The continuous high demand on permanent magnets in industries opened new research plateau to develop alternative magnetic material. The current used permanent magnet materials in the market still suffer from high cost and insufficient magnetic or thermal properties. The central focus of this dissertation work is the optimization of cobalt carbide based nanomaterial by means of modifying polyol synthesis assisted by nucleation agent and systematic statistics using JMP software tool. In most existing literatures, producing cobalt carbide (Co2C or Co3C) lack reproducibility and consistency resulting in nonsolid magnetic properties results. The practical requirements for cobalt carbide to be used as permanent magnet are high coercivity (Hc), high magnetization (Ms), resulting in a high-energy product (HcxMs). Previous literatures have shown coercivities of 1.5 to 2.5 kOe for cobalt carbides under aggressive temperatures conditions (300oC) or after aligning the particles under magnetic field. A statistical guided method performed a sequence of experiments toward producing high coercivities using surface response design. Primarily, the statistical study to optimize cobalt carbide was made by analyzing experimental condition to fulfill high magnetic properties with tuned conditions as much as possible. Therefore, having the advantage for superior control on process variable when shifting cobalt carbide for scale up production in flow chemistry set up using microreaction system (MMRS). The optimization is based upon selecting the most important conditions in polyol reaction to produce cobalt carbide (Co2C or Co3C) and feed JMP software model e.g. reaction temperature, reaction time, and or precursor concentration…etc. These factors called (effects) used to design experiments and generate tables to run minimum experiments. Points of each effect (levels) are selected based on previous knowledge and experience with the synthesis. The output called (response) can be any of the magnetic properties of our interest e.g. magnetization (Ms), coercivity (Hc), or energy magnetic product (HcxMs). In the first model fit of cobalt carbide magnetic was studied in a polyol reaction to increase its magnetic energy product and optimize the experimental conditions. The results disclosed increase in magnetic energy product (6.2 MGOe) when validating the prediction model conditions suggested by JMP: shorter reaction time, and lower precursor concentration conditions at maximum reaction temperature. Finally, to my knowledge studying the effect of the nucleating agent to alter cobalt carbide growth have not been studied so far. Therefore, statistical study design using central composite design (CCD) to investigate the nucleating agent effect of silver nitrite on cobalt carbide coercivity was made. The importance of nucleating agent on coercivity is vigorous to attain and control the growth direction of cobalt carbide nanoparticles. This is due to the shape anisotropy contribution to enhance coercivity unlike weak shape anisotropy attributed to agglomeration of nanoparticles demonstrated in previous studies. Enhancement of coercivity reached 3 kOe with aspect ratio control as a function of silver nitrite concentration under lower reaction temperature. The continuous high demand on permanent magnets in industries opened new research plateau to develop alternative magnetic material. The current used permanent magnet materials in the market still suffer from high cost and insufficient magnetic or thermal properties. The central focus of this dissertation work is the optimization of cobalt carbide based nanomaterial by means of modifying polyol synthesis assisted by nucleation agent and systematic statistics using JMP software tool. In most existing literatures, producing cobalt carbide (Co2C or Co3C) lack reproducibility and consistency resulting in nonsolid magnetic properties results. The practical requirements for cobalt carbide to be used as permanent magnet are high coercivity (Hc), high magnetization (Ms), resulting in a high-energy product (HcxMs). Previous literatures have shown coercivities of 1.5 to 2.5 kOe for cobalt carbides under aggressive temperatures conditions (300oC) or after aligning the particles under magnetic field. A statistical guided method performed a sequence of experiments toward producing high coercivities using surface response design. Primarily, the statistical study to optimize cobalt carbide was made by analyzing experimental condition to fulfill high magnetic properties with tuned conditions as much as possible. Therefore, having the advantage for superior control on process variable when shifting cobalt carbide for scale up production in flow chemistry set up using microreaction system (MMRS). The optimization is based upon selecting the most important conditions in polyol reaction to produce cobalt carbide (Co2C or Co3C) and feed JMP software model e.g. reaction temperature, reaction time, and or precursor concentration…etc. These factors called (effects) used to design experiments and generate tables to run minimum experiments. Points of each effect (levels) are selected based on previous knowledge and experience with the synthesis. The output called (response) can be any of the magnetic properties of our interest e.g. magnetization (Ms), coercivity (Hc), or energy magnetic product (HcxMs). In the first model fit of cobalt carbide magnetic was studied in a polyol reaction to increase its magnetic energy product and optimize the experimental conditions. The results disclosed increase in magnetic energy product (6.2 MGOe) when validating the prediction model conditions suggested by JMP: shorter reaction time, and lower precursor concentration conditions at maximum reaction temperature. Finally, to my knowledge studying the effect of the nucleating agent to alter cobalt carbide growth have not been studied so far. Therefore, statistical study design using central composite design (CCD) to investigate the nucleating agent effect of silver nitrite on cobalt carbide coercivity was made. The importance of nucleating agent on coercivity is vigorous to attain and control the growth direction of cobalt carbide nanoparticles. This is due to the shape anisotropy contribution to enhance coercivity unlike weak shape anisotropy attributed to agglomeration of nanoparticles demonstrated in previous studies. Enhancement of coercivity reached 3 kOe with aspect ratio control as a function of silver nitrite concentration under lower reaction temperature.

Neste trabalho foram produzidos filmes finos de Si[100]/buffer/NiFe/FeMn/Ta (buffer = Cu; Ta) e válvulas de spin de Si[100]/Cu/NiFe/Cu/NiFe/FeMn/Ta via Sputtering, e seus comportamentos magnéticos foram estudados analisando curvas de inversão de primeira ordem (First Order Reversal Curves, FORCs). Um Modelo de Preisach com Exchange-Bias foi desenvolvido e sua implementação computacional permitiu simular a histerese e as curvas forcas das bicamadas de NiFe/FeMn. O modelo também permitiu reproduzir os comportamentos assimétricos dos dois ramos da curva de histerese destes filmes. A análise dos resultados evidenciou os efeitos de campo médio sobre a camada de Py em função da espessura da camada de FeMn. A aplicação da análise FORC nas válvulas de spin se revelou interessante para estudar o grau de acoplamento entre as camadas livre e pressa, assim como os efeitos de campo médio em cada camada. / In this work, thin films of Si[100]/buffer/NiFe/FeMn/Ta (buffer = Cu; Ta) and spin valves of Si[100]/Cu/NiFe/Cu/NiFe/FeMn/Ta were produced via sputtering and their magnetic behavior were studied by First Order Reversal Curves (FORC\'s) analysis. A Preisach Model with Exchange-Bias was developed and applied in order to simulate the hysteresis and the first order reversal curves of the NiFe/FeMn bilayers. In addition, the model allowed to reproduce the asymmetric behaviors present in both branches of the hysteresis curve in these films. The study put in evidence the mean field effects on de Py layer as a function of the thickness of the FeMn layer. The application of the FORC analysis in the spin valves was interesting to study the degree of coupling between the free and the pressed layers, as well as the effect of mean field in each layer.

Neste trabalho foram produzidos filmes finos de Si[100]/buffer/NiFe/FeMn/Ta (buffer = Cu; Ta) e válvulas de spin de Si[100]/Cu/NiFe/Cu/NiFe/FeMn/Ta via Sputtering, e seus comportamentos magnéticos foram estudados analisando curvas de inversão de primeira ordem (First Order Reversal Curves, FORCs). Um Modelo de Preisach com Exchange-Bias foi desenvolvido e sua implementação computacional permitiu simular a histerese e as curvas forcas das bicamadas de NiFe/FeMn. O modelo também permitiu reproduzir os comportamentos assimétricos dos dois ramos da curva de histerese destes filmes. A análise dos resultados evidenciou os efeitos de campo médio sobre a camada de Py em função da espessura da camada de FeMn. A aplicação da análise FORC nas válvulas de spin se revelou interessante para estudar o grau de acoplamento entre as camadas livre e pressa, assim como os efeitos de campo médio em cada camada. / In this work, thin films of Si[100]/buffer/NiFe/FeMn/Ta (buffer = Cu; Ta) and spin valves of Si[100]/Cu/NiFe/Cu/NiFe/FeMn/Ta were produced via sputtering and their magnetic behavior were studied by First Order Reversal Curves (FORC\'s) analysis. A Preisach Model with Exchange-Bias was developed and applied in order to simulate the hysteresis and the first order reversal curves of the NiFe/FeMn bilayers. In addition, the model allowed to reproduce the asymmetric behaviors present in both branches of the hysteresis curve in these films. The study put in evidence the mean field effects on de Py layer as a function of the thickness of the FeMn layer. The application of the FORC analysis in the spin valves was interesting to study the degree of coupling between the free and the pressed layers, as well as the effect of mean field in each layer.

In dieser Arbeit wurden mit der gepulsten Laserdeposition Nd-Fe-B-Schichten abgeschieden. Diese Schichten wurden auf einem geheizten Substrat deponiert und reagierten zu der hart-magnetischen Nd2Fe14B-Phase. Eine weitere Phase in den Schichten ist Neodym aufgrund der überstöchiometrischen Abscheidung von Neodym zur Unterstützung der Phasenbildung von Nd2Fe14B und zur Entkoppelung der Nd2Fe14B-Körner. Für die Mikrostruktur und die magnetischen Eigenschaften der Schichten sind die Grenzflächen zum Substrat und zur Umgebung von entscheidender Bedeutung, da sich die überwiegende Anzahl der Körner im Kontakt mit zumindest einer der beiden Grenzflächen befindet. Aus diesem Grund stand die Untersuchung des Einflusses der Grenzflächen auf das Wachstum, die Mikrostruktur und die magnetischen Eigenschaften der Nd-Fe-B-Schichten im Mittelpunkt der Arbeit. Die Nd-Fe-B-Schichten wurden sowohl auf Chrom- als auch auf Tantalbuffern deponiert. Ein Buffer wurde zur Einstellung der Mikrostruktur und zum Schutz der Nd-Fe-B-Schicht vor Diffusion und Reaktionen mit den Elementen des Substrates benutzt. Die Untersuchungen zeigten, dass der Chrombuffer diese Bedingungen nur unzureichend erfüllt. Die Schichten, die auf dem Tantalbuffer deponiert wurden wachsen bei tiefen Depositionstemperaturen als zusammenhängende Schicht auf und zeigen eine magnetische Vorzugsorientierung mit der magnetisch leichten Richtung parallel zur Substratnormalen. Mit steigender Depositionstemperatur verbessert sich die Ausprägung der magnetischen Vorzugsorientierung bis die vollständige Ausrichtung aller magnetischen Momente parallel zur Substratnormale erreicht ist. Die Topologie dieser Schichten weist einzeln stehende Nd2Fe14B-Körner auf, was durch ein nicht benetzendes Verhalten von Nd2Fe14B auf Tantal erklärt wird. An Schichten, die bei Depositionstemperaturen um 630 °C auf dem Tantalbuffer abgeschieden wurden, konnte das epitaktische Wachstum von Nd2Fe14B nachgewiesen werden. Auch diese Schichten zeigen die Mikrostruktur der isoliert voneinander stehenden Körner. Obwohl die Korngröße dieser Körner etwa 2 µm beträgt, zeigen diese Schichten ein Koerzitivfeld von bis zu 2 T. Diese hohen Werte des Koerzitivfeldes werden durch die Vermeidung des Einbaus von Defekten in den Körnern erreicht. Zusammenfassend können diese Schichten als mikrometergroße und parallel zueinander angeordnete Einkristalle beschrieben werden. Aus diesem Grund konnten mit diesen Schichten Einkristallmessungen wie die Temperaturabhängigkeit der Sättigungspolarisation und des Spinreorientierungswinkels reproduziert werden. Aufgrund des epitaktischen Wachstums von Nd2Fe14B auf Tantal(110) konnte auch auf amorphen Substraten hochremanente und hochkoerzitive Schichten abgeschieden werden. Dafür wird ausgenutzt, dass der Tantalbuffer auch auf einem amorphen Substrat aufgrund der Wachstumauslese texturiert aufwächst und auf den einzelnen Körnern des texturierten Tantalbuffers die Nd2Fe14B-Körner lokal epitaktisch nukleieren können. Die Nd2Fe14B-Körner dieser Schichten sind nicht isoliert voneinander, sondern zeigen eine zusammenhängende Topologie. Diese Schichten besitzen ein Koerzitivfeld von etwa 1,3 T. Da Nd2Fe14B eine leicht oxidierende Phase ist, müssen die Nd-Fe-B-Schichten vor Korrosion geschützt werden. So wurde gezeigt, dass das Koerzitivfeld bei an Luft gelagerten Schichten innerhalb von einer Woche auf die Hälfte des ursprünglichen Wertes abfällt. Dieser Abfall konnte durch Defekte bzw. weichmagnetische Phasen als Ergebnis der Oxidation an den Oberflächen der Nd2Fe14B-Körnern erklärt werden. Die Verhinderung der Oxidation und damit der Verschlechterung der magnetischen Eigenschaften konnte sehr effektiv, d.h. ohne eine messbare Veränderung der magnetischen Eigenschaften über einen Zeitraum von 6 Monaten; durch die Abscheidung einer Chromdeckschicht erreicht werden.

Les processus d'aimantation dans des aimants de type NdFeB ont été étudiés dans le cadre de cette thèse, sur la base de mesures d'aimantation macroscopiques et de caractérisations locales (MFM). Deux types d'échantillons ont été analysés : des aimants massifs dont les propriétés excellentes résultent d'un processus d'infiltration de NdCu le long des joints de grain (échantillons fournis par Toyota Motor Corporation) et des échantillons sous forme de couches épaisses, dont les microstructures, et, de ce fait les propriétés magnétiques, diffèrent. La variation thermique du champ coercitif et celle du volume d'activation ont été analysées dans le cadre de deux modèles, respectivement dénommé micromagnétique et global. Les valeurs déduites des deux paramètres principaux caractérisant la coercitivité (N représentant les effets du champ démagnétisant et α reliant le champ coercitif aux propriétés magnétiques intrinsèques de la phase dure) indiquent que dans les aimants massifs les différences de coercitivité entre échantillons sont dues pour l'essentiel à la variation de N alors que dans les films, c'est la variation du paramètre α qui joue le rôle principal. Le volume d'activation à une température donnée, dérivé de mesures de trainage magnétique, a des valeurs proches pour tous les échantillons massifs. Au contraire, il varie d'un échantillon à l'autre dans le cas des films : plus le champ coercitif est fort, plus petit est le volume d'activation. Une conclusion générale de cette étude est que les propriétés magnétiques au sein du volume d'activation sont proches de celles de la phase dure Nd2Fe14B. Le lien entre microstructure et coercivité a été examiné dans les films épais par microscopie de force magnétique (MFM). Des observations de films dans différents états rémanents le long du cycle d'hystérésis ont été réalisées. Des « domaines d'interactions » ont été révélés dans les films de faible coercitivté. Dans de tels films, comme dans ceux de coercitivité moyenne, le renversement d'aimantation est dominé par la propagation de domaines, alors que dans les films de plus forte coercitivité, la nucléation suivie de la propagation de domaines d'orientation inverse à celle de l'aimantation principale dominent. / Magnetization reversal in NdFeB-type permanent magnets was studied in this thesis, based on both global (magnetometry) and local (magnetic force microscopy) experimental techniques. Two types of samples were analyzed: bulk magnets of which magnetic properties are greatly improved as a result of NdCu infiltration along the grain boundaries (samples provided by Toyota Motor Corporation) and thick film magnets with different microstructures and thus different coercive fields. The temperature dependence of the coercive field and that of the activation volume were analyzed in the framework of two models: the micromagnetic and the global model. The derived values of the two main parameters characterizing coercivity (N representing demagnetizing field effects and α linking the coercive field to the intrinsic magnetic properties of the hard phase) indicate that, in bulk magnets, the difference in coercivity between different samples is related mainly to N whereas in films the parameter alfa plays the leading role. The activation volume derived from magnetic after effect measurements is similar for all bulk samples at a given temperature. On the opposite, it varies in the case of films : the higher the coercive field, the smaller the activation volume. Altogether, it is concluded that the magnetic properties within the activation volume are close to those of the main phase. The link between microstructure and coercivity was studied in thick films, using magnetic force microscopy. Imaging of films that present different microstructures was performed in different remanent states along the hysteresis cycle. Interaction domains were observed in the case of films with lower coercive field. In such low coercivity films, as well as in medium coercivity ones, magnetization reversal is dominated by domain wall propagation, instead of nucleation + propagation in high coercivity films.

In this study, the ageing effects on powder used for cemented carbide insert production are examined. Ageing is throughout this study, defined as the time dependent change of the magnetic properties: coercive field strength and saturation magnetization. Testing is done using eight different powder compositions stored in both air and in an argon cabinet for 10 weeks, where sampling is done at specific intervals. Samples are stored in vacuum sealed bags for a combined sintering at the last phase of the test. Magnetic properties are assumed to be dependent on the amount of oxides needed to be reduced by taking carbon from the material itself during the vacuum stage of the sintering. To achieve interpretive results, this study also tested available sintering furnaces (DMK and DEK) by sintering trays with patterns of test pieces. This shows that DEK furnaces are much better for the ageing tests performed in this study, since less variation of the magnetic properties are measured because of the symmetrical heat gradient over each tray. Ageing tests strongly suggest that the cause of ageing comes from water absorbed by the PEG in the powder composition. Changing the molecular weight of the PEG seems to have an effect on the powder's ageing sensitivity. Measurements performed in this study show less ageing for Cr-rich DA-powders than for cubic carbide rich DQ-powders.

Made available in DSpace on 2014-12-17T15:14:43Z (GMT). No. of bitstreams: 1 AndreSWTS_capa_ate_secao2.pdf: 3305591 bytes, checksum: 5f27842b5915ba4ade82c5d3c89c759b (MD5) Previous issue date: 2007-12-07 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / The e?ect of ?nite size on the magnetic properties of ferromagnetic particles systems is a recurrent subject. One of the aspects wide investigated is the superparamagnetic limit where the temperature destroys the magnetic order of ferromagnetic small particles. Above the block temperature the thermal value of the magnetic moment of the particle vanishes, due to thermal ?uctuations. The value of the blocking temperature diminishes when the size of the particle is reduced, re?ecting the reduction of the anisotropy energy barrier between the uniform states along the uniaxial axis. The increasing demand for high density magnetic media has recently attracted great research interest in periodic arrangements of nanometric ferromagnetics particles, approach in the superparamagnetic limit. An interesting conjecture is the possibility of stabilization of the magnetic order of small ferromagnetic particles (F) by interface coupling with antiferromagnetic (AF) substrate. These F/AF systems may also help to elucidate some details of the e?ect of exchange bias, because the e?ect of interface roughness and the paper of domain walls, either in the substrate or the particle, are signi?cantly reduced. We investigate the magnetic phases of small ferromagnetic particles on a antiferromagnetic substrate. We use a self-consistent local ?eld method, incorporating the interface ?eld and the dipole interaction between the spins of the ferromagnetic particle. Our results indicate that increasing the area of the interface favors the formation of the uniform state. Howere above a critical height value appears a state non-uniform is formed where the spins of in the particle s free surface are rotated with respect to the interface spins direction. We discuss the impact of the competition between the dipolar and interface ?eld on the magnetic charge, that controls the ?eld of ?ux leakage of the particle, and on the format of the hysteresis curves. Our results indicate that the liquid magnetic charge is not a monotonically increasing function of the height of the particle. The exchange bias may display anomalous features, induced for the dipolar ?eld of the spins near the F/AF interface / O efeito de tamanho ?nito nas propriedades magn?ticas de sistemas de part?culas ferromagn?ticos ? um tema recorrente. Um dos aspectos largamente investigados ? o limite superparamagn?tico em que a temperatura desestabiliza a ordem magn?tica de part?culas ferromagn?ticas pequenas. Acima da temperatura de bloqueio o valor m?dio t?rmico do momento magn?tico da part?cula se torna nulo, devido a ?utua??es t?rmicas. A temperatura de bloqueio diminui quando o tamanho da part?cula ? reduzido, re?etindo a queda na barreira de energia de anisotropia entre os estados de magnetiza??o uniforme ao longo do eixo uniaxial. A demanda crescente por meios de grava??o magn?tica de alta densidade tem atualmente despertado grande interesse de pesquisa em arranjos peri?dicos de part?culas ferromagn?ticas de dimens?es nanom?tricas, beirando o limite superparamagn?tico. Uma conjectura interessante, levantada experimentalmente, se refere ? possibilidade de estabiliza??o da ordem magn?tica de part?culas ferromagn?ticos (F) via o acoplamento de interface com substratos antiferromagn?ticos (AF) com temperatura de N?el acima da temperatura ambiente. Esses sistemas se prestam igualmente para elucidar alguns detalhes do efeito de Exchange bias , dado que, o efeito de rugosidade de interface e o papel de paredes de dom?nio, seja no substrato ou na part?cula, s?o reduzidos. Investigamos as fases magn?ticas de uma pequena part?cula ferromagn?tica, com diversas geometrias e disposi??es de deposi??o sobre um substrato antiferromagn?tico. Usamos um m?todo de campo local auto-consistente, incorporando o campo de interface e a intera??o dipolar entre os spins da part?cula ferromagn?tica. Nossos resultados indicam que aumentando a ?rea da interface favorece a forma??o do estado uniforme. Por?m se a altura da part?cula ? superior a um valor cr?tico surge um estado n?o-uniforme em que os spins se orientam de modo a minimizar a carga magn?tica super?cial. Discutimos o impacto que a competi??o entre esses efeitos tem na carga magn?tica l?quida, que controla o campo de fuga da part?cula e no formato das curvas de histerese. Nossos resultados indicam que a carga l?quida n?o ? uma fun??o monot?nicamente crescente da altura da part?cula e que o deslocamento da histerese pode sofrer altera??es relevantes, induzidas pelo campo dipolar, fugindo do padr?o esperado normalmente em sistemas F/AF extensos

Orientador: Marco Antonio Bica de Moraes / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Fisica Gleb Wataghin / Made available in DSpace on 2018-08-18T19:35:50Z (GMT). No. of bitstreams: 1 Fischer_GiovanaZaniniGadioli_D.pdf: 32265979 bytes, checksum: f410dfb24adff86c43498027515957c8 (MD5) Previous issue date: 2011 / Resumo: Neste trabalho, a técnica de magnetron-sputtering foi empregada para fabricar filmes multicamadas de Gd/W e Gd/Cr, cujas propriedades magnéticas foram investigadas em função da espessura das camadas de Gd, dGd, e da temperatura do substrato, TS, durante a deposição. Espectroscopia de retroespalhamento Rutherford e espectroscopia fotoeletrônica de raios-x foram utilizadas, respectivamente, para detectar possível contaminação de oxigênio e para verificar a continuidade da camada de Gd sobre W e Cr. Difratometria de raios-X de baixo ângulo (GAXRD) e microscopia eletrônica de varredura (MEV) foram empregadas para investigar a estrutura cristalina e morfologia das amostras. As análises de GAXRD mostraram que nas amostras Gd/W as camadas de Gd são amorfas. Nas amostras Gd/Cr, entretanto, a cristalinidade do Gd aumenta com o aumento de dGd e TS. Pelas medidas de MEV foi visto que os filmes de Gd tanto sobre W quanto Cr são granulares. Para investigar as propriedades magnéticas utilizamos um magnetômetro SQUID e um PPMS. O primeiro foi utilizado para as medidas de momento magnético em função do campo estático, Hdc, e da temperatura, T. O PPMS foi utilizado nas investigações de susceptibilidade magnética ac em função de T, medidas em diferentes frequências de oscilação do campo e diferentes Hdc. A complexa natureza magnética dos filmes com dGd = 10 nm foi observada através das isotermas M x H, que não apresentaram saturação, para a maioria das amostras, nem mesmo em baixas temperaturas e altos campos. Pela análise dos dados magnéticos em função da temperatura, observamos que o caráter ferromagnético nas amostras se acentua à medida que TS e dGd aumentam. A temperatura de Curie, TC, também depende de TS e dGd, aumenta de 247 a 297 K com o aumento dos dois últimos parâmetros. A partir das isotermas M x H o momento magnético de saturação a 0 K foi calculado, e ele mostrou-se dependente de TS. A existência de vidros magnéticos nas amostras com dGd = 10 nm foi fortemente sugerida pelos resultados obtidos de magnetização e susceptibilidade ac, ambas em função de T. Para filmes com dGd = 10 nm, o efeito magnetocalórico foi investigado através da variação de entropia magnética, ?SM, em função da temperatura, para a remoção de um campo de 50 kOe. Curva de ?SM x T para as amostras Gd/Cr com TS = 300 e 500 ºC exibiram picos a alta temperatura denotando ferromagnetismo. Por outro lado, a amostra Gd/Cr depositada a 30ºC e todos os filme Gd/W não apresentaram nenhum pico em ?SM x T, indicando ausência ou baixa quantidade da fase ferromagnética. Todas as medidas são consistentes em indicar múltiplas fases magnéticas nas amostras e temperaturas de transição. Uma forte consistência entre as medidas magnéticas, GAXRD e MEV é verificada / Abstract: Direct current magnetron sputtering was used to synthetize Gd/W and Gd/Cr multilayer films, whose magnetic properties were investigated as a function of the Gd layer thickness, dGd, and the substrate temperature, TS, during deposition. Rutherford backscattering spectroscopy and x-ray photoelectron spectroscopy were employed, respectively, to detect possible oxygen contamination and to check the continuity of the coverage of the Gd layers on top of those of W and Cr. Grazing angle X-ray diffraction (GAXRD) and scanning electron microscopy (SEM) were used to investigate the crystalline structure and the morphology of the samples. The GAXRD analyses have shown that in the Gd/W samples the Gd layers are amorphous. In the Gd/Cr samples, however, Gd is crystalline. In these samples, the Gd crystalline order increases with increasing TS and dGd. From the SEM analysis, it was found that the Gd layers in either Gd/W or Gd/Cr samples were granular. To investigate the magnetic properties of the films, SQUID and PPMS magnetometries were used. With the former technique, the magnetic moments of the samples were measured as a function of a dc magnetic field, Hdc, and temperature, T. By PPMS, alternating magnetic fields, superimposed by different Hdc fields were used. The moments were measured as a function of T, Hdc and the frequency of the alternating field. The complex magnetic nature of the films with dGd = 10 nm was observed from the M x H isotherms, which did not show, for most of the samples, saturation even at high magnetic films and low temperatures. From the magnetic data as a function of temperature, it was observed that ferromagnetic character of the samples is enhanced as dGd and TS were increased. The Curie temperature, TC, also depends on TS and dGd as it increases from 247 to 297 K as the latter variables are increased. From the M x H isotherms the saturation magnetic moment at 0 K was determined, and it was observed that it depends on TS. The existence of magnetic glass states in samples with dGd = 10 nm was strongly suggested from both magnetization and ac susceptibility measurements as a function of T. For films with dGd = 10 nm, the magnetocaloric effect was investigated by the magnetic entropy change, ?SM, as a function of the temperature for the removal of a 50 kOe field. The ?SM x T plots for the Gd/Cr samples deposited at TS = 300 and 500 ºC exhibited high temperature peaks denoting ferromagnetism. On the other hand, for the Gd/Cr sample deposited at 30 ºC and for the all the Gd/W samples, such peaks were not seen, indicating the absence, or low-content, ferromagnetic phase. All magnetic measurements are consistent in indicating multiple magnetic phases in the samples and magnetic transition temperatures. A strong consistency among the magnetic and the GAXRD and SEM observations was also verified / Doutorado / Física da Matéria Condensada / Doutora em Ciências

This diploma thesis is focused on investigation of metallic thin films and nanostructures using scanning probe microscopy. Magnetic properties of these objects are studied by magnetic force microscopy, which is modification of scanning probe microscopy. In the theoretical part basic principles of scanning probe microscopy and magnetic force microscopy are summarized, and also principle of creation of magnetic domains and some special properties of ferromagnetic and antiferromagnetic materials. Further, two techniques of fabricating nanostructures are described. Experimental part is focused on imaging and simulating of magnetic domains. Further, exchange bias is revealed. This phenomenon is present in systems composed from ferromagnetic and antiferromagnetic materials. One part of this diploma thesis is also focused on discussion of problems with magnetic force microscopy.

Magnetic measurements are useful tools for quality control of cemented carbides. Previous work at Sandvik Mining and Rock Technology has shown that the coercivity increases with increased cooling rate during sintering for a specific grade.  This study aims to investigate why the coercivity changes with the cooling rate and if this is true for other cemented carbide grades as well. Three different cemented carbide grades were sintered with different cooling rates and evaluated with coercivity, Cobalt-magnetic saturation and hardness measurements, and with microscopy and Electron Backscatter Diffraction analysis. It was found that the coercivity increased with increasing cooling rates for the previously studied grade, but not for the two other grades. It was expected that the increased coercivity would indicate a decrease in WC grain size, but the results showed that the WC grain size of the fastest and slowest cooling rate were the same. However, a change in size of the Co areas between the WC grains was found. The fast cooled sample showed smaller Co areas than the slow cooled sample. These Co/WC grain boundaries increase the coercivity. An increased fraction of hcp-Co/fcc-Co was also found for the fast cooled material which also increases the coercivity. No relationship between the hardness and the coercivity or the cooling rate was found.   The contiguity for the different grades was also calculated.  No significant difference in contiguity between the different cooling rates of each material was found but the contiguity values between the different materials differed.  This is probably mainly dependent on the different binder contents of the materials. / Magnetiska egenskaper är en viktig del av kvalitetskontrollen av hårdmetaller.  Tidigare forskning hos Sandvik Mining and Rock Technology har visat att koerciviteten hos en hårdmetallsort ökar med ökad kylhastighet vid sintring.  Målet med den här studien är att undersöka varför koerciviteten ökar med kylhastigheten och om detta även gäller andra hårdmetallsorter.  Tre olika hårdmetallsorter sintrades med olika kylhastigheter undersöktes med mätningar av koercivitet, magnetisk mättnat i koboltfasen och hårdhet,  samt med mikroskopi och Electron Backscatter Diffraction analys. Det  visade  sig  att  koerciviteten  ökade  med  ökad  kylhastighet  för  hårdmetallsorten  som  studerats tidigare, men inte för de andra två sorterna.  En ökad koercivitet förväntas visa på en minskad WC-kornstorlek, men resultaten visar att det långsamt kylda och snabbkylda provet hade samma WC-kornstorlek.  Däremot upptäcktes en ändring av storleken på Co-områdena mellan WC-kornen.  Det snabbkylda provet visade en mindre storlek av Co-områdena jämfört med det långsamt kylda provet. Fler Co/WC-korngränser i det snabbkylda provet leder till en ökad koercivitet.  Fraktionen av hcp-Co/fcc-Co-korngränser ökade också för det snabbkylda provet vilket också ökar koerciviteten. Inget samband mellan hårdheten och koerciviteten eller kylhastigheten upptäcktes.  Beräkning av kontiguiteten för de olika sorterna genomfördes också. Ingen signifikant skillnad i koercivitet mellan de olika kylhastigheterna för the olika sorterna hittades,  men kontiguiteten mellan de olika sorterna varierade. Det beror mest troligt på att dom olika sorterna har olika mängd matrismaterial.