An Innovative Cylindrical magnetron sputtering source for the deposition of HIE-ISOLDE superconducting Nb/Cu QWRs – Daniel Adrien Franco Lespinasse PhD Thesis

Author: Daniel Adrien Franco Lespinasse; Type of thesis: PhD Thesis
Abstract: In the framework of Eucard project, it has been carried out, in collaboration with CERN, the R&D on magnetron sputtering deposition on the HIE-ISOLDE cavity geometry, as an alternative method to deposit niobium thin films. In this research a new magnetron configuration source was tested at the National Institute of Nuclear Physics (INFN-LNL), in order to deposit a uniform niobium thin film onto copper superconducting Quarter Wave Resonator cavities. The methodology was divided in three. A first part, in which a test dummy cavity and a test cathode were used in order to deposit stainless steel onto copper quartz. The purpose of the use of steel has been finding the right parameters of sputtering and also to analyze the uniformity of the film. In this first phase it have been tested several magnetic confinements, which allowed the optimization of the deposition. In parallel it was performed the deposition of stainless steel onto copper strips, to realize the stripping test as a method to analyze the uniformity of the film. The second part was focused on the deposition of niobium thin film onto quartz samples placed along the resonator to improve the superconducting properties, specifically Residual Resistivity Ratio (RRR) and Critical Temperature (Tc); nevertheless other magnetic confinements were tested to maintain the uniformity of the coating. It was studied the influence on superconducting properties of two principal parameters of the sputtering process: the power and the substrate temperature. After setting the deposition parameters, a definitive magnetron confinement was used to deposit the real copper QWR. The RF performance was also measured after the design, construction and installation of a test cryostat. Finally, it was found the magnetic source to deposit a niobium thin film uniformly over QWR cavities. Increasing the substrate temperature and the sputtering power, the transition temperature of the niobium thin film was around 9,3K and it was obtained a maximum RRR of 61. Only 30 min were necessary to deposit the film with a uniformity of 2±1 μm along the cavity. SEM results allowed to analyze the microstructure of the niobium film. Bigger grains were founds on the inner conductor closer to the magnetron source. In addition a test cryostat was successfully built in order to measure the RF performance; the system can be useful to perform measurements at 4.2 and 1.8 K. Respect to the RF performance the first Nb/Cu cavity is under the specifications of CERN with a maximum Q value of 2e8 and an accelerating field of 2MV/m; however this first result is extremely important to start with the optimization phase. Some parameters will be changed in order to improve the performance and push the SRF community to use the magnetron sputtering technique as an economical method to deposit superconducting cavities in short times.

Industrial R&D on Innovative Surface Treatments for an Ecological Descaling of “Acciaierie Valbruna” Stainless Steel Wire Rods in Replacement of the Traditional Acid Etching – Vlada Pastushenko PhD Thesis

Author: Vlada Pastushenko; Type of thesis: PhD Thesis
Abstract: This work deals with an industrial research on ecological innovative descaling treatments for stainless steels, in substitution of the acid etching process: from the study and the research on samples, the most efficient techniques and their application to industrial purpose are explained. The research has basically covered the study of two pre-finishing treatments (high pressure water blasting and “dry ice”-blasting) and two etching treatments (electropolishing with ionic liquids and in aqueous media). In the field of stainless steels, the surface oxide of iron Fe (III) is combined with the multiple elements added to alloys in order to increase their characteristics (carbon, chromium, nickel and other). Moreover, the surface oxide is presented as a layer very tenacious and compact. In addition, heat treatment leads to the formation of a layer without chromium more readily attacked by oxygen from the atmosphere. Surface treatments are required to remove the surface oxide and recover the
chromium layer. The chemical pickling, that is one of the most common etching processes, depends on many factors, such as the size of the pieces, the type of plant, the type of alloy et al. In general, the traditional solutions contain from 10% to 20% by weight of nitric acid, and 1% to 5% by weight of hydrofluoric acid. The oxidizing environment is provided by nitric acid, which effectively removes the oxide surface, and is subsequently used without the hydrofluoric acid to restore the passive layer (passivation). From the environmental point of view, however, the use of this reagent is very costly:
• Air pollution: the formation of nitrogen oxides (NOx) during the process causes fumes and vapours. These gases are harmful to health, highly polluting (production of acid rain) and extremely aggressive towards metals.
• Water pollution: the high concentration of nitrates and nitrites is one of the causes of eutrophication. In particular, nitrites may form carcinogenic compounds such as nitrosamines, which can enter the food chain through fish.
• Health and safety: hydrofluoric acid is highly corrosive and a poison. It should be handled with extreme attention, using protective equipment and safety precautions. Once absorbed into the blood through the skin, it reacts with blood calcium and may cause cardiac arrest. In addition, it combines with calcium and magnesium of the bones. Since its action can be delayed for many hours, it can distribute throughout the body, causing the erosion of bones. These features have shown how the study of alternative “green” treatments is crucial.

Protocol for the preparation of alumina/metal brazed joints-Master Thesis MANUEL RAMONES

Author: MANUEL RAMONES ; Type of thesis: Master thesis
Abstract: Brazing is the joining of materials through the use of heat and a filler metal with a melting temperature above 450°C but below the melting point of the metals being joined. This technique joins parts by creating a metallurgical bond between the filler metal and the surfaces of the two materials joined. There are several factors which have direct influence on the final quality of a brazed piece:
the filler metal selection, the heating technique, the atmosphere in which the process is performed, the cleaning procedure, the assembly of pieces, etc. In metal-ceramic junctions, ceramic surfaces, especially oxides, are very stable chemically, consequently, molten metals do not wet them well. There are several techniques that allow to overcome the chemical challenge. In order to develop a procedure that ensures the conditions to achieve a successful brazing process, several techniques for metal-ceramic brazing in a controlled atmosphere (vacuum) were tested. Brazing using active filler metals and direct brazing using ceramic metallization by sputtering were studied in this work. Alumina (Al2O3) was chosen as the ceramic part, whereas stainless steel 304 and Inconel were chosen as metallic components, cylindrical samples were assembled in lap configuration and were heated by IR lamps. The pieces were cut and the cross-section was studied by Scanning Electron Microscope SEM and energy-dispersive X-ray spectroscopy (EDS, EDX) searching for evidence of filler metal uniform spread and diffusion. The samples brazed using Pallabraze 850 disc of 0.01 mm of thickness for braze Inconel and Metallized alumina with 1m of Titanium and using Argon atmosphere showed the more uniform distribution and diffusion.

Purification technique of 6 GHz Tesla type suoerconducting Nb cavities: A new approach for improving RF performances-Master Thesis RAM KRISHNA THAKUR

Author: RAM KRISHNA THAKUR ; Type of thesis: Master Thesis
Abstract: The lowest possible surface resistivity and higher accelerating field are the paramount considerations, hence are obligatory for accelerating cavities. Since, superconducting materials are used to make radio-frequency cavities for future accelerators. In the case of rf cavities, superconductors are being used in order to minimize the power dissipated and increase the figures of merit of a radio-frequency cavity, such as the quality factor and accelerating gradient.
Hence, these could be achieved by improving surface treatment to the cavity, and processing techniques must be analyzed in order to optimize these figures of merit.
The research work reported in this dissertation mainly carried out on tesla type seamless 6GHz Nb and Cu cavities. We have developed two innovative techniques: firstly, for mechanical polishing of cavities, and secondly for purification of these cavities at atmospheric pressure under cover of 4Helium gas (for protection) and at ultra-high vacuum (UHV) system. These cavities are
fabricated by spinning technology to create seamless cavities.
The main advantages of 6 GHz bulk-Nb cavities are saving cost, materials and time to collect statistics of surface treatments and RF test in a very short time scale. Cavities are RF tested before and after high temperature treatment under atmospheric pressure (under cover of inert gas atmosphere to protect inner and outer surface of cavity) inside transparent quartz tube, and under
UHV conditions. Induction heating method is used to anneal the cavity at temperatures higher than 2000°C and close to the melting point of Nb for less than a minute while few seconds at maximum temperature. Before RF test and UHV annealing, the surface treatment processes like tumbling, chemical, electro-chemical (such as BCP and EP), ultrasonic cleaning and high pressure rinsing (HPR) have been employed. High temperature treatment for few minutes at
atmospheric pressure allow to reduce hydrogen, oxygen and other elemental impurities, which effects on cavity Q-factor degradation, hence recovers rf performances of these cavities. This research work will address these problems and illustrate the importance of surface treatments. Continue reading

Study of the Electropolishing of 6GHz Niobium cavity in ionic liquids-Master Thesis OLGA MALKOVA

Author: OLGA MALKOVA ; Type of thesis: Master Thesis
Abstract: INFN – LNL Laboratories have been already working for several years on the problem of removing fluoride ions from a solution for polishing of niobium. Ionic liquids are one of the possible solutions for this problem. The first results of niobium polishing have already been obtained in ionic liquid – Choline Chloride with Urea. During polishing in the ionic liquid was obtained smooth shiny surface with a roughness comparable as obtained after polishing in classic electrolyte. Various additives such as sulfamic acid, ammonium sulfamate, can improve the condition of the surface.
Our task is to apply this knowledge to polish RF cavities. In our work we try to create new ionic liquid and improve one that was previously obtained. In our laboratory we built new system for electropolishing 6 GHz cavities considering the experience of previous years.

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