This thesis deals with topic of high entropy alloys. The teoretical part explains what are high entropy alloys, how are they different from conventional alloys, how is their chemical composition proposed and what potencial these alloys have. The experimental part describes procedures of preparation of three high entropy alloys witch consists of Co, Cr, Fe, Ni and Ti, where the concentration of all elements except Ti remains the same. These alloys were prepared via mechanical alloying and sintered by SPS process. Crucial part of this thesis is characterization of these three alloys with EDS and XRD supported by hardness measuring and tensile tests.

The goal of this work was to evaluate the electrochemical properties of TiZrNbTa thin films deposited by magnetron sputtering using an industrial physical vapor deposition system. Samples were deposited on both Si(001) and 316L stainless steel. The samples deposited on Si(001) were either crystalline (bcc reflections) or amorphous, depending on the sputtering parameters. The crystalline films were composed of thin films with two different layers. The upper layer was nanocolumnar composed of elongated nanocolumns, while the lower was dense. The amorphous films had only one nanocolumnar layer and higher porosity. Polarization curves revealed that all samples had low corrosion current densities, in the order of 10-8 A/cm2. The samples showed an extended passive region up to 3.0 V vs Ag/AgCl due to the growth of a passivating oxide. The surface of the samples consisted of Nb2O5, ZrO2, TiO2 and Ta2O5. The chronoamperometry tests showed current oscillations, related to a break-down and reformation of the passive film. Electrochemical impedance spectroscopy revealed that all samples behaved similarly in all three electrolytes, and the simulated electrical circuits were indicating no corrosion reactions. A decrease in capacitance values after polarization was observed and was related to the formed surface oxide. Samples deposited on 316L stainless steel showed a passive regime for a shorter potential window, probably related to surface defects of the films. Heat treatments at 400 and 800 Celsius for 20 hours could not trigger the phase transformation from single bcc to hcp or dual bcc, as predicted by the Thermo-Calc software.

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This project presents an attempt to construct a setup and implement a reliable technique for measuring the magnetocaloric effect (MCE) on various materials via a direct method for the acquisition of the data. The main objective of the latter is to produce a ∆Tadiabatic vs T graph over a reasonable temperature span (-100◦C up to 220◦C) by thermal monitoring of a magnetic material exposed to an oscillating magnetic field with a maximum strength of 1.2T. The setup consists of a vacuum-insulated glass tube containing the sample placed between two electromagnets of a vibrating-sample magnetometer (VSM) and increasingly heated by a resistance wire, while the temperature is recorded directly by a thermocouple. The first experiments are performed on Gadolinium (Gd) samples as a reference material in order to verify the overall reliability of the system. The obtained results on Gadolinium show that meaningful data can be acquired with this direct method, although the initially-extracted ∆Tadiabatic near room temperature stands at the accuracy limit (25%) generally accepted with this method. Unexpected interference signals from the thermocouple are encountered for high temperatures and are shown to be due to magnetic dependence from one of its constituents. Data from high temperatures can however be reliably corrected with respect to a baseline signal from a neutral nonmagnetic material. As such magnetocaloric properties of two Manganese-rich high entropy alloys are investigated with one exhibiting at most ∆Tadiabatic = 0.2◦C at its Curie temperature TC = 60◦C. Suggestions regarding the possibility of operating the setup at sub-zero temperatures are put forward and promising results from a new spot- welded thermocouple show a significantenhancement of the initial setup accuracy. / Detta projekt presenterar ett försök att konstruera en installation och implementera en pålitlig teknik för att mäta den magnetokolorisk effekten (MCE) på olika material via en direkt metod för insamling av data. Det sistnämnda syftet är att producera en ∆Tadiabatisk vs T över ett rimligt temperaturintervall (-100◦C up to 220◦C). Detta genom en termisk övervakning av ett magnetiskt material utsatt för ett oscillerande magnetfält med en maximal magnitud på 1.2 T. Utrustningen utgörs av ett vakuumisolerade glasrör som innehåller provet, vilket är placerat mellan två elektromagneter från en vibrating-sample magnetometer (VSM) och som stegvis värms upp av en resistanstråd, medan temperaturen registreras direkt av ett termoelement. De inledande experimenten utförs på prover av Gadolinium (Gd) som referensmaterial för att verifiera systemets totala tillförlitlighet. De erhållna resultaten från Gadolinium proverna visar att meningsfulla data kan produceras med denna direkta metod. Även om de extraherade ∆Tadiabatisk vid rumstemperatur befinner sig inom precisions gränsen (25%), vilken är allmänt accepterad med avseende på den direkta metoden. Oväntade missvisande signaler från termoelementet uppträder vid höga temperaturer och visar sig bero på magnetiskt beroende från instumentet. Data från höga temperaturer kan emellertid pålitligt korrigeras med en baslinjesignal från ett neutralt icke-magnetiskt material. Därmed undersöks de magnetokoloriska egenskaper hos två Mangan-rika hög entropi legeringar, där en uppvisar som högst ∆Tadiabatisk = 0.2◦C vid dess Curie-temperatur TC = 60◦C. Förslag beträffande möjligheten att använda installationen vid temperaturer under noll läggs fram. Lovande resultat från ett nytt punktsvetsat termoelement visar en betydande förbättringav den inledande installationens noggrannhet.

Plasma centrifugal atomization is a method widely used in the production of spherical powders of metals and alloys with relatively low melting points. A novel plasma centrifugal atomization process suitable for high melting point materials (i.e. 3500 ᵒC and above) was developed by Metasphere Technology AB, currently Höganäs Sweden AB. In this process, feedstock material in the form of crushed powder with particle sizes in the range 400-1000 µm is fed into a rotating crucible and subsequently melted by the glow discharge of a plasmatron. Due to high rotational speeds, a melt film forms at the edge of the crucible and breaks into fine droplets that are ejected into the reactor chamber and solidified in a whirl of cold inert gases. Capability of the plasmatron to reach very high temperatures, combined with extremely rapid cooling of the ejected droplets, allow for the fabrication of fine powders of refractory alloys exhibiting metastable phases that cannot be obtained otherwise.  Oil drilling, ore processing and metal shaping applications, among other, require tool materials capable of withstanding harsh working conditions under heavy loads. Owing to their physical, chemical and mechanical properties, tungsten-carbon alloys are among the most suited materials for such applications. Melting followed by rapid solidification of tungsten-carbon mixtures with 3.9 wt.% C results in a biphasic structure composed of WC lamellae inserted in a W2C matrix, known as cast tungsten carbide (CTC). Due to the metastable nature of both phases present, CTC exhibits exceptional mechanical properties. CTC is mainly used as reinforcing dispersed phase in metal matrix composite hardfacing overlays, which are deposited by plasma transferred arc (PTA) welding or laser cladding onto steel tools. High-entropy alloys (HEAs) are defined as multi-component solid solutions with equimolar or near-equimolar concentration of all principal elements. Owing to their outstanding mechanical, corrosion, erosion, oxidation and radiation resistance properties compared to conventional alloys, HEAs are among the most suited materials for aerospace and nuclear applications. Several processing routes have allowed for laboratory-scale production of HEAs. Nevertheless, size and shape of bulk components that can be thus produced are largely limited. In a quest for up-scaling the processing of high-end bulk HEA components, plasma centrifugal atomization of pre-alloyed refractory HEA spherical powders suitable for additive manufacturing was envisaged. In this work, capabilities of the novel plasma centrifugal atomization for processing of refractory alloys into fine spherical powders have been evaluated based on two different material systems, namely CTC and a refractory HEA containing Ti, V, Zr, Nb, Mo, Hf, Ta, W. Challenges of local mechanical characterization of micron-sized powders have been addressed and a robust method for testing of individual particles has been developed. Mechanical properties such as hardness and fracture toughness of plasma atomized CTC powders have been extensively investigated and related to the corresponding thermal stories. Experimental results suggest significant straining of the crystal lattice in the case of as-atomized CTC, possibly due to extremely high cooling rates experienced by the solidifying particles. This has been ruled out the main reason for the outstanding mechanical properties of plasma atomized CTC compared to both spheroidized CTC and conventional cast & crushed CTC. Effective stress relieve was possible upon heat treatment. Plasma atomization of the refractory HEA yielded similar results, where an extremely fine microstructure with no noticeable chemical segregation was obtained. Indentation hardness of this novel microstructure was found to be approximately 25% higher than that of similar alloys reported in literature. HEA powder thus produced was then consolidated into bulk HEAs with very simple geometries, proving that this powder can be further processed into components of more or less complexity for pre-defined applications.

Metal-based high entropy oxides are considered promising electrode materials for use in Li- ion batteries. In this work, the most widely studied high entropy oxide Mg0.2Ni0.2Cu0.2Co0.2Zn0.2O (M-HEO) with rock salt structure was successfully synthesized by Modified Pechini synthesis, characterized by X-ray diffraction analysis, and investigated as anode active material (negative electrode) in a coin cell. M-HEO has the concept of entropy stabilisation of crystal structure in oxide system with the configurational entropy value of 1,6R which confirmed that M-HEO classified as high entropy oxide.  To test the electrochemical performance, full cells comprising M-HEO as anode, lithium manganese oxide (LMO) as cathode together with ionic liquid electrolyte were assembled to explore their potential for practical applications. The electrochemical cycling performance was studied by two electrochemical experiments which are three-electrode cyclic voltammetry and galvanostatic charge/discharge. The cyclic voltammetry measurement was used to determine the behaviour of the system such as potential window and scan rate, while galvanostatic charge/discharge was used to determine the performance of the battery over time by applying constant current.  The results demonstrate that high entropy oxide possess a stable structure. This points out the direction for the preparation of M-HEOs with stable structure and excellent performance and provides a promising candidate for anode materials for LIBs. / Metallbaserade högentropioxider anses vara lämpliga för användning av elektrodmaterial för litium-jon batterier. I detta arbete syntetiserades den första högentropioxiden Mg0.2Ni0.2Cu0.2Co0.2Zn0.2O (M-HEO) som har stensaltstruktur genom Modifierad Pechini- syntesmetod, karakteriserad av röntgendiffraktionsanalys och undersöktes som aktivt material i den negativa elektroden. M-HEO har konceptet av entropistabilisering av kristallstrukturen i oxidsystem som har det konfigurerade entropivärdet av 1,6R. Detta bekräftade att M-HEO klassificerades som högentropioxid.  För att testa den elektrokemiska prestandan, användes fullceller bestående av M-HEO som anod, litiummanganoxid (LMO) som katod tillsammans med jonisk flytande elektrolyt. Detta gjordes för att undersöka M-HEO potentiella praktiska tillämpningar. Den elektrokemiska cyklingsprestandan studerades genom två elektrokemiska experiment, cyklisk voltammetri med tre-elektroder och galvanostatisk laddning/urladdning med knapp-celler. Den cykliska voltammetri mätningen användes för att bestämma vart i systemet sker redox reaktion för att sedan kunna identifiera på vilka potentialintervall samt skanningshastighet, medan galvanostatisk laddning/urladdning användes för att bestämma batteriets prestanda över tid genom att applicera konstant ström. Resultaten visar sig att hög entropi oxider har en stabil stensaltstruktur. Detta bidrar till att M-HEO som har en stabil struktur kan vara ett lämpligt anodmaterial i litium-jon batterier.

Ziel der Arbeit ist es, die Eignung pulvermetallurgischer Verfahren für die spätere industrielle Nutzung, die Werkstoffeigenschaften sowie das Sinterverhalten für High-Entropy Alloys (HEAs) zu evaluieren. Aufgrund des einphasigen Gefüges ist CoCrFeMnNi eine geeignete Modelllegierung, um die grundlegenden Eigenschaften von HEAs zu analysieren und wird im Rahmen dieser Dissertation exemplarisch für die High-Entropy Alloys verwendet. Verdüstes CoCrFeMnNi-Pulver wird mit drucklosem Sintern und Spark Plasma Sintern unter Verwendung von geeigneten Prozessparametern kompaktiert. Ausgewählte mechanische und physikalische Eigenschaften von CoCrFeMnNi werden bestimmt und im Vergleich mit konventionellen Legierungen bewertet. Die festigkeitssteigernden Mechanismen Kornfeinung und Ausscheidungshärtung werden diskutiert. Durch die Zugabe von Titan zu dem inertgasverdüsten HEA-Pulver wird dafür eine aushärtbare Legierung hergestellt. Zum besseren Verständnis der beim Sintern in HEAs ablaufenden Diffusionsvorgänge wird ein Modell zum Ausheilen isolierter Poren anhand eines vereinfachten Systems für einen binären Mischkristall entwickelt und diskutiert. Des Weiteren wird die Aktivierungsenergie beim Sintern anhand von Schwindungsversuchen berechnet und anschließend mit konventionellen Legierungen verglichen.

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High entropy alloys (HEAs) are made of at least five principal elements in near-equimolar proportions. The vast number of possible alloys and unconventional combinations of properties are the main benefits of HEAs. Ti, Nb, Cr, Al and N were chosen in order to create a hard, corrosion resistant coating with good thermal stability. TiNbCrAl multicomponent nitride thin films with Ti content between 0 to 14.4 at.% were deposited using multi-magnetron reactive high power impulse magnetron sputtering (R-HiPIMS) to investigate the feasibility of this method and to study how the Ti content affects the properties of the film. The samples deposited using reactive direct current magnetron sputtering (R-DCMS) were used as benchmarks. The settings required for near-equimolar composition were fixed, with Ti magnetron power as the only variable. Substrate was grounded and not intentionally heated. The composition of HiPIMS samples was more stable while the DCMS samples had significant fluctuations in Al and N content when varying the Ti target power, and were understoichiometric in nitrogen, (T iCrN bAl)1N1−δ, due to low degree of ionization of N. All crystalline samples had NaCl-type fcc structure. Crystalline DCMS samples were (111) textured, while the higher ionization characteristic for HiPIMS resulted in samples with competitive growth between two growth directions. The energetic particle bombardment caused the columnar structure of the film to be denser and less jagged, while DCMS samples containing Ti were significantly more porous. Denser, harder and stiffer films with significantly higher compressive stress were produced with HiPIMS. The hardness and stiffness were almost linearly dependent on Ti content, with density slightly decreasing as the Ti content increased. Higher Ti content increased the rate of corrosion of the films.