítios paramagnéticos, sextetos cristalinos e distribuições Gaussianas de campos hiperfinos. As medidas magnéticas mostram que as ligas possuem propriedades de material magnético mole. A magnetização e a coercividade diminuem com o tempo de moagem, indicando um aumento no número de átomos não-magnéticos em torno do átomo de ferro e a diminuição do tamanho do grão, respectivamente. Com o aumento da concentração de Al, o tamanho do grão da solução sólida tende a diminuir e o sistema perde seu ordenamento magnético. As curvas DTA mostram uma transformação exotérmica associada à cristalização de fases amorfas e ao ordenamento da solução sólida Fe(Al, Si, B) para formar outros compostos. O tratamento térmico dos pós moídos forma os intermetálicos FeAl, FeAl IND.2. As amostras submetidas a tempos de moagem maiores dão origem a fases nanocristalinas e amorfas com alto grau de contaminação pelos componentes de moinho. / The purpose of the present work is the synthesis of Fe IND.78-xAl IND.xSi IND.9B IND.13 alloy, with x=0, 10, 20, 30 and 50, by mechanical alloying in a high energy planetary ball mil. The effect of the milling time and Al content on the structure and magnetic properties has been studied by X-ray diffraction, scanning electron microscopy, SQUID, differential analysis thermal (DTA) and Mossbauer spectroscopy. After milling a Fe-Al-Si-B solid solution with a bcc structure is formed. The atoms are assumed to be randomly distributed in lattice, the grain size decrease dramatically at the early milling stages with further milling to remain relatively stable at the late stages. The Mossbauer spectra show lines broad, a characteristic of milled materials, and were fitted by considering paramagnetic phases, crystalline sextet and Gaussian distributions of hyperfine fields. The magnetic measurements show soft magnetic properties. The magnetization and coactivity decrease with milling time, indicating an increasing number of nonmagnetic atoms around the iron atoms and decrease of grain size, respectively. With increasing Al content, the grain size of the solid solutions decreased, and the system loses its magnetic order. The DTA curves show the exothermic transformation associated to crystallization of amorphous phase and ordering of the Fe(Al,Si,B) solid solutions to form other compounds. The annealing of milled powders form the ordered FeAl and FeAl IND.2 intermetallic. Long milling times resulted in Nano crystalline and amorphous phases highly contaminated by the milling tools.

Thesis. 1976. Ph.D.--Massachusetts Institute of Technology. Dept. of Materials Science and Engineering. / Microfiche copy available in Archives and Science. / Vita. / Includes bibliographical references. / Ph.D.

No description available.

III-V compound semiconductors such as Gallium Arsenide, Indium Phosphide as well as Indium Arsenide have recently demonstrated the capability of applications in high speed semiconductor devices compared to those made from Silicon. As a result, III-V compound semiconductors have drawn attention of material researchers, in particular in understanding the effects that may occur during manufacturing of these devices. Optical and electrical properties of a device may alter when a foreign atom is introduced during the manufacturing of the device. However, the foreign atom may also lead to the formation of lattice disorder (defects). A convenient way of introducing impurity atoms into a substrate and tailoring their functionality for particular applications is by ion implantation. Mössbauer spectroscopy is a useful technique usually utilized for understanding site location of the impurity atoms in a lattice and the formation of defect complexes. The focus of this dissertation is the study of lattice location of ion implanted ⁵⁷Mn/⁵⁷Fe ions in the III-V semiconductors InP, n-type InAs and p type InAs, and the annealing of implantation induced lattice damage in these samples. ⁵⁷Fe Mössbauer spectroscopy studies have been conducted on III-V semiconductors InP, n-type InAs and p-type InAs with the 57Fe Mössbauer state being populated following the implantation of radioactive ⁵⁷Mn⁺ ions which has the advantage that extremely low fluence implantations are sufficient to give data with good statistics. The ⁵⁷Mn⁺ ions were accelerated to 60 keV at the ISOLDE/CERN facility and implanted with fluences of up to 2x10¹² ions/cm² into single crystal samples which were held at 300 –700 K in an implantation chamber. βdecay of the Mn⁺ imparts an average recoil energy of 40 keV to the daughter ⁵⁷*Fe which are then re-distributed onto interstitial and/or substitutional sites, or trapped in defect complexes and damage sites. The Mössbauer spectra were collected with a light-weight parallel plate avalanche counter, with ⁵⁷Fe enriched stainless steel electrodes, mounted on a conventional drive unit outside the implantation chamber. The spectra were analyzed with the Mössbauer fitting code VINDA which allowed for simultaneous fits of the set of spectra for each sample collected at different temperatures. Acceptable fits to the Mössbauer spectra of the InP, n-type InAs and p-type InAs samples required three components: an asymmetric doublet attributed to Fe atoms in implantation induced damaged environments, a single line assigned to Fe on substitutional In sites, and a weak symmetric doublet assigned to impurity-vacancy complexes. In InP there is already an appreciable substitutional Fe (Feѕ) fraction on implantation at room temperature; while in the InAs samples FeS only becomes significant above 400 K. In all samples, the asymmetric doublet dominates the spectra below 400 K. Implantation damage, however, anneals quite rapidly and at high temperatures (above 400 K), the single line due to Feѕ dominates the spectra while the Fe-defect complex dissociates at 500 K. The implantation induced damage is observed to anneal fast in the arsenide samples compared to the phosphide sample. The slow annealing of the damage in InP was supported by the higher Debye temperature (290 K) extracted from the temperature dependence of the site population for the damage site in InP compared with InAs (194 K and 200 K for n-type and p-type, respectively). Variations in the isomer shift and quadrupole splitting for the damage site in InP at high temperatures (above 400 K) suggest structural changes in the neighborhood of the ⁵⁷Fe probe. Furthermore, the isomer shifts of the spectral components were consistent with near trivalent state and fully trivalent state i.e., Fe³⁺ with d⁵ electron configuration for Fe ions in the damage site and at the substitutional (In) site, respectively. The impurity Fe atoms associated with vacancies are identified to be in the Fe²⁺ state with a d⁶ electron configuration. ________________________________________________________________ / Thesis (M.Sc.)-University of KwaZulu-Natal, Westville, 2011.

Este trabalho tem como objetivo a síntese da liga Fe IND.78-X Al IND.X Si IND.9 B IND.13, com o X=0, 10, 20, 30 e 50, através da moagem utilizando para isto um moinho de bolas de alta energia. As técnicas de difração de raios-X, microscopia eletrônica de varredura, SQUID, análise térmica diferencial (DTA) e espectroscopia Mössbauer são utilizadas na verificação da dependência da estrutura e propriedades magnéticas com o tempo de moagem e diferentes concentrações de Al. Com a moagem uma solução sólida com estrutura BCC é formada, com os átomos sendo distribuídos de forma aleatória na rede. O tamanho de grãos descresce rapidamente nos primeiros estágios de moagem e depois, com a continuação da moagem, permanece aproximadamente constante. Os espectros Mössbauer apresentam linhas alargadas, uma característica dos materiais submetidos a moagem, e forma ajustados considerando sítios paramagnéticos, sextetos cristalinos e distribuições Gaussianas de campos hiperfinos. As medidas magnéticas mostram que as ligas possuem propriedades de material magnético mole. A magnetização e a coercividade diminuem com o tempo de moagem, indicando um aumento no número de átomos não-magnéticos em torno do átomo de ferro e a diminuição do tamanho do grão, respectivamente. Com o aumento da concentração de Al, o tamanho do grão da solução sólida tende a diminuir e o sistema perde seu ordenamento magnético. As curvas DTA mostram uma transformação exotérmica associada à cristalização de fases amorfas e ao ordenamento da solução sólida Fe(Al, Si, B) para formar outros compostos. O tratamento térmico dos pós moídos forma os intermetálicos FeAl, FeAl IND.2. As amostras submetidas a tempos de moagem maiores dão origem a fases nanocristalinas e amorfas com alto grau de contaminação pelos componentes de moinho. / The purpose of the present work is the synthesis of Fe IND.78-xAl IND.xSi IND.9B IND.13 alloy, with x=0, 10, 20, 30 and 50, by mechanical alloying in a high energy planetary ball mil. The effect of the milling time and Al content on the structure and magnetic properties has been studied by X-ray diffraction, scanning electron microscopy, SQUID, differential analysis thermal (DTA) and Mossbauer spectroscopy. After milling a Fe-Al-Si-B solid solution with a bcc structure is formed. The atoms are assumed to be randomly distributed in lattice, the grain size decrease dramatically at the early milling stages with further milling to remain relatively stable at the late stages. The Mossbauer spectra show lines broad, a characteristic of milled materials, and were fitted by considering paramagnetic phases, crystalline sextet and Gaussian distributions of hyperfine fields. The magnetic measurements show soft magnetic properties. The magnetization and coactivity decrease with milling time, indicating an increasing number of nonmagnetic atoms around the iron atoms and decrease of grain size, respectively. With increasing Al content, the grain size of the solid solutions decreased, and the system loses its magnetic order. The DTA curves show the exothermic transformation associated to crystallization of amorphous phase and ordering of the Fe(Al,Si,B) solid solutions to form other compounds. The annealing of milled powders form the ordered FeAl and FeAl IND.2 intermetallic. Long milling times resulted in Nano crystalline and amorphous phases highly contaminated by the milling tools.

No description available.