| Niobium, a 4d transition metal, has the highest superconducting transition temperature (Tc=9.2K) of any elemental superconductor as type II superconductor with coherent length, sigma approximately that of the penetration length, lambda. Pure niobium is grey in color and very soft, which makes this metal easily fabricable into different shapes for superconducting radio- frequency (SRF) cavities. Such cavities are used in some modern accelerators (SNS, CEBAF, XFEL), and are intended for usage in the next generation of particle accelerators, such as ILC. Since the crucial part of the cavities is top 100 nm of Nb near the inner cavity surface, considering the penetration depth is around 40 nm, it has attracted more and more attention in improving the surface process for optimizing the performance of the cavities. Nowadays, the main treatment of the Nb surface includes electro polishing (EP), buffered chemical polishing (BCP), high temperature baking (800 °C, 1000 °C and 1200 °C) and mild baking (120 °C). Firstly, the two half cells are welded together and the weld line is quite rough; there exists a lot of visible pits and defects on the inner shell of cavities.;In this Ph.D. thesis, novel techniques in a scanning transmission electron microscope (STEM) that can be used to analyze the atomic scale structure-property relationship, both at room tem- perature and high/LN 2 temperature, are explored. Specifically, by using correlated Z-contrast imaging and electron energy loss spectrum (EELS), the structure, composition and bonding can be characterized directly on the atomic scale, also, light atoms, like H, O and C, are visible in ABF images. For the examining the defect behavior on the cavity surface, heating and cold stages are involved to simulate the baking treatment and low-temperature environments. These studies will serve as an important reference for qualifying different surface treatments to further improve SRF cavities' performance.;The experimental results were obtained using JEOL JEM-ARM200CF STEM/TEM, having a cold-field emission gun and being operated at 200 kV. It is equipped with a probe-side Cs corrector, multiple imaging detectors (HAADF, LAADF, ABF, BF) and spectrometers (Gatan Infina EELS, Oxford Instruments XMAX EDS). This setup can achieve spatial resolution better than 70 pm and energy resolution 0.35 eV. Utilizing STEM imaging technologies, the crystal structure of Nb and even light impurities are visualized in HAADF and ABF images. Atomic- resolution EELS contains information about the local density of occupied states as the physical principle behind EELS relates to the interaction of the fast electrons with the sample to cause either collective excitations of electrons (plasmons), or discrete transitions between atomic energy levels.;The study for different Nb oxides establishes a set of methodologies to quantify the Nb cavity surface oxidation state based on low-loss/core-loss EELS. Oxygen K-edge split due to orbital hybridation and Nb-M peak chemical shift work well for identifying the Nb valence in oxide. Using this method, the surface oxidation state of Nb is studied, and the effects of oxygen diffusion during the mild baking process is revealed. I suggest that this diffusion may act as an important reason for the observed Q-slope in high field region. Considering that the SRF cavities are operated inside liquid helium vessels, the behavior of surface impurity at low temperature draws more and more attention. Since NbH is conducting material with a transition temperature of 150 K and hydrogen can easily concentrate near the surface, NbH is regarded as the key for the observed Q-disease at low temperature. But the difficulty of studying Nb hydride in a TEM is obvious: the light atom (for hydrogen, Z=1) is almost impossible to visualize in STEM images; the only hydrogen peak in EELS is the H K-edge which is located at 12 eV and it is easily covered by tail of zero-loss peak or plasmon peaks. The second part of my research starts with a study of different NbH superlattices using electron beam diffraction patterns, and then careful low-loss EELS measurements to identify hydrogen concentration at the Nb cavity surface. All of these results provide strong evidence for the existence of hydrogen near the cavity surface, the diffusion of hydrogen into bulk Nb atLN2 temperature, and the relationship between hydrogen segregation and local defects. The last part of the thesis focuses on the surface deformation caused by local strain. Local strain is a common problem of Nb cavity fabrication. Nb carbon layers and particles form at the cavity surface after strain tests, and inside of such particles, smaller dislocations are found which exhibit high strain center and higher oxygen concentration. It is clear that the impurities of light atoms is unavoidable during the cavity manufacturing process, oxide is the dominant impurity and it forms a distinguishable amorphous layer around 5 nm in thickness, hydrides are present following the oxide layer and can diffusion into Nb matrix more than 20 nm. Undoubtedly, these impurities will reduce the cavities' performance, and it will be necessary to find more effective methods for post-production cavity treatments to obtain a smoother and cleaner surface. Another problem, local strain, will effect the surface structure and introduce grain boundaries and other extended defects. Potentially, these defects may interact with surface impurities, correspondingly, the hydrogen segregation increases the mobility of the defects. Such positive correlation will accelerate the degeneration of the surface structure and finally lead to catastrophic effect on the local superconductivity.;In summary, various impurities of Nb are investigated with atomic resolution. Methodologies for quantifying Nb oxides and hydrides are developed. Direct observation of hydrogen atoms is realized in ABF images at room temperature, and can also serve as a promising method to identify different hydrides in Nb bulk at LN2 temperature if the cold stage is stable enough. My work on the local strain of Nb cavities points out that Nb carbides play a significant role in the performance of SRF cavities at low temperature and intermediate to high fields. |
