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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

Elektrochemische Fe-Ga-Legierungsabscheidung zur Herstellung von Nanostrukturen

Pohl, Diana 09 September 2015 (has links) (PDF)
Eisen-Gallium-Legierungen sind aufgrund ihrer hohen Magnetostriktion und ihrer hervorragenden mechanischen Eigenschaften sehr interessant für Anwendungen sowohl in Form von Sensoren als auch Aktoren. Die fortschreitende Miniaturisierung erfordert die Herstellung von Bauteilen in eindimensionaler Struktur und komplexen Geometrien. Beide Herausforderungen sind mit templatbasierter elektrochemischer Abscheidung zugänglich. Es konnte gezeigt werden, dass dünne Fe-Ga-Schichten schon aus einfachen wässrigen Elektrolyten abgeschieden werden können. Gallium kann nur in Anwesenheit von Fe induziert reduziert werden. Gleichzeitig konnte nachgewiesen werden, dass durch die Hydrolyseneigung der Ga-Ionen immer Hydroxide gebildet und in das Deposit eingebunden werden. Durch die Einführung einer alternierenden potentiostatischen Abscheidung mit einem Reduktions- und einem Relaxationsschritt können dennoch dichte und homogene Fe80Ga20-Schichten mit wenigen Defekten und einem vernachlässigbar kleinen Sauerstoffgehalt hergestellt werden. Die Übertragung der so gefundenen Abscheideparameter zur templatbasierten Nanodrahtherstellung ist nur bis zu einem Porendurchmesser von 100nm möglich. Wird der Durchmesser der Porenkanäle weiter verringert, führt aufgrund eingeschränkter Diffusionsvorgänge die Abscheidung zu segmentierten und sauerstoffreichen Depositen. Die Modifizierung des Elektrolyten durch Komplexierung der Metallionen verhindert die Bildung und Einbindung der Hydroxide. Damit können auch für Porendurchmesser kleiner 100nm Drähte in AAO-Template abgeschieden werden. Diese sind dicht, defektfrei und weisen keinen Zusammensetzungsgradienten entlang der Wachstumsrichtung auf. Detaillierte TEM-Untersuchungen konnten zeigen, dass die Herstellung durch ein einfacheres potentiostatisches Abscheideregime zu weniger verspannten und dennoch homogenen und defektfreien Drähten führt. Für die Herstellung von magnetisch aktiven Drähten sollte daher die potentiostatische der gepulsten Abscheidung vorgezogen werden.
2

Elektrochemische Fe-Ga-Legierungsabscheidung zur Herstellung von Nanostrukturen

Pohl, Diana 19 August 2015 (has links)
Eisen-Gallium-Legierungen sind aufgrund ihrer hohen Magnetostriktion und ihrer hervorragenden mechanischen Eigenschaften sehr interessant für Anwendungen sowohl in Form von Sensoren als auch Aktoren. Die fortschreitende Miniaturisierung erfordert die Herstellung von Bauteilen in eindimensionaler Struktur und komplexen Geometrien. Beide Herausforderungen sind mit templatbasierter elektrochemischer Abscheidung zugänglich. Es konnte gezeigt werden, dass dünne Fe-Ga-Schichten schon aus einfachen wässrigen Elektrolyten abgeschieden werden können. Gallium kann nur in Anwesenheit von Fe induziert reduziert werden. Gleichzeitig konnte nachgewiesen werden, dass durch die Hydrolyseneigung der Ga-Ionen immer Hydroxide gebildet und in das Deposit eingebunden werden. Durch die Einführung einer alternierenden potentiostatischen Abscheidung mit einem Reduktions- und einem Relaxationsschritt können dennoch dichte und homogene Fe80Ga20-Schichten mit wenigen Defekten und einem vernachlässigbar kleinen Sauerstoffgehalt hergestellt werden. Die Übertragung der so gefundenen Abscheideparameter zur templatbasierten Nanodrahtherstellung ist nur bis zu einem Porendurchmesser von 100nm möglich. Wird der Durchmesser der Porenkanäle weiter verringert, führt aufgrund eingeschränkter Diffusionsvorgänge die Abscheidung zu segmentierten und sauerstoffreichen Depositen. Die Modifizierung des Elektrolyten durch Komplexierung der Metallionen verhindert die Bildung und Einbindung der Hydroxide. Damit können auch für Porendurchmesser kleiner 100nm Drähte in AAO-Template abgeschieden werden. Diese sind dicht, defektfrei und weisen keinen Zusammensetzungsgradienten entlang der Wachstumsrichtung auf. Detaillierte TEM-Untersuchungen konnten zeigen, dass die Herstellung durch ein einfacheres potentiostatisches Abscheideregime zu weniger verspannten und dennoch homogenen und defektfreien Drähten führt. Für die Herstellung von magnetisch aktiven Drähten sollte daher die potentiostatische der gepulsten Abscheidung vorgezogen werden.
3

Avaliação da magnetostricção em ligas Fe1-xMx (M = V, Sn) e caracterização de suas propriedades magnéticas e microestruturais / Evaluation of magnetostriction and microstructural characterization of Fe-Sn and Fe-V alloys

Claudio Teodoro dos Santos 25 January 2008 (has links)
Materiais magnetostrictivos exibem deformação elástica na presença de um campo magnético aplicado e por isso são de grande interesse para aplicação em sensores e atuadores. Trabalhos publicados no ano 2000 mostraram que a adição de Ga e Al ao Fe resulta em ligas com elevada magnetostricção em campos baixos. A partir daí os esforços foram direcionados para a descoberta de novas ligas magnetostrictivas à base de Fe com propriedades similares às encontradas nas ligas Fe-Ga e Fe-Al. No presente trabalho foram adicionados o Sn e o V ao Fe com o objetivo de avaliar a magnetostricção e a microestrutura das ligas formadas. Para isso, foram produzidas por fusão a arco as ligas Fe-9%at.Sn, Fe-20%at.Sn e as ligas Fex% at.V para x = 20, 25 e 30. As ligas Fe-Sn foram submetidas a tratamentos térmicos em 550 e 750°C por 24 h e em 880°C por 6 h e depois resfriadas rapidamente para a retenção das fases (Fe?,Sn), FeSn, Fe3Sn2 e Fe5Sn3. Já as ligas Fe-V foram tratadas em 1100°C por 6 h para homogeneização da fase única (Fe?,V). A caracterização microestrutural e análise quantitativa das fases foram feitas por microscopia óptica e eletrônica de varredura, microanálise por energia dispersiva (EDS) e difratometria de raios X. Também foi medida a microdureza Vickers das amostras. A magnetostricção foi medida por dilatometria de capacitância usando um dilatômetro de placa inclinada inserido no equipamento Maglab da Oxford Instruments, em campos na faixa de -1,5 a 1,5 T e temperaturas próximas de 203 K. A magnetização de saturação das amostras foi obtida em 77, 203 e 300 K utilizando o PPMS 6000 da Quantum Design. A magnetostricção de saturação (?S) das amostras da liga Fe-9Sn foi negativa e o comportamento das curvas similar ao do Fe puro. As amostras da liga Fe- 20Sn apresentaram ?S positiva devido à presença das fases ferromagnéticas Fe3Sn2 e Fe5Sn3. A ?S das ligas Fe-V foi positiva e maior em módulo do que a das ligas Fe-Sn. Concluiu-se que a substituição do Fe por Sn e V de modo geral melhorou a magnetostricção do Fe, porém a melhora não foi tão relevante quanto a observada pela substituição por Ga. / Magnetostrictive materials exhibit elastic strain in the presence of an applied magnetic field and therefore are of great interest for use in sensors and actuators. Works published in 2000 showed that the addition of Ga and Al in Fe results in alloys with high magnetostriction at low fields. Since then efforts have been directed to the discovery of new magnetostrictive Fe based alloys with similar properties to those found in Fe-Ga and Fe-Al alloys. In the present work Sn and V were added to Fe with the purpose of evaluating the magnetostriction and microstructure of these alloys. Therefore, Fe-9at.%Sn, Fe-20at.%Sn alloys and Fexat.% V alloys for x = 20, 25 and 30 were produced by arc melting. The Fe-Sn alloys were heat-treated at the temperatures of 550 and 750°C for 24 h and 880°C for 6 h and then rapidly cooled to the retention of the (?Fe,Sn), FeSn, Fe3Sn2 and Fe5Sn3 phases. Fe-V alloys were heat-treated at the temperature of 1100°C for 6 h to homogenize the (?Fe,Sn) single phase. Microstructural characterization and quantitative analysis of the phases were made by optical and scanning electron microscopy, microanalysis by energy dispersive spectroscopy (EDS) and X-ray powder diffraction. The Vickers microhardness of the samples was also measured. The magnetostriction was measured by capacitance dilatometry using a tilted plate dilatometer inserted into the Maglab platform by Oxford Instruments, using applied field in the range from -1.5 to 1.5 T and at temperatures close to 203 K. The samples saturation magnetization was obtained at 77, 203 and 300 K using the Quantum Design PPMS 6000. The saturation magnetostriction (?S) of the Fe-9Sn alloy samples was negative and the ?S vs. H curves behavior are similar to the pure Fe. Fe-20Sn alloy samples had positive ?S due to the presence of Fe3Sn2 and Fe5Sn3 ferromagnetic phases. The Fe-V alloys ?S was positive and larger in module than the Fe-Sn alloys ?S. We concluded that the substitution of Fe by Sn and V in a general way improved the magnetostriction of Fe, but the improvement was not as significant as observed with the substitution by Ga.
4

Avaliação da magnetostricção em ligas Fe1-xMx (M = V, Sn) e caracterização de suas propriedades magnéticas e microestruturais / Evaluation of magnetostriction and microstructural characterization of Fe-Sn and Fe-V alloys

Santos, Claudio Teodoro dos 25 January 2008 (has links)
Materiais magnetostrictivos exibem deformação elástica na presença de um campo magnético aplicado e por isso são de grande interesse para aplicação em sensores e atuadores. Trabalhos publicados no ano 2000 mostraram que a adição de Ga e Al ao Fe resulta em ligas com elevada magnetostricção em campos baixos. A partir daí os esforços foram direcionados para a descoberta de novas ligas magnetostrictivas à base de Fe com propriedades similares às encontradas nas ligas Fe-Ga e Fe-Al. No presente trabalho foram adicionados o Sn e o V ao Fe com o objetivo de avaliar a magnetostricção e a microestrutura das ligas formadas. Para isso, foram produzidas por fusão a arco as ligas Fe-9%at.Sn, Fe-20%at.Sn e as ligas Fex% at.V para x = 20, 25 e 30. As ligas Fe-Sn foram submetidas a tratamentos térmicos em 550 e 750°C por 24 h e em 880°C por 6 h e depois resfriadas rapidamente para a retenção das fases (Fe?,Sn), FeSn, Fe3Sn2 e Fe5Sn3. Já as ligas Fe-V foram tratadas em 1100°C por 6 h para homogeneização da fase única (Fe?,V). A caracterização microestrutural e análise quantitativa das fases foram feitas por microscopia óptica e eletrônica de varredura, microanálise por energia dispersiva (EDS) e difratometria de raios X. Também foi medida a microdureza Vickers das amostras. A magnetostricção foi medida por dilatometria de capacitância usando um dilatômetro de placa inclinada inserido no equipamento Maglab da Oxford Instruments, em campos na faixa de -1,5 a 1,5 T e temperaturas próximas de 203 K. A magnetização de saturação das amostras foi obtida em 77, 203 e 300 K utilizando o PPMS 6000 da Quantum Design. A magnetostricção de saturação (?S) das amostras da liga Fe-9Sn foi negativa e o comportamento das curvas similar ao do Fe puro. As amostras da liga Fe- 20Sn apresentaram ?S positiva devido à presença das fases ferromagnéticas Fe3Sn2 e Fe5Sn3. A ?S das ligas Fe-V foi positiva e maior em módulo do que a das ligas Fe-Sn. Concluiu-se que a substituição do Fe por Sn e V de modo geral melhorou a magnetostricção do Fe, porém a melhora não foi tão relevante quanto a observada pela substituição por Ga. / Magnetostrictive materials exhibit elastic strain in the presence of an applied magnetic field and therefore are of great interest for use in sensors and actuators. Works published in 2000 showed that the addition of Ga and Al in Fe results in alloys with high magnetostriction at low fields. Since then efforts have been directed to the discovery of new magnetostrictive Fe based alloys with similar properties to those found in Fe-Ga and Fe-Al alloys. In the present work Sn and V were added to Fe with the purpose of evaluating the magnetostriction and microstructure of these alloys. Therefore, Fe-9at.%Sn, Fe-20at.%Sn alloys and Fexat.% V alloys for x = 20, 25 and 30 were produced by arc melting. The Fe-Sn alloys were heat-treated at the temperatures of 550 and 750°C for 24 h and 880°C for 6 h and then rapidly cooled to the retention of the (?Fe,Sn), FeSn, Fe3Sn2 and Fe5Sn3 phases. Fe-V alloys were heat-treated at the temperature of 1100°C for 6 h to homogenize the (?Fe,Sn) single phase. Microstructural characterization and quantitative analysis of the phases were made by optical and scanning electron microscopy, microanalysis by energy dispersive spectroscopy (EDS) and X-ray powder diffraction. The Vickers microhardness of the samples was also measured. The magnetostriction was measured by capacitance dilatometry using a tilted plate dilatometer inserted into the Maglab platform by Oxford Instruments, using applied field in the range from -1.5 to 1.5 T and at temperatures close to 203 K. The samples saturation magnetization was obtained at 77, 203 and 300 K using the Quantum Design PPMS 6000. The saturation magnetostriction (?S) of the Fe-9Sn alloy samples was negative and the ?S vs. H curves behavior are similar to the pure Fe. Fe-20Sn alloy samples had positive ?S due to the presence of Fe3Sn2 and Fe5Sn3 ferromagnetic phases. The Fe-V alloys ?S was positive and larger in module than the Fe-Sn alloys ?S. We concluded that the substitution of Fe by Sn and V in a general way improved the magnetostriction of Fe, but the improvement was not as significant as observed with the substitution by Ga.
5

Diffusion-controlled phase transitions as a tool for tailoring Fe-Ga functional properties

Palacheva, V.V., Emdadi, A., Emeis, F., Bobrikov, I.A., Divinski, S.V., Balagurov, A.M., Wilde, G., Golovin, I.S. 17 September 2018 (has links)
No description available.
6

Structural Investigations of Highly Strictive Materials

Yao, Jianjun 22 May 2012 (has links)
Ferroelectric (piezoelectric) and ferromagnetic materials have extensively permeated in modern industry. (Na1/2Bi1/2)TiO3-BaTiO3 (NBT-x%BT) single crystals and K1/2Na1/2NbO3 (KNN) textured ceramics are top environment-friendly candidates which have potential to replace the commercial lead zirconate titanate or PZT. High magnetostrictive strain (up to 400 ppm) of Fe-xat.%Ga makes this alloys promising alternatives to existing magnetostrictive materials, which commonly either contain costly rare-earth elements or have undesirable mechanical properties for device applications. These systems have common characteristics: compositional/thermal/ electrical dependent structural heterogeneity and chemical disorder on sub-micron or nano scale, resulting in diverse local structures and different physical properties. In this work, I have investigated domain and local structures of NBT-x%BT crystals, KNN ceramics and Fe-xat.%Ga alloys under various conditions, mainly by scanning probe and electron transmission techniques. In NBT-x%BT single crystals, polarized light, piezo-response force (PFM) and transmission electron (TEM) microscopies were used to study domain structures and oxygen octahedral tiltings. Hierarchical domain structures were found in NBT: a high-temperature tetragonal ferroelastic domain structure is elastically inherited into a lower temperature rhombohedral ferroelectric phase. Nanoscale domain engineering mechanism was found to still work in NBT-x%BT system and a modified phase diagram was proposed based on domain observations. An increased intensity of octahedral in-phase tilted reflections and a decrease in the anti-phase ones was observed, with increasing x as the morphotropic phase boundary (MPB) is approached. It was also found that Mn substituents favor the formation of long range ordered micro-sized ferroelectric domains and octahedral in-phase tilted regions near the MPB. Nano-size heterogeneous regions were observed within submicron domain structure, indicating that the nanoscale polarization dynamics are not confined by domain boundaries, and the high piezoelectricity of NBT-x%BT is due to a polarization dynamics with high sensitivity to electric field and a broadened relaxation time distribution. In KNN textured ceramics, an aging effect was found to exist in the orthorhombic single phase field, not only in the orthorhombic and tetragonal two-phase field as previously reported. No variation of phase structure was revealed between before and after aging states. However, pronounced changes in domain morphology were observed by both PFM and TEM: more uniform and finer domain structures were then found with aging. These changes were even more pronounced after poling the aged state. A large number of sub-micron lamellar domains within micron-domains were observed: suggesting a domain origin for improved piezoelectric properties. In Fe-xat.%Ga alloys, an underlying inhomogeneity from Ga atoms embedded into the α-Fe matrix was believed to be the origin of giant magneostrictive properties. I have systematically investigated the phase structure and nano-size heterogeneity of Fe-xat.%Ga alloys subjected to different thermal treatments using standard TEM and high resolution TEM for 10<x<30. Nano-precipitates were observed in all specimens studied: A2, D03 and B2 phases were found depending on x. Nano-precipitates of D03 were observed to be dominant for compositions near the magnetostriction peaks in the phase diagram. Quenching was found to increase the volume fraction of nanoprecipitates for x=19, near the first magnetostriction peak. With increasing x to 22.5, nanoprecipitates were observed to undergo a D03 – B2 transformation. A high density of D03 precipitates of nanoscale size was found to be the critical factor for the first maximum in the magnetostriction. / Ph. D.
7

Užití kovových materiálů pro selektivní růst / Application of metallic materials for selective growth

Němeček, Tomáš January 2008 (has links)
The Si(100) surface and Ga surface phases up to 1 ML on their oxidation have been studied by XPS and LEED. The selective growth of Ga on the SiO2/Si structures fabricated by EBL has been analyzed using SEM and AFM methods. It was proved that Ga clusters grow in structures beside the oxide. The structure of alumina on Ni3Al(111) and NiAl(110) substrates was fully determined by combining the results of STM measurements and DFT simulations. It was determined the alumina/NiAl(110) does not form a suitable template for ordered Fe and Co clusters growth. However, the next research confirmed the alumina/Ni3Al(111) forms template appropriate to clusters growth purpose.
8

An Investigation of the Structural and Magnetic Transitions in Ni-Fe-Ga Ferromagnetic Shape Memory Alloys

Heil, Todd M. 06 January 2006 (has links)
The martensite and magnetic transformations in Ni-Fe-Ga ferromagnetic shape memory alloys are very sensitive to both alloy chemistry and thermal history. A series of Ni-Fe-Ga alloys near the prototype Heusler composition (X2YZ) were fabricated and homogenized at 1423 °K, and a Ni₅₃Fe₁₉Ga₂₈ alloy was subsequently annealed at various temperatures below and above the B2/L21 ordering temperature. Calorimetry and magnetometry were employed to measure the martensite transformation temperatures and Curie temperatures. Compositional variations of only a few atomic percent result in martensite start temperatures and Curie temperatures that differ by about 230 °K degrees and 35 °K degrees, respectively. Various one-hour anneals of the Ni₅₃Fe₁₉Ga₂₈ alloy shift the martensite start temperature and the Curie temperature by almost 70 °K degrees. Transmission electron microscopy investigations were conducted on the annealed Ni₅₃Fe₁₉Ga₂₈ alloy. The considerable variations in the martensite and magnetic transformations in these alloys are discussed in terms of microstructural differences resulting from alloy chemistry and heat treatments. The phase-field method has been successfully employed during the past ten years to simulate a wide variety of microstructural evolution in materials. Phase-field computational models describe the microstructure of a material by using a set of field variables whose evolution is governed by thermodynamic functionals and kinetic continuum equations. A two dimensional phase-field model that demonstrates the ferromagnetic shape memory effect in Ni2MnGa is presented. Free energy functionals are based on the phase-field microelasticity and micromagnetic theories; they account for energy contributions from martensite variant boundaries, elastic strain, applied stress, magnetocrystalline anisotropy, magnetic domain walls, magnetostatic potential, and applied magnetic fields. The time-dependent Ginzburg-Landau and Landau-Lifshitz kinetic continuum equations are employed to track the microstructural and magnetic responses in ferromagnetic shape memory alloys to applied stress and magnetic fields. The model results show expected microstructural responses to these applied fields and could be potentially utilized to generate quantitative predictions of the ferromagnetic shape memory effect in these alloys. / Ph. D.
9

Structure, Microstructure and Magnetic Properties of Fe-Ga and R-Fe based Magnetostrictive Thin Films

Basumatary, Himalay January 2016 (has links) (PDF)
Magnetostrictive materials belong to an important class of smart magnetic materials which have potential applications as ultrasonic transducers, sensors, actuators, delay lines, energy harvesting devices etc. Although, magnetostrictive property is exhibited by almost all ferro and ferrimagnetic materials, the R-Fe type (R represents rare earth elements) intermetallic compounds display maximum promise owing to the large magnetostriction exhibited by them at ambient temperature. Among the several R-Fe type compounds, Tb-Fe and Sm-Fe alloys are found to exhibit maximum room temperature positive and negative magnetostriction respectively. Recently, Fe-Ga based alloys have gained significant interest as newly emerging magnetostrictive material due to a good combination of magnetic and mechanical properties. These magnetostrictive materials in thin film form are of interests for several researchers both from fundamental and applied perspectives. Currently, many researchers are exploring the possibility of using magnetostrictive thin films in micro- and nano-electromechanical systems (MEMS and NEMS). Three material systems viz. Fe-Ga, Tb-Fe and Sm-Fe in thin film form have been chosen for our investigations. DC magnetron sputtering and e-beam evaporation techniques were used for deposition of these thin films on Si (100) substrates. Several aspects such as evolution of microstructure, film surface morphology, structure and change in film composition with different processing conditions were investigated in detail, as the existing literature could not provide a clear insight. Further, detailed magnetic characterizations of these films were carried out and established a process-structure-property correlation. The thesis is divided into seven chapters. The first chapter presents a brief introduction of magnetostrictive phenomena and the physics behind its origin. A brief history of evolution of magnetostrictive materials with superior properties is also brought out. Introduction to the material systems considered for the present study has also been presented. Discussions on various aspects like crystal structures, magnetic properties, and phase diagrams of these material systems are also included in this chapter. Magnetostriction in thin films and its importance in current technological applications are discussed in short. Further, a summary of existing literature on thin films of these materials has been narrated to highlight the perspective of the work done in subsequent chapters. In addition to this, a clear picture of the grey area for further investigations has been provided. Formulation of detailed scope of work for this study is also provided in this chapter. Details of different experimental techniques used in this study for deposition and characterization of these films are given in chapter 2. In the third chapter of the thesis a detailed study on the structural, microstructural and magnetic properties of Fe-Ga films deposited using dc magnetron sputtering technique are presented. The effect of sputtering parameters such as (i) Ar pressure, (ii) sputtering power, (iii) substrate temperature and (iv) deposition time/film thickness on the magnetic properties of the films are discussed in detail. All the films are found to be polycrystalline in nature with A2 type structure as evidenced from grazing incidence X-ray diffraction (GIXRD) and transmission electron microscope (TEM) studies. Surface morphology of the films are found to be affected with processing conditions considerably. Thermomagnetic behaviour of the films studied using a Superconducting Quantum Interference Device (SQUID) magnetometer under zero field cooled (ZFC) and field cooled (FC) conditions are also presented. The sputtering parameters are also found to influence the magnetic properties of the films through modifications in microstructure, surface morphology and film compositions. Irrespective of the sputtering parameters, room temperature (RT) deposited Fe-Ga films are found to exhibit large magnetic coercively and large saturation magnetic field as compared to the bulk alloy of similar compositions which are not desirable for micromagnetic device applications. A significant improvement in the magnetic properties of the films was obtained in the films deposited at higher substrate temperatures and is correlated with modifications in grain size and film surface roughness. These films are also found to exhibit better magnetostriction than the RT deposited films. Further, the magnetic properties of Fe-Ga films as a function of film thickness in the range 2 – 480 nm are also presented. The nature of variation of coercively with film thickness was correlated with grain size effect and explained successfully with the help of random anisotropy model. In the fourth chapter, studies on the microstructural and magnetic properties of Tb-Fe films were presented. It was reported earlier that TbxFe100-x films exhibit in-plane magnetic anisotropy for the films with x > 42 at.% of Tb and out-of-plane anisotropy for the composition 28 < x < 42. Presence of these anisotropies is technologically important for different applications. We have studied the magnetic properties of Tb-Fe films in these two composition range. TbxFe100-x films with 54  x  59 were prepared using dc magnetron sputtering technique under varying Ar pressure and sputtering power and the details about microstructural and magnetic properties are presented in this chapter. All the films are found to be amorphous in nature. While the composition of the film is found to remain constant with sputtering power, the Fe concentration in the film is found to be depleted with increase in Ar pressure. Magnetic properties are found to change from superparamagnetic to ferromagnetic behaviour with increase in sputtering power. Curie temperature of the films are found to be low (below RT) and is explained based on sperimagnetic ordering of magnetic sub-lattices. The perpendicular magnetic anisotropy (PMA) or out-of-plane anisotropy behaviour of Tb-Fe films were not studied in detail as a function of film thickness. We have successfully prepared TbxFe100-x films with 29  x  40 using e-beam evaporation technique using alloy target composition of TbFe in order to study the PMA behaviour as a function of film thickness. The thickness of the films was varied from 50 to 800 nm. All the films are found to be amorphous and columnar growth structure with fine channels of voids are observed from the TEM studies. Detailed magnetization and thermomagnetic measurements were carried out using SQUID magnetometer at different temperatures. The out-of-plane magnetic coercivity of the films was found to increase with film thickness and then decreases with further increase in thickness. Maximum coercivity of ~ 20 kOe has been obtained for the 400 nm thick film. Magnetic domain patterns were studied using magnetic force microscopy (MFM) technique and the observed magnetic properties are correlated with domain pattern and microstructures. Although there are several reports on device applications of Sm-Fe thin films which exhibit negative magnetostriction, a comprehensive study on the effect of different process parameters on the magnetic properties and its correlation with structure and microstructure is still elusive. Hence, Sm-Fe films were deposited on Si (100) substrate using dc magnetron sputtering technique under varying Ar pressure and sputtering power. Effect of these parameters on the microstructural and magnetic properties of the films was studied in detail and is presented in chapter 5. The curie temperature of the films was found to increase with increase in sputtering power and Ar pressure. This was attributed to increase in film thickness and size of islands (atomic clusters). Coercivity as low as 30 Oe has been achieved in the film deposited at 15 mTorr Ar pressure. The Curie temperature for the films deposited at higher Ar pressure (10 and 15 mTorr) are found to be above RT. Maximum saturation magnetostriction of ~ - 390 -strains has been achieved in the film deposited at 15 mTorr Ar pressure. Rapid thermal processing (RTP) experiments were also carried out to increase the magnetic ordering in the films deposited at low Ar pressure (5 mTorr) by imparting structural ordering. Large improvement in magnetization and Curie temperature of the film was observed after RTA. However, this could be attributed to the formation of nano-crystalline Fe phase as evidenced from the TEM studies and thermomagnetic measurements. An overall summary of the experimental results has been presented in chapter 6. The scope of work for further study in future has also been highlighted in chapter 7.
10

An Investigation On The Effect Of Structural And Microstructural Attributes On Magnetostriction Of Tb-Dy-Fe And Fe-Ga Alloys

Palit, Mithun 07 1900 (has links) (PDF)
Giant magnetostrictive RFe2 type (R represents rare earths) intermetallics form an important class of magnetic materials keeping in view of their potential applications as sensors and/ or actuators. In this thesis, one such mixed rare earth compound (Tb,Dy)Fe2 has been chosen for investigations. Being a technologically important material system, several investigations concerning physical and magnetic properties of the material and effect of processing parameters on magnetic properties have been reported in the available literature. However, existing literature does not provide a clear insight into some important aspects such as phase equilibria, evolution of texture and microstructure of directionally solidified Tb-Dy-Fe alloys. Therefore, the present work was undertaken to bring out tangible process-structure-property correlations with an emphasis to clarify the grey areas in the available literature. The investigation on the nature of ternary phase equilibria of Tb-Dy-Fe was taken up with an aim to understand the effect of Tb/Dy ratio on phase equilibria and magnetic properties of TbxDy1-xFe1.95 (x=0-1) alloys. Microstructural and micro-chemical analysis along with study of lattice parameter has been used to predict the nature of phase equilibria and the deviation from the assumed pseudo-binary behaviour. Further, from the microstructural investigations and study of lattice parameter and Curie temperature, a schematic sketch of a section of the ternary diagram, where (Tb,Dy) / Fe =1.95, was formulated and presented. Directional solidification technique is the most widely adopted method for processing the (Tb,Dy)Fe2, to impart grain orientation for practical applications. Therefore, it was aimed in the present study to understand the evolution of texture and microstructure in directionally solidified Tb0.3Dy0.7Fe1.95 alloy by modified Bridgman and zone melting techniques. The alloy was directionally solidified by modified Bridgman technique with a series of growth rates 5 - 100 cm/h, at a constant temperature gradient of 150oC/ cm. Microstructural investigation revealed formation of island banding at lower growth rate and peritectic coupled growth at higher growth rates. The texture study indicated a transition of growth texture from <113> to <110> and finally to <112> with increase of growth rate. A mechanism based on atomic attachment kinetics is proposed to explain the orientation selection with growth rate. The texture and microstructure have been correlated with magnetostriction and static strain co-efficient (dλ/dH) of the Bridgman solidified alloys. The solidification morphology observed in Bridgman solidified samples was found to be mostly plane front. Therefore, in order to understand the microstructure and texture evolution in cellular/ dendritic regime, directional solidification of Tb0.3Dy0.7Fe1.95 was attempted by zone melting technique with a lesser temperature gradient of 100oC/cm. A detailed texture study indicated a transition in preferred growth direction from <110> to <112> with increase of growth rate. In this case of cellular/ dendritic growth regime, a mechanism based on atomic attachment kinetics has been proposed and the preferred morphologies of the solid-liquid interface for <110> and <112> growth have been modelled. The modelled interfaces have been correlated to the shape of cell/ dendrite cross-section observed for the growth rates adopted in this study. Apart from the investigation carried out on the (Tb,Dy)Fe2 alloys, attempts have been made to understand the role of microstructure, especially the ordered phases on the magnetostriction of an emerging magnetostrictive material Fe-Ga. A series of alloy compositions of Fe-x at % Ga (x=17, 20, 23 and 25) were prepared and subjected to different thermal treatments and characterized for microstructural features and magnetostriction. Microstructure investigation of slow cooled, quenched and quenched + aged alloys reveals formation of ordered DO3 phase from disordered A2 phase by first order transformation in 17 and 20 at% Ga alloys, whereas for 23 and 25 at% alloys, the transformation takes place by continuous ordering. It could be observed that large magnetostriction arises owing to the presence of disordered A2 phase or ordered DO3 phase alone. The magnetostriction however decreases substantially when these two phases are co-existing.

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