Nuclear magnetic resonance force microscopy (NMRFM) is a technique that combines aspects of scanning probe microscopy (SPM) and nuclear magnetic resonance (NMR) to obtain 3 dimensional nanoscale spatial resolution and perform spectroscopy. We describe the components of a helium-3 NMRFM probe and studies of ammonium sulfate ((NH₄)₂SO₄) and magnesium diboride (MgB₂). For our room temperature (NH₄)₂SO₄ studies we were able to perform a 1-D scan and perform nutation and spin echo experiments. In our 77 K MgB₂ we demonstrate a 1-D scan of a 30 micron powder sample. In addition, we describe magnetic measurements of the possible dilute semiconductors Mn[subscript x]Sc[subscript 1-x]N and Fe₀.₁Sc₀.₉N. / text

While magnesium diboride (MgB2) was first synthesized in the 1950s, MgB2’s superconductive properties were not discovered until 2001. It has the highest superconducting transition temperature of all the metallic superconductors at ~39 K at atmospheric pressure. MgB2 is also unique in that it has a two superconductive gaps, a pi gap at 2 meV and a sigma gap at 7.1 meV. There are a theoretical models discussing the inter- and intra- gap scattering of the superconductivity of MgB2 and the Josephson transport of MgB2 Josephson Junctions. The focus of this work is to further the study of all-MgB2 Josephson junctions and quantum interference device technology. This work discusses the transport in all-MgB2 Josephson junctions and designing, fabricating, and measuring multi-junction devices. The junctions studied include all-MgB2 sandwich-type Josephson junctions (one with TiB2 normal conducting barrier and another with an MgO insulating barrier). The junction MgB2 films were deposited by hyprid physical-vapor deposition and the junction barrier were deposited by sputtering. The junctions were patterned and etched with UV photolithography and argon ion milling. With the TiB2 barrier we studied Josephson transport by the proximity effect. With these junctions, we also observed complete suppression of the critical current by an applied magnetic field showing for the first time a leakage free barrier in an all-MgB2 Josephson junction with a single ultrathin barrier. We also studied junctions utilizing MgO barrier deposited by reactive sputtering which gave a larger characteristic voltage of 1-3 mV compared to TiB2 barriers. By connecting several SQUIDs with varying loop areas we developed of two types of superconducting quantum interference filters (SQIFs). The first SQIF designed with 21 SQUIDs connected in parallel and the SQUID loops are sensitive to magnetic fields applied parallel to the substrate. The SQUID loop areas were designed to vary in such a way that the voltage modulation gave a unique peak corresponding to the absolute value of the applied magnetic field. The SQIF shows an antipeak height of 0.25 mV with a transfer function of 16 V/T at 3 K. The lowest noise measured for this SQIF is 110 pT/Hz1/2. The second SQIF is designed with 17 SQUIDs in parallel and the SQUID loops are sensitive to magnetic field perpendicular to the substrate. This SQIF has shown improved voltage modulation with a peak height of 1 mV and a transfer function of 7800 V/T. The noise sensitivity was measured at 70 pT/Hz1/2. The sensitivity of the SQIF shows MgB2 potential superconductor to improve performance of current superconductive electronics. Utilizing known all-MgB2 junctions and SQUID parameters two rapid single flux quantum (RSFQ) circuits were designed and tested. A toggle flip flop (TFF) operating as a frequency divider was developed. The TFF design consisted of a Josephson transmission line, a splitter, and an interferometer (a DC SQUID). The TFF utilized an improved designed, compared to previous all-MgB2 TFFs, and showed operation up to 335 GHz at 7 K and operation up to 30 K. A low frequency set-reset flip flop (SRFF) was also developed to demonstrate RSFQ digital logic. The SRFF design includes a DC-SFQ converter, a Josephson transmission line, and an inductively coupled readout SQUID. The SRFF demonstrates proper digital logic by toggling between a high and low voltage state with a sequential set and reset input. While these developed devices are not close to the potential that MgB2 allows, they do show the promise MgB2 based devices have in making more sensitive and faster superconductive logic devices. / Physics

This thesis describes the fabrication and characterization of ex situ magnesium diboride (MgB<sub>2<) bulk material to study its sintering behaviour. Since the discovery of superconductivity in magnesium diboride in 2001, many research studies have identified the attractive properties of this easy-to-fabricate, low cost superconductor which can attain high critical current density even without heat-treatment. However there is little consensus in the literature on the processing requirements to produce high quality MgB<sub>2< material with low impurity content and high density. In this work, the key parameters in the production of dense ex situ MgB<sub>2< produced from Alfa Aesar MgB<sub>2< powder are established by examining the effect of modifying the characteristics of the starting material and the processing parameters during pressureless and pressure assisted heat-treatment. The particle size distribution, impurity content and particle morphology of Alfa Aesar MgB<sub>2< powder were determined using laser dffraction, X-ray diffraction, X-ray photoelectron spectroscopy, electron dispersive spectroscopy, scanning electron microscopy and transmission electron microscopy. This powder was also modified by separation (sieving and sedimentation) and milling (ball milling and attrition milling), with changes made to the powder determined by the same techniques. A pressureless heat-treatment method using a magnesium diboride powder bed was developed. This minimised MgO formation in samples produced from as-purchased MgB<sub>2< powder to less than 8 wt.% for heat-treatment at 1100°C. MgO content was determined by X-ray diffraction using calibrated standards. MgB<sub>2< bulk material was produced from as-purchased and modified powders by pressureless heat-treatment under Ar gas, and characterized using Archimedes' density method, X-ray diffraction, Vickers hardness testing, scanning electron microscopy, and magnetization measurements. Very limited densification was observed for all samples prepared by pressureless heat-treatment, with only limited increases in connectivity observed for some samples heat-treated at 1100°C. Pressure-assisted bulk samples were prepared from as-purchased MgB<sub>2< and selected modified powders using resistive sintering, spark plasma sintering, and hot pressing. These were characterized using the same techniques, which indicated much more extensive densification with similar levels of impurity formation as for pressureless heat-treatment at 1100°C. The results indicate that densification and applied pressure are strongly correlated, while the effect of temperature is less significant. The optimum processing environment (inert gas or vacuum) was dependent on the technique used. These results indicate that pressure-assisted heat-treatment is required in order to produce dense bulk MgB<sub>2<.

No description available.

No description available.

In the present study the results of investigations on polycrystalline MgB2 and on single crystals of YNi2B2C and HoNi2B2C are presented. In particular, measurementes of specific electrical resistance, thermal conductivity, thermoelectric power, and of the linear thermal expansion coefficient were performed. Moreover, the specific heat of polycristalline borocarbide samples was evaluated. From the measured data, the temperature dependencies of the Lorenz number and of the Grueneisen parameter can be determined, also the pressure dependence of the superconducting transition temperature using the Ehrenfest relation. At low temperatures a characteristic deviation of the resistivity from the Bloch-Grueneisen law in the normal state for all investigated substances was observed. A reentrant behaviour in resistivity and thermoelectric power occurs at the antiferromagnetic phase transition of HoNi2B2C. The thermal conductivity of MgB2 below 7 K is dominated by the scattering of phonons at grain boundaries. The absence of both, a maximum of thermal conductivity in the superconducting state, and the change of its slope at the superconducting transition temperature points to the validity of the two-band model that also describes the temperature dependence of specific heat. Measurements of thermoelectric power confirm the different normal-state character of the charge carriers of the investigated superconductors. Diffusion thermopower and phonon drag describe the measured data of all investigated compounds ov a wide range of temperature. The thermal expansion of HoNi2B2C below 10 K is dominated by the magnetic contribution. For all investigated substances the Grueneisen parameter features very large values in selected temperature ranges. In the case of MgB2, its temperature dependence is evidently connected with the properties of the relevant phonon mode. For the borocarbides, the electrical resistance depends very weakly on the crystallographic direction, but in contrast the thermal conductivity does in a quite strong manner. Despite of the antiferromagnetic phase transition in the case of HoNi2B2C, thermoelectric power and thermal expansion show minor anisotropy. / In der vorliegenden Arbeit werden Ergebnisse von Untersuchungen an polykristallinem MgB2 sowie an YNi2B2C- und HoNi2B2C-Einkristallen analysiert. Dafür erfolgten Messungen des spezifischen elektrischen Widerstands, der Wärmeleitfähigkeit, der Thermokraft und des linearen thermischen Ausdehnungskoeffizienten. Zudem wurde die spezifische Wärmekapazität polykristalliner Borkarbide bestimmt und aus den erhaltenen Daten die Temperaturabhängigkeit der Lorenz-Zahl und des Grüneisen-Parameters sowie mittels der Ehrenfest-Relation die Druckabhängigkeit der Sprungtemperatur ermittelt. Bei tiefen Temperaturen findet man im normalleitenden Zustand für alle betrachteten Substanzen ein charakteristisches Abweichen des Widerstands vom Bloch-Grüneisen-Gesetz. Bei HoNi2B2C tritt beim antiferromagnetischen Phasenübergang im Widerstand und in der Thermokraft ein reentrant-Verhalten auf. Die thermische Leitfähigkeit von MgB2 wird unterhalb von 7 K durch die Streuung der Phononen an Korngrenzen bestimmt. Das Fehlen eines Maximums in der Wärmeleitfähigkeit im supraleitenden Zustand und einer Anstiegsänderung bei der Sprungtemperatur liefert einen Hinweis auf die Gültigkeit des Zweibandmodells, mit welchem auch der Temperaturverlauf der Wärmekapazität erklärt werden kann. Messungen der Thermokraft bestätigen den unterschiedlichen Charakter der Ladungsträger im normalleitenden Zustand der untersuchten Supraleiter, wobei Elektronendiffusion und Phonon Drag die Messdaten aller betrachteten Verbindungen in weiten Temperaturbereichen beschreiben. Für HoNi2B2C wird die thermische Ausdehnung unterhalb von 10 K durch den Beitrag der magnetischen Ordnung bestimmt. Der Grüneisen-Parameter weist für alle untersuchten Substanzen in Teilbereichen sehr große Beträge auf. Sein Temperaturverlauf hängt bei MgB2 offenbar mit Eigenschaften der maßgeblichen Phononenmode zusammen. Für die Borkarbide ist die Richtungsabhängigkeit des elektrischen Widerstandes sehr schwach, in der Wärmeleitfähigkeit hingegen recht stark ausgeprägt. Abgesehen vom antiferromagnetischen Phasenübergang bei HoNi2B2C weisen Thermokraft und Ausdehnungskoeffizient eine geringe Anisotropie auf.

In the present study the results of investigations on polycrystalline MgB2 and on single crystals of YNi2B2C and HoNi2B2C are presented. In particular, measurementes of specific electrical resistance, thermal conductivity, thermoelectric power, and of the linear thermal expansion coefficient were performed. Moreover, the specific heat of polycristalline borocarbide samples was evaluated. From the measured data, the temperature dependencies of the Lorenz number and of the Grueneisen parameter can be determined, also the pressure dependence of the superconducting transition temperature using the Ehrenfest relation. At low temperatures a characteristic deviation of the resistivity from the Bloch-Grueneisen law in the normal state for all investigated substances was observed. A reentrant behaviour in resistivity and thermoelectric power occurs at the antiferromagnetic phase transition of HoNi2B2C. The thermal conductivity of MgB2 below 7 K is dominated by the scattering of phonons at grain boundaries. The absence of both, a maximum of thermal conductivity in the superconducting state, and the change of its slope at the superconducting transition temperature points to the validity of the two-band model that also describes the temperature dependence of specific heat. Measurements of thermoelectric power confirm the different normal-state character of the charge carriers of the investigated superconductors. Diffusion thermopower and phonon drag describe the measured data of all investigated compounds ov a wide range of temperature. The thermal expansion of HoNi2B2C below 10 K is dominated by the magnetic contribution. For all investigated substances the Grueneisen parameter features very large values in selected temperature ranges. In the case of MgB2, its temperature dependence is evidently connected with the properties of the relevant phonon mode. For the borocarbides, the electrical resistance depends very weakly on the crystallographic direction, but in contrast the thermal conductivity does in a quite strong manner. Despite of the antiferromagnetic phase transition in the case of HoNi2B2C, thermoelectric power and thermal expansion show minor anisotropy. / In der vorliegenden Arbeit werden Ergebnisse von Untersuchungen an polykristallinem MgB2 sowie an YNi2B2C- und HoNi2B2C-Einkristallen analysiert. Dafür erfolgten Messungen des spezifischen elektrischen Widerstands, der Wärmeleitfähigkeit, der Thermokraft und des linearen thermischen Ausdehnungskoeffizienten. Zudem wurde die spezifische Wärmekapazität polykristalliner Borkarbide bestimmt und aus den erhaltenen Daten die Temperaturabhängigkeit der Lorenz-Zahl und des Grüneisen-Parameters sowie mittels der Ehrenfest-Relation die Druckabhängigkeit der Sprungtemperatur ermittelt. Bei tiefen Temperaturen findet man im normalleitenden Zustand für alle betrachteten Substanzen ein charakteristisches Abweichen des Widerstands vom Bloch-Grüneisen-Gesetz. Bei HoNi2B2C tritt beim antiferromagnetischen Phasenübergang im Widerstand und in der Thermokraft ein reentrant-Verhalten auf. Die thermische Leitfähigkeit von MgB2 wird unterhalb von 7 K durch die Streuung der Phononen an Korngrenzen bestimmt. Das Fehlen eines Maximums in der Wärmeleitfähigkeit im supraleitenden Zustand und einer Anstiegsänderung bei der Sprungtemperatur liefert einen Hinweis auf die Gültigkeit des Zweibandmodells, mit welchem auch der Temperaturverlauf der Wärmekapazität erklärt werden kann. Messungen der Thermokraft bestätigen den unterschiedlichen Charakter der Ladungsträger im normalleitenden Zustand der untersuchten Supraleiter, wobei Elektronendiffusion und Phonon Drag die Messdaten aller betrachteten Verbindungen in weiten Temperaturbereichen beschreiben. Für HoNi2B2C wird die thermische Ausdehnung unterhalb von 10 K durch den Beitrag der magnetischen Ordnung bestimmt. Der Grüneisen-Parameter weist für alle untersuchten Substanzen in Teilbereichen sehr große Beträge auf. Sein Temperaturverlauf hängt bei MgB2 offenbar mit Eigenschaften der maßgeblichen Phononenmode zusammen. Für die Borkarbide ist die Richtungsabhängigkeit des elektrischen Widerstandes sehr schwach, in der Wärmeleitfähigkeit hingegen recht stark ausgeprägt. Abgesehen vom antiferromagnetischen Phasenübergang bei HoNi2B2C weisen Thermokraft und Ausdehnungskoeffizient eine geringe Anisotropie auf.