Measuring with high precision the electrical resistance of highly ordered natural graphite samples from a Brazil mine, we have identified a transition at ∼350 K with ∼40 K transition width. The steplike change in temperature of the resistance, its magnetic irreversibility and time dependence after a field change, consistent with trapped flux and flux creep, and the partial magnetic flux expulsion obtained by magnetization measurements, suggest the existence of granular superconductivity below 350 K. The zero-field virgin state can only be reached again after zero field cooling the sample from above the transition. Paradoxically, the extraordinarily high transition temperature we found for this and several other graphite samples is the reason why this transition remained undetected so far. The existence of well ordered rhombohedral graphite phase in all measured samples has been proved by x-rays diffraction measurements, suggesting its interfaces with the Bernal phase as a possible origin for the high-temperature superconductivity, as theoretical studies predicted. The localization of the granular superconductivity at these two dimensional interfaces prevents the observation of a zero resistance state or of a full Meissner state.

Thesis advisor: Stephen Wilson / The magnetic interaction in materials generally can be categorized into two extremes: localized and itinerant. This work will focus on the electronic and magnetic properties of two prototypical magnetic compounds, which fall into the opposite extremes, i:e:, the spin-orbit coupled Mott insulator Sr₂IrO₄ (Sr214) described by the localized Heisenberg model and the itinerant helical (nearly-ferromagnetic) metal MnSi pictured with band or Stoner magnetism. The single layered cuprate analogue Sr₂IrO₄ has attracted considerable attentions in recent years, due to its unusual electronic and magnetic properties and the potential to access superconducting states. The exotic jeff = 1/2 ground state for the Ir⁴⁺ (5d⁵) ions results from the delicate balance of competing/cooperating energy scales, such as the stronger spin-orbit coupling (SOC) in 5d materials as compared to 3d transition metal oxides (TMOs), crystal electric field (CEF) splitting and electron-electron correlations. Superconducting states are theoretically predicted to be achievable if sufficient carriers are introduced into this spin-orbit assisted compound, which later triggers tremendous experimental works toward the realization of superconductivity. Here in this work a combined study of various probes, such as transport, magnetization, X-ray and neutron scattering measurements, focusing on the electronic and magnetic properties, is presented in the perturbed spin-orbit coupled Mott (SOM) state. Specifically in electron doped (Sr₁₋ₓLaₓ)₂IrO₄, a detailed mapping of magnetism with respect to electron doping is presented, demonstrating the gradual transition from long range magnetic order in parent state, to intermediate short range order, and eventually into the incommensurate (IC) spin density wave (SDW) state with increasing electron doping. Our picture supports the conjecture that the quenched Mott phases in electron-doped Sr₂IrO₄ and hole doped La₂CuO₄ share common competing electronic phases. On the other hand, the prototypical itinerant metal MnSi is examined by inelastic neutron scattering (INS). Our experimental data directly demonstrate the collapse of linear spin wave theory for localized Heisenberg magnets in the large energy limit, although the low energy dispersion is still described by the ferromagnetic spin wave theory. Most importantly, our observations display the chimney-like dispersion spectrum up to the energy scale of at least 240 meV, which is more than one order of magnitude larger than the Heisenberg interaction energy scale. For the first time, solid characterizations of Stoner excitations in itinerant helimagnet (nearly ferromagnetic) have been demonstrated up to an exceedingly large energy scale. Our intriguing results will greatly promote further understanding and exploration of Stoner excitations in itinerant magnets. / Thesis (PhD) — Boston College, 2018. / Submitted to: Boston College. Graduate School of Arts and Sciences. / Discipline: Physics.

by Yu-Kit Lam =鉍系超導體在各製備階段之機械及超導特性 / 林宇傑. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2000. / Includes bibliographical references. / Text in English; abstracts in English and Chinese. / by Yu-Kit Lam = Bi xi chao dao ti zai ge zhi bei jie duan zhi ji xie ji chao dao te xing / Lin Yujie. / Table of Contents --- p.i / Acknowledgments --- p.iv / Abstract --- p.v / Chapter Chapter 1 --- Related Work on Bulk Bi-based High Tc Superconductor --- p.1 / Chapter 1.1 --- Historical Background of Superconductivity --- p.1 / Chapter 1.2 --- Basic Properties of Superconductivity --- p.4 / Chapter 1.3 --- Basic Properties of Bi-based Superconductor --- p.7 / Chapter 1.4 --- Fabrication Methods of Bi-based Superconductor --- p.12 / Chapter 1.4.1 --- Precursor Preparation --- p.12 / Chapter 1.4.1.1 --- Solid State Reaction Method --- p.12 / Chapter 1.4.1.2 --- Sol-gel Method --- p.15 / Chapter 1.4.1.3 --- Co-decomposition Method --- p.17 / Chapter 1.4.1.4 --- Freeze-drying and Spray-drying Methods --- p.17 / Chapter 1.4.1.5 --- Comparison for precursor preparation methods --- p.18 / Chapter 1.4.2 --- Pelletization and Sintering --- p.20 / Chapter 1.5 --- Potential applications of Bi-based superconductors --- p.22 / Chapter 1.5.1 --- Criteria for practical applications --- p.22 / Chapter 1.5.2 --- Superconducting tapes --- p.23 / Chapter 1.5.3 --- Current leads --- p.26 / Chapter 1.6 --- Objectives of the Project --- p.27 / Chapter 1.7 --- References --- p.28 / Chapter Chapter 2 --- Fabrication of Bulk Bi(Pb)-2223 Superconductor --- p.33 / Chapter 2.1 --- Introduction --- p.33 / Chapter 2.2 --- Precursor Preparation --- p.33 / Chapter 2.3 --- Grinding Process --- p.34 / Chapter 2.4 --- Pelletization Process --- p.35 / Chapter 2.5 --- The Sintering --- p.37 / Chapter 2.6 --- Characterizations --- p.38 / Chapter 2.7 --- References --- p.40 / Chapter Chapter 3 --- Principles and Instruments of Characterizations --- p.41 / Chapter 3.1 --- Scanning Electron Microscopy and Energy Dispersive X-ray Spectroscopy --- p.41 / Chapter 3.1.1 --- Basic Principle --- p.41 / Chapter 3.1.2 --- Sample Preparation --- p.42 / Chapter 3.2 --- Crystal Structure Determination Using X-ray Diffraction Spectroscopy --- p.44 / Chapter 3.3 --- Vibrating Sample Magnetometer --- p.48 / Chapter 3.3.1 --- Basic Principle --- p.48 / Chapter 3.3.2 --- Sample Preparation --- p.49 / Chapter 3.4 --- Standard Four-Probe Method for Electrical Measurement --- p.51 / Chapter 3.5 --- Density Measurement of Sintered Samples --- p.52 / Chapter 3.6 --- Hardness Tests --- p.54 / Chapter 3.7 --- Determination of Flexural Strength of Sintered Samples --- p.56 / Chapter 3.8 --- References --- p.57 / Chapter Chapter 4 --- Results and Discussions / Chapter 4.1 --- Results from X-Ray Diffraction Spectroscopy --- p.58 / Chapter 4.1.1 --- Green Pellet --- p.58 / Chapter 4.1.2 --- 50-Hour Sintered Pellet --- p.58 / Chapter 4.1.3 --- "100-Hour, 150-Hour, and 200-Hour Sintered Pellets" --- p.59 / Chapter 4.1.4 --- Volume Fraction of the High Tc Phase --- p.59 / Chapter 4.2 --- Microstructure Observed by Scanning Electron Microscopy --- p.63 / Chapter 4.2.1 --- Green Pellet --- p.63 / Chapter 4.2.2 --- 50-Hour Sintered Pellet --- p.64 / Chapter 4.2.3 --- "100-Hour, 150-Hour, and 200-Hour Sintered Pellets" --- p.64 / Chapter 4.3 --- Chemical Composition Using Energy Dispersive X-ray Spectroscopy --- p.68 / Chapter 4.4 --- Results from Vibrating Sample Magnetometer --- p.71 / Chapter 4.5 --- Densification of Sintered Samples --- p.75 / Chapter 4.6 --- Hardness at Various Stages of Processing --- p.77 / Chapter 4.7 --- Flexural Strength at Various Stages of Processing --- p.79 / Chapter 4.8 --- I-V Characterization Using Standard Four-Probe Method --- p.82 / Chapter 4.9 --- Weibull Modulii of Sintered Samples --- p.85 / Chapter 4.10 --- Future Oultlook --- p.86 / Chapter 4.11 --- References --- p.87 / Chapter Chapter 5 --- Summary --- p.89 / Appendix A Polishing of Pelletizing Mold / Chapter A.1 --- Introduction --- p.92 / Chapter A.2 --- Grinding Process --- p.92 / Chapter A.3 --- Final Polishing Process --- p.93

自從 Onnes 于1911 年發現超導現象以來，超導就一直是凝聚態領域非常熱門的一個課題。隨之而來的一個問題是超導在量子尺寸效應的影響下將如何變化。在1959 年，Anderson 提出了一個超導受尺寸影響而消失的判據：當超導體的尺寸足够小以至於超導體費米面附近電子的平均能隙大於超導能隙或與其相當時，超導便被尺寸效應破壞。基於這個判據，超導和費米面附近的電子態密度密切相關。Si(111)表面上生長的鉛島在調製費米面附近的態密度上是一個很好的系統，因為它既可以在垂直方向上通過量子阱態調節，也可以通過水平方向的尺寸限制來調節。另外，相對於其他系綜或者粉末超導體，在Si(111)表面上生長的單個鉛島系統上研究超導排除了諸如尺寸分佈，顆粒間相互耦合以及相位漲落等因素對於超導的影響。 / 在這篇論文的緒論中，我首先簡單介紹了基本的超導知識，如 BCS 理論，Eliashberg 理論以及超導在超導體-絶緣體-正常金屬形成的隧道結上的表現形式。跟著，我重點回顧了之前在系綜超導體以及金屬納米結構中進行的超導尺寸效應研究。對於目前廣泛研究的鉛島系統，我將重點談及最近發現的贗能隙，這對研究鉛島的超導至關重要。 / 在第二章，我簡單介紹了樣品的生長和掃描隧道譜的相關知識。爲了分析鉛島的超導譜，我們用了兩種方法去分析他們。一種是零電壓下電導的方法，另一種是超導譜分析方法。在這章的最後，我詳細介紹了Dynes 方程及去捲積的方法。 / 在第三章，我將介紹我博士學習期間一個非常重要的工作，提高儀器的能量分辨率。通過改造儀器結構，合理的接地，屏蔽射頻噪聲，以及清除電壓源的噪聲，我成功地將能量分辨率從0.9 meV 提高到0.2 meV。在最後我會將儀器改進后的結果與之前的結果儀器與其他組的結果進行比較。 / 在儀器改進之前，我們發現那時的測量結果非常差，由此得出的結論也是不正確的。爲了比較儀器改造的重要性，在第四章，我將簡單介紹儀器改進前的結果。在當時差的條件下，我們探測出對於9ML 厚的鉛島，3.2 K 以上不超導的鉛島尺寸，大約為30 nm²。並且鉛島經歷了一個從強電子聲子耦合到弱電子聲子耦合的轉變。 / 在儀器改進之後，我們不僅糾正了之前在九層鉛島上進行超導研究時的一些結論。此外，也觀察到了由於尺寸變化或者費米面上態密度變化導致超導的細微區別。由於尺寸效應，我們發現在一些小的鉛島上存在一個過渡區。另外，由於八層鉛島費米面上的態密度比九層的高，超導轉變溫度也因此有一個系統性的提高。對於這兩個層數的鉛島，他們的超導轉變溫度都隨尺寸減小受到一個緩慢的抑制。對於非常小的鉛島，我們發現其仍然超導。這和Anderson 判據的預期以及其他實驗結果不一致，激發我們進一步探索是否非晶化的潤濕層參與了這種非常小的鉛島的超導。 / 這些工作，對於全面理解超導的尺寸效應以及態密度影響是非常基本和關鍵的，這也將進一步激發人們在這個領域進行更多的探索。 / Superconductivity has always been a hot topic in the field of condensed matter physics since its discovery by Onnes in 1911. How the superconductivity was affected by size attracted much attention especially after P. W. Anderson proposed a criterion of the breakdown of superconductivity in 1959, where the superconductors will lose their superconductivity when the energy level spacing at Fermi level (E[subscript F]) is comparable to or larger than the superconducting energy gap. As stated in the criterion, the superconductivity correlates greatly with the density of states (DOS) at E[subscript F] within the superconducting gap. The system of individual Pb islands grown on Si(111) provides an ideal platform to modulate the DOS at EF through both the quantum size confinement and the quantum well states (QWS) effects. Moreover, this system excludes the problems of size distribution, couplings among particles and phase fluctuation of the previously studied ensembles of particles. / In my thesis, I first introduce briefly the basic knowledge of superconductivity, such as BCS theory and Eliashberg theory, as well as its behaviors in a normal metal-insulator-superconductor tunneling junction. Then the study of superconductivity by quantum size effect on ensemble superconductors and metallic nanostructures is reviewed. For the widely studied system of Pb islands, I discuss in more detail the recently discovered pseudogap which was important and critical for analyzing the superconductivity. / In chapter 2, the knowledge of sample growth is given and a simple introduction to scanning tunneling spectroscopy is presented. To study the superconductivity spectra of Pb islands, we use two methods to analyze them, one the zero bias conductance (ZBC) method and the other the superconductivity spectrum analysis. In the end of this chapter, Dynes function and deconvolution procedure are introduced in detail. / In chapter 3, I introduce one of my important works in my Phd study, to improve the instrumental energy resolution. By reconstructing the instrumental structure, grounding properly, shielding RF noise, and cleaning the voltage gap source, the instrumental energy resolution has been improved greatly from ~0.9 meV to ~0.2 meV. I compare our current results both with previous results and results from other groups. / Before the instrumental improvement, we find that the measurements were very poor and the conclusion thus obtained were incorrect. To show the importance of the instrumental improvement, I introduce briefly the previous work in chapter 4. Under the poor instrumental condition, we found that the limiting size of superconductivity above 3.2 K was determined to be ~30 nm² for 9 ML thick Pb islands and that Pb island superconductors undergo a change from strong to weak electron-phonon coupling. / After the instrumental improvement, we not only correct some conclusions of the previous studies on superconductivity of 9 ML Pb islands, but also observed the more non-trivial variation of superconductivity from the change of island size or density of state (DOS) at Fermi level (E[subscript F]) by the quantum well states (QWS). A critical regime is observed for small Pb islands. As the DOS of 8 ML Pb islands at E[subscript F] is larger than that of 9 ML Pb islands, the transition temperatures (T[subscript C]) of 8 ML Pb islands hold a systematic difference larger than those of 9 ML Pb islands. The T[subscript C] results for both 8 ML and 9 ML Pb islands follow the same gradual suppression and the ratio 2△(0)/k[subscript B]T[subscript C] remains unchanged by the size effect. Further study indicates that for very small 8 ML and 9 ML Pb islands they are still superconducting, inconsistent with the Anderson criteria and other experimental results. This observation suggests a possible role of wetting layer on superconductivity of these small Pb islands. / This work, I believe, is fundamentally interesting and beneficial to understand deeply the phenomena of superconductivity modulated by size effect and DOS change at E[subscript F] and will inspire more future studies in this field. / Detailed summary in vernacular field only. / Detailed summary in vernacular field only. / Detailed summary in vernacular field only. / Detailed summary in vernacular field only. / Detailed summary in vernacular field only. / Detailed summary in vernacular field only. / Detailed summary in vernacular field only. / Liu, Jiepeng = 掃描隧道譜研究Si(111)表面上單個鉛島的超導尺寸效應及態密度影響 / 羅杰鵬. / Thesis (Ph.D.)--Chinese University of Hong Kong, 2012. / Includes bibliographical references (leaves 136-144). / Electronic reproduction. Hong Kong : Chinese University of Hong Kong, [2012] System requirements: Adobe Acrobat Reader. Available via World Wide Web. / Abstract also in Chinese. / Liu, Jiepeng = Sao miao sui dao pu yan jiu Si(111) biao mian shang dan ge qian dao de chao dao chi cun xiao ying ji tai mi du ying xiang / Luo Jiepeng. / Chapter 1 --- Superconductivity affected by quantum size effect --- p.2 / Chapter 1.1 --- Overview --- p.3 / Chapter 1.2 --- Basic theories to superconductivity --- p.4 / Chapter 1.2.1 --- BeS theory --- p.5 / Chapter 1.2.2 --- Eliashberg equation --- p.8 / Chapter 1.2.3 --- Superconductivity of S-I-N tunneling junction --- p.10 / Chapter 1.3 --- Size effect of superconductivity for ensemble or powder superconductors --- p.12 / Chapter 1.3.1 --- Anderson criteria --- p.13 / Chapter 1.3.2 --- Size-dependent T[subscript C] for different superconductors --- p.13 / Chapter 1.4 --- Size effect of superconductivity for metallic nanostructures --- p.17 / Chapter 1.4.1 --- Metallic nanostructures --- p.17 / Chapter 1.4.2 --- Quantum well states of metallic nanostructures --- p.18 / Chapter 1.4.3 --- Pb nanostructures on Si(111)-7 x 7 --- p.20 / Chapter 1.5 --- summary --- p.25 / Chapter 2 --- Experimental introductions and data analysis methods --- p.26 / Chapter 2.1 --- Experimental introduction --- p.27 / Chapter 2.1.1 --- Growth of Pb islands --- p.28 / Chapter 2.1.2 --- Substrates effects --- p.32 / Chapter 2.2 --- STS studies of Pb islands --- p.36 / Chapter 2.2.1 --- Basic knowledge of STS --- p.36 / Chapter 2.2.2 --- STS results of Pb islands --- p.40 / Chapter 2.3 --- Data analysis methods --- p.41 / Chapter 2.3.1 --- Zero bias conductance analysis --- p.41 / Chapter 2.3.2 --- Superconductivity spectrum analysis --- p.43 / Chapter 2.4 --- Dynes function fitting --- p.44 / Chapter 2.4.1 --- Dynes function --- p.44 / Chapter 2.4.2 --- Deconvolution --- p.47 / Chapter 2.4.3 --- BCS-like analysis --- p.49 / Chapter 2.5 --- Summary --- p.50 / Chapter 3 --- Instrument improvements --- p.51 / Chapter 3.1 --- Previously existed problems --- p.52 / Chapter 3.2 --- Problem analysis and solutions --- p.54 / Chapter 3.2.1 --- Structure and Preamplifier --- p.54 / Chapter 3.2.2 --- Grounding --- p.56 / Chapter 3.2.3 --- Bias voltage source cleaning --- p.57 / Chapter 3.2.4 --- RF noise shielding --- p.60 / Chapter 3.3 --- Tip drift in perpendicular direction when taking STS --- p.65 / Chapter 3.4 --- Improved results --- p.68 / Chapter 3.4.1 --- Comparisons with previous results --- p.68 / Chapter 3.4.2 --- Comparisons with other groups --- p.69 / Chapter 3.5 --- Summary --- p.72 / Chapter 4 --- Superconductivity of 9 ML thick Pb islands with poor energy resolution --- p.75 / Chapter 4.1 --- STS results --- p.76 / Chapter 4.1.1 --- STS results at large energy scale --- p.76 / Chapter 4.1.2 --- STS results at small energy scale Zero bias conductance analysis --- p.79 / Chapter 4.2.1 --- ZBC results --- p.79 / Chapter 4.2.2 --- Comparisons with theoretical calculations --- p.83 / Chapter 4.3 --- Superconductivity spectrum analysis --- p.85 / Chapter 4.3.1 --- Method to obtain superconductivity spectra --- p.86 / Chapter 4.3.2 --- BCS-like analysis --- p.93 / Chapter 4.4 --- Explanation and possible mechanism --- p.97 / Chapter 4.5 --- Summary --- p.99 / Chapter 5 --- DOS modulated superconductivity with improved energy resolution --- p.101 / Chapter 5.1 --- Introduction --- p.102 / Chapter 5.2 --- Experiments --- p.103 / Chapter 5.3 --- Behaviors of zero bias conductance results --- p.104 / Chapter 5.3.1 --- Power law behavior --- p.104 / Chapter 5.3.2 --- Critical regime and To determination --- p.106 / Chapter 5.4 --- Recheck previous results --- p.112 / Chapter 5.4.1 --- Pseudogap --- p.112 / Chapter 5.4.2 --- Transition temperature --- p.115 / Chapter 5.5 --- DOS modulated superconductivity --- p.121 / Chapter 5.5.1 --- Quantum well states of 8 ML and 9 ML Pb islands --- p.121 / Chapter 5.5.2 --- T[subscript C] behavior on a 8 ML and 9 ML Pb island --- p.123 / Chapter 5.5.3 --- Superconductivity behaviors for a set of 8 ML and 9 ML Pb islands --- p.124 / Chapter 5.5.4 --- Superconductivity of very small Pb islands --- p.129 / Chapter 5.6 --- Summary --- p.130 / Chapter 6 --- Conclusions and outlook --- p.132 / Chapter 6.1 --- Conclusions --- p.133 / Chapter 6.2 --- Outlook --- p.134 / Bibliography --- p.136

Unconventional superconductors are those which are not described by the BCS theory, and for which no known theoretical description currently exists. The careful study of the behaviour of superconducting vortices in such systems yields crucial insights into the underlying physics of these exciting materials. This thesis describes a series of magnetometry experiments conducted on three different unconventional superconductors: Sr2RuO4, MgB2 and Bi2Sr2CaCu2O8+; utilising two techniques: Scanning Hall probe microscopy and magneto-optical imaging. An exotic p-wave chiral order parameter is thought to exist in Sr2RuO4 and is expected to produce several identifiable magnetic signatures. A search for these signals via scanning Hall probe measurements failed to detect any such signatures, but did capture a structural transition of the vortex lattice that is consistent with the proposed chiral order parameter. Studies of several samples also suggest that the vortex behaviour is strongly modified with even tiny amounts of disorder, a conclusion that has important consequences for interpretations of vortex patterns in Sr2RuO4. Several recent experiments have reported vortex configurations consistent with a competing short-range repulsion and long-range attraction in the intervortex interaction in MgB2 single crystals. We observe the spontaneous formation of vortex chains and labyrinths in a 160nm MgB2 thin-film that are suggestive of a non-monotonic vortex interaction, but perhaps more indicative of an intermediate-range attraction in harness with short and long-range repulsions. The suitability of seven potential mechanisms of vortex attraction in MgB2 are reviewed in light of the unusually short electronic mean-free path of our sample. Finally, magneto-optical imaging has been used to study the penetration of flux into regular polygon-shaped Bi2Sr2CaCu2O8+ platelets with various geometries. The variation of HP with geometry qualitatively contradicts conventional estimates of demagnetisation factors based on equivalent ellipsoids using inscribed circles. This work has important implications for the estimation of appropriate effective demagnetisation factors in arbitrarily shaped superconducting bodies.

This thesis is composed of three projects including the AC magnetic susceptibility study of high-temperature superconductor YBa$_2$Cu$_3$O$_{7-\delta}$, the ionic-liquid gating study of the Mott insulator Sr$_2$IrO$_4$, and the single-electron study of quantum dot device with self-assembled nanocrystal PbS. Chapter 1 covers a general introduction to all three projects. The basic background and the motivation for each project are presented. Project I is covered in Chapter 2, Chapter 3, and Chapter 4. The first part of Chapter 2 is a theoretical introduction to the Bardeen-Cooper-Schrieffer theory of superconductivity with its main conclusions presented. This chapter builds a basis for the use of high pressure technique to YBa$_2$Cu$_3$O$_{7-\delta}$ in the later chapters. The rest of Chapter 2 reviews the work in the study of high-temperature superconductors, especially on YBa$_2$Cu$_3$O$_{7-\delta}$, on both experiments and theories and the possible applications of high-temperature superconductors. Chapter 3 introduces the YBa$_2$Cu$_3$O$_{7-\delta}$ sample preparation process and the characterisation. A dry cryomagnetic equipment was employed for the measurement. The results and the discussion are presented in Chapter 4. Project II is described in Chapter 5, Chapter 6, and Chapter 7. Chapter 5 firstly introduces the background knowledge of the gated material SrTiO$_3$ and the technical details of the ionic-liquid gating technique. Then the sample growth and the characterisation are presented. The fabrication process of Sr$_2$IrO$_4$ and SrTiO$_3$ (material for a control experiment) are described in Chapter 6. Chapter 7 covers the measurement and the result of the fabricated devices and related discussion. Project III ranges from Chapter 8, and Chapter 9. A literature review of quantum-dot devices and self-assembled nanocrystals is presented in Chapter 8. The experimental design of this nanocrystal quantum dot device is also included. Following it, the fabrication process of quantum-dot devices and the techniques used for fabrication are introduced in the start of Chapter 9. Chapter 9 also gives a description of the probe-station for measurements. The results and discussion of the measurements are covered in the last section of Chapter 9. Chapter 10 summarises and concludes the three projects stated above and gives some suggestions about the directions for future work.

Intercalation is known to be an efficient method for tuning the band structure of layered materials to bring out superconductivity, without significantly altering the crystal structure of the host material. Graphite intercalation compounds and intercalated transitional metal dichalcogenides (TMDs) are two most studied representatives. This thesis presents an experimental study of several new superconductors obtained by intercalation of layered materials, including MoS2, black phosphorus and a topological insulator Bi2Se3. Polymorphism is an essential feature of MoS2. While, superconductivity in doped 2H-MoS2 has been extensively studied. Superconductivity in its 1T and 1T' counterparts has been neither observed, nor even predicted theoretically. In this thesis, we have investigated potassium (K)-intercalated MoS2 and found that doping with K induces both structural and superconducting phase transitions. We demonstrate that all three phases of MoS2 - 2H, 1T and 1T'- become superconducting as a result of intercalation, with critical temperature Tc of 6.9 K, 2.8 K and 4.6 K, respectively. Black phosphorus has been 'rediscovered' in the last few years due to its layered structure and unique electronic properties. This thesis describes successful intercalation of black phosphorus with several alkali metals (Li, K, Rb, Cs) and alkaline earth metal Ca, with all five compounds showing superconductivity. Importantly, and very unexpectedly, the found superconductivity of intercalated black phosphorus is independent of the intercalant, with all five compounds having exactly the same superconducting characteristics (Tc, critical fields, anisotropy). We suggest that the superconductivity is due to heavily doped phosphorene layers, with alkali metal atoms acting mainly as charge reservoirs. Superconducting topological insulators, such as Bi2Se3, are regarded as the most promising candidates for topological superconductivity. However, the nature of superconductivity in doped Bi2Se3, such as CuxBi2Se3, SrxBi2Se3 and NbxBi2Se3, remains controversial and so far no convincing evidence of topological superconductivity has been reported for these materials. In this thesis, we report superconductivity in a new family of superconductors derived from Bi2Se3, by intercalation with K, Rb and Cs metals. All three superconductors exhibit qualitatively identical but highly anomalous behaviour of magnetisation, with several new features consistent with the properties of topological superconductors. Specifically, the new materials exhibit a highly unusual extra diamagnetic screening in the Meissner state and two coexisting superconducting phase, including surface superconductivity that we attribute to heavily doped surface states of the original topological insulator (Bi2Se3). This work provides a new platform in the study of the interplay between the topological and superconducting orders. In conclusion, superconductivity has been induced in MoS2, black phosphorus and Bi2Se3 through alkali or alkaline earth metal intercalation. The study of these new superconducting materials has been summarised in the thesis.

Zhao Kun. / Thesis (Ph.D.)--Chinese University of Hong Kong, 2001. / Includes bibliographical references. / Electronic reproduction. Hong Kong : Chinese University of Hong Kong, [2012] System requirements: Adobe Acrobat Reader. Available via World Wide Web. / Mode of access: World Wide Web. / Abstracts in English and Chinese. / Zhao Kun.

Orientador: Rafael Zadorosny / Banca: Fernando Rogerio de Paula / Banca: Fauze Ahmad Aouada / Banca: Maycon Motta / Banca: César Vanderley Deimling / Resumo: Neste trabalho será apresentado o estudo da preparação de filmes supercondutores do sistema BiSrCaCuO. A partir de um pó adquirido comercialmente com composição nominal Bi 1.8 Pb 0.4 Sr 2 CaCu 2 O x, foi preparado um filme tratado termicamente a 800oC (B12CM800) por 7 minutos. Outro filme usando um pó de composição semelhante, produzido pelo método de Pechini modificado para este fim, foi preparado e tratado termicamente a 810oC (B12SM810) durante 7 minutos em forno de micro-ondas. Também foi produzido pelo método de Pechini, um pó de composição nominal Bi 1.8 Pb 0.4 Sr 2 Ca 2 Cu 3 O x, o qual foi utilizado na preparação de outros três filmes tratados termicamente a 780oC (B23SM780), 810oC (B23SM810) e 840oC (B23SM840), durante 10, 5 e 5 minutos, respectivamente. Os filmes foram crescidos sobre um substrato cristalino de LaAlO 3 (100) e tratados termicamente em um forno de micro-ondas doméstico (2.45 GHz, 1200 W) devidamente adaptado para esta finalidade. As propriedades estruturais foram estudadas utilizando as técnicas de difração de raios-X, DRX, e a microscopia eletrônica de varredura, MEV. A técnica de DRX indicou a formação da fase 2212 nos filmes B12CM800, B12SM810, B23SM780 e B23SM810, assim como o surgimento da fase 2201 e de fases agregadas, Ca 2 PbO 4 e Bi 2 CaO 4 . O filme B23SM840 apresentou, além das fases 2212 e secundárias, também a fase 2223. A técnica de MEV indicou a formação de estruturas na forma de placas crescidas em camadas, típicas do material em estudo, além da formação de estruturas superficiais ricas em Ca em todos os filmes, exceto para o B23SM840, que apresentou apenas a formação de placas. Utilizando a técnica de energia dispersiva de raios-X, EDX, foi possível verificar uma provável composição nominal dos filmes correspondente à fase 2223 para o filme B23SM840 e 2212 para os demais. As medidas elétricas foram feitas utilizando o método de quatro pontas, possibilitando... / Abstract: In the present work, the preparation of superconducting films of the BSCCO system will be presented. From a commercially available powder with nominal composition Bi 1.8 Pb 0.4 Sr 2 CaCu 2 O x, a film was prepared and heat-treated at 800°C (B12CM800). Powder with a similar composition was produced by the Pechini method modified for this purpose and a film heat-treated at 810oC (B12SM810) was them prepared. Also produced by Pechini method, a powder with nominal composition Bi 1.8 Pb 0.4 Sr 2 Ca 2 Cu 3 O x was used to prepare other three films thermally treated at 780oC (B23SM780), 810oC (B23SM810) and 840oC (B23SM840). The films were grown on crystalline substrates of LaAlO 3 (100) and thermally treated in a domestic microwave oven (2.45 GHz, 1200 W) adapted suitably for this purpose. The structural properties were studied using X-ray diffraction techniques, XRD, and scanning electron microscopy, SEM. The XRD technique indicated the formation of the 2212 phase in the B12CM800, B12SM810, B23SM780 and B23SM810 films, as well as the appearance of the 2201 phase and the following secondary phases: Ca 2 PbO 4 and Bi 2 CaO 4 . The film B23SM840 also indicated the formation of 2223 besides the 2212 phase and aggregates. The SEM technique presented the formation of structures with plate shape, typical of this material, and a superficial formation of structures rich in Ca on all the films, except for the B23SM840 film, which showed only the formation of plates. The energy dispersive X-rays technique, EDX, was carried out to verify a likely nominal composition of the films corresponding to 2223 phase for the B23SM840 film and 2212 phase for the others. The electrical measurements were made using the four-probe method, enabling the identification of the critical transition temperatures, T c, T c-onset, T c- midpoint and T c-offset, also the determination of the critical current density, J c . All films shown a characteristic T c of the 2212 ... / Doutor

Os compostos \'LN IND.2\'\'CU\'\'O IND. 4-Y\' (\'LN\'= \'PR\', \'ND\', \'SM\', \'EU\') apresentam supercondutividade quando o lantanídeo (\'LN\') é parcialmente substituído por \'CE\' ou \'TH\' e em seguida são submetidos a um tratamento térmico de redução para a remoção de uma pequena quantidade de oxigênio da estrutura. Desta forma, compostos policristalinos \'LN IND. 2-x\'\'M IND.X\'\'CU\'\'O IND.4-Y\' (\'LN\'= \'PR\', \'ND\', \'SM\', \'EU\'; \'M\' = \'CE\', \'TH\'; 0 \'< OU =\' X \'< OU =\' 0,20) foram preparados a partir de precursores sol-gel. A vantagem desta técnica de preparação é que os tratamentos térmicos são feitos em temperaturas abaixo da tempertura eutética, evitando a presença de uma fase líquida durante a sinterização dos materiais em estudo. A investigação da cinética de formação destes compostos foi feita através de medidas de difração de raios X e análise térmica diferencial e mostrou que os materiais preparados por processo sol-gel apresentam uma distribuição homogênea dos cátions. As propriedades supercondutoras foram investigadas através de medidas de magnetização e resistência elétrica em diversas amostras e uma ênfase foi dada às séries de \'EU IND. 2-X\'\'CE IND. X\'\'CU\'\'O IND. 4-Y\' (0 \'< OU =\' X \'< OU =\' 0,18) e o desaparecimento da supercondutividade em \'(\'SM IND. 1-X\'\'EU IND. X\') IND. 1,85\'\'CE IND. 0,15\'\'CU\'\'O IND. 4-Y\' (0 \'< OU =\' X \'< OU =\' 1). Os resultados foram interpretados a partir da adoção de um modelo de supercondutividade granular. As propriedades estruturais foram analisadas em mais de 50 amostras desta família de óxidos através de medidas de difração de raios X. O refinamento de estrutura pelo método de Rietveld permitiu concluir que a introdução de portadores em \'LN IND. 2-x\'\'M IND.X\'\'CU\'\'O IND.4-Y\' (\'LN\'= \'PR\', \'ND\', \'SM\', \'EU\'; \'M\' = \'CE\', \'TH\'; 0 \'< OU =\' X \'< OU =\' 0,20) ocorre através da substituição parcial do lantanídeo por \'CE\' ou \'TH\' e influencia diretamente as distâncias das ligações entre \'CU\' e \'O\'nos planos de \'CU\'\'O IND. 2\', responsáveis diretos pelas propriedades supercondutoras nesta família de óxidos supercondutores. / Polycrystalline samples of \'LN IND.2\'\'CU\'\'O IND. 4-Y\' (\'LN\'= \'PR\', \'ND\', \'SM\', \'EU\') exhibit superconductivity when subject to two different steps: i) substitution of \'CE\' or \'TH\' for the Ln element in the Ln2Cu04-y T\' phase parent compound; and ii) reduction of the resultant material. Polycrystalline samples of \'LN IND. 2-x\'\'M IND.X\'\'CU\'\'O IND.4-Y\' (\'LN\'= \'PR\', \'ND\', \'SM\', \'EU\'; \'M\' = \'CE\', \'TH\'; 0 \'< OR =\' X \'< OR =\' 0,20) were prepared through a sol-gel precursor. This chemical route was employed for producing homogeneous, pure, and microstructurally controlled ceramics at sufficiently low sintering temperatures, below the eutectic temperature. The kinetics of the phase formation was studied by x ray powder diffraction and thermal analysis. These results showed that all samples are homogeneous under the cationic point of view. Measurements of electrical resistance and magnetic susceptibility were performed mostly on polycrystalline samples belonging to the frontier where superconducting properties are suppressed in this family as \'EU IND. 2-X\'\'CE IND.X\'\'CU\'\'O IND. 4-Y\' (0 \'< OR =\' X \'< OR =\' 0,18) and \'(\'SM IND. 1-X\'\'EU IND. X\') IND. 1,85\'\'CE IND. 0,15\'\'CU\'\'O IND. 4-Y\' (0 \'< OR =\' X \'< OR =\' 1). The results were discussed within a superconducting granular scenario. Over 50 compounds of this family of oxides were characterized by x ray powder diffraction and all diffractograms were refined through Rietveld analysis. The results revealed that carriers are injected into \'CU\'\'O IND. 2\' planes through a partial substitution of \'CE\' or \'TH\' for the \'LN\' in \'LN IND. 2-x\'\'M IND.X\'\'CU\'\'O IND.4-Y\' (\'LN\'= \'PR\', \'ND\', \'SM\', \'EU\'; \'M\' = \'CE\', \'TH\'; 0 \'< OR =\' X \'< OR =\' 0,20). The dopings are accompanied by an expansion of the \'CU\'-\'O\' bond length within the \'CU\'\'O IND. 2\' planes, an essential feature for the appearance of superconductivity in these series.