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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
91

Electrochemical Application and AFM Characterization of Nanocomposites : Focus on Interphase Properties

Huang, Hui January 2017 (has links)
The use of graphene and conductive polyaniline nanomaterials in the field of electrochemistry is increasing due to their excellent conductivity, rapid electron transfer and high specific surface area. However, these properties are strongly dependent on the preparation processes. To accelerate the development of advanced electrochemical sensors for the simultaneous detection of trace amounts of heavy metal ions, two facile and green methods are proposed to improve their performance in this thesis. The first one was dedicated to make graphene-carbon nanotube hybrid nanocomposites. The introduction of carbon nanotubes not only greatly enhances the conductivity of graphene but also suppresses, to some degree, the aggregation between graphene nanosheets. Another method proposed in this thesis work was to synthesize a phytic acid doped polyaniline nanofiber based nanocomposite. The synergistic contribution from polyaniline nanofibers and phytic acid enhances the accumulation efficiency and the charge transfer rate of metal ions during the differential pulse anodic stripping voltammetry analysis. The above-mentioned nanocomposite modified electrodes were all successfully applied to real samples for the simultaneous detection of Cd2+ and Pb2+ with good recovery rates. Meanwhile, corrosion protection is another important branch in the field of electrochemistry. In this direction, an active alkyd-polyaniline composite coating with self-healing functionality was prepared. The polyaniline used in this thesis was doped with p-toluene sulfonic acid, which was employed to increase the conductivity of polyaniline, and 1 wt.% of as-prepared polyaniline nanoparticles were found to offer an effective conductive network for anticorrosion. Finally, the reasons that such low loading levels of nanomaterials can result in significantly reinforced properties in nanocomposites were studied with combined atomic force microscopy (AFM) techniques. The results demonstrated that the interphase for a 40-nm-sized silica particle could extend to 55–70 nm in poly(ethyl methacrylate) (PEMA) and poly(isobutyl methacrylate) (PiBMA) polymer matrix, and the interphase exhibited a gradient distribution in surface nanomechanical properties. / <p>QC 20170315</p>
92

Failure mechanisms in APS and SPS thermal barrier coatings during cyclic oxidation and hot corrosion

Jonnalagadda, Krisha Praveen January 2017 (has links)
Thermal Barrier Coatings (TBCs) are advanced material systems that are being used in the hot sections of gas turbines such as combustor, turbine blades, and vanes. The top ceramic coating in TBCs provides insulation against the hot gases and the intermediate metallic bond coat provides oxidation and corrosion resistance to the underlying turbine components. Durability of thermal barrier coatings is very important for the overall performance of the gas turbine. TBCs can fail in several different ways and there is a combination of more than one failure mechanism in most situations. One of the most widely used TBC is atmospheric plasma sprayed (APS) yttria stabilized zirconia (YSZ). Both the deposition technique and the TBC material have certain limitations. The main aim of this research is to study new TBC materials and/or new deposition techniques and compare with the conventional YSZ and understand their failure mechanisms during cyclic oxidation and hot corrosion. Thermal cyclic oxidation of a newly developed high purity nano YSZ thermal barrier coating has been studied. Cross sectional analysis of exposed as well as completely failed samples showed a mixed-type failure caused by crack propagation parallel to the bond coat/top coat interface. The majority of the damage occurred towards the end of the coating life. A finite element model has been developed to study the probability of crack growth along different paths that leads to the final failure. Hot corrosion mechanism in suspension plasma sprayed two-layer gadolinium zirconate/YSZ, three-layer dense gadolinium zirconate/gadolinium zirconate/YSZ, and a single-layer YSZ has been studied in the presence of sodium sulfate and vanadium pentoxide. The test results showed that gadolinium zirconate coatings were more susceptible to corrosion compared to YSZ coatings despite gadolinium zirconate coatings having lower reactivity with the corrosive salts. Thermal cycling behavior of a high chromium bond coat has been studied. Cross-sectional analysis showed formation of sandwich type microstructure with chromium rich oxide and alumina as the top and the bottom layers. Inter-diffusion of minor elements between different MCrAlY coatings – substrate systems has been studied using, diffusion simulation software, DICTRA. The simulation results showed that the diffusion of minor elements in the coatings is dependent on the rate of β phase depletion in the beginning. After the depletion of β phase there was no clear dependence of the coating composition on the diffusion of minor elements.
93

Methods to create compressive stress in high strength steel components

Abdin, Amir, Feyzabi, Kaveh, Hellman, Oskar, Nordström, Henrietta, Rasa, Dilman, Thaung Tolförs, Gustav, Öqvist, Per-Olof January 2018 (has links)
Residual compressive stresses can be used to increase the lifetime of parts under cyclic stress as they negate the applied tensile stresses that cause crack initiation and propagation in the material. The goal of this project was to investigate methods to induce stresses, their advantages and disadvantages as well as depth and magnitude of induced stresses, and also to find methods of analyzing the induced residual stresses. This was done on behalf of Epiroc Drilling Tools AB in order for them to induce stresses on the insides of their long, narrow and hollow rods, where stress induction is difficult. Shot peening was used as a reference as that is the method currently in use by the company. The results show that the two most promising methods are cavitation peening and laser shock peening; two relatively new methods with large magnitudes and depth of induced stress as well as a great capability of inducing stresses on the hard-to-reach insides of the rods. Ultrasonic needle peening, ultrasonic shot peening as well as induction hardening, cryogenic treatment and friction stir processing were also investigated. Methods of analyzing the stresses include X-ray diffraction and slitting, hole drilling and ultrasonic methods.
94

Exploration of Non-Aqueous Metal-O2 Batteries via In Operando X-ray Diffraction

Liu, Chenjuan January 2017 (has links)
Non-aqueous metal-air (Li-O2 and Na-O2) batteries have been emerging as one of the most promising high-energy storage systems to meet the requirements for demanding applications due to their high theoretical specific energy. In the present thesis work, advanced characterization techniques are demonstrated for the exploration of metal-O2 batteries. Prominently, the electrochemical reactions occurring within the Li-O2 and Na-O2 batteries upon cycling are studied by in operando powder X-ray diffraction (XRD). In the first part, a new in operando cell with a combined form of coin cell and pouch cell is designed. In operando synchrotron radiation powder X-ray diffraction (SR-PXD) is applied to investigate the evolution of Li2O2 inside the Li-O2 cells with carbon and Ru-TiC cathodes. By quantitatively tracking the Li2O2 evolution, a two-step process during growth and oxidation is observed. This newly developed analysis technique is further applied to the Na-O2 battery system. The formation of NaO2 and the influence of the electrolyte salt are followed quantitatively by in operando SR-PXD. The results indicate that the discharge capacity of Na-O2 cells containing a weak solvating ether solvent depends heavily on the choice of the conducting salt anion, which also has impact on the growth of NaO2 particles. In addition, the stability of the discharge product in Na-O2 cells is studied. Using both ex situ and in operando XRD, the influence of sodium anode, solvent, salt and oxygen on the stability of NaO2 are quantitatively identified. These findings bring new insights into the understanding of conflicting observations of different discharge products in previous studies. In the last part, a binder-free graphene based cathode concept is developed for Li-O2 cells. The formation of discharge products and their decomposition upon charge, as well as different morphologies of the discharge products on the electrode, are demonstrated. Moreover, considering the instability of carbon based cathode materials, a new type of titanium carbide on carbon cloth cathode is designed and fabricated. With a surface modification by loading Ru nanoparticles, the titanium carbide shows enhanced oxygen reduction/evolution activity and stability. Compared with the carbon based cathode materials, titanium carbide demonstrated a higher discharge and charge efficiency.
95

Insights into dynamic covalent chemistry for bioconjugation applications

Wang, Shujiang January 2017 (has links)
Dynamic covalent chemistry (DCC) is currently exploited in several areas of biomedical applications such as in drug discovery, sensing, molecular separation, catalysis etc. Hydrazone and oxime chemistry have several advantages, such as mild reaction conditions, selectivity, efficiency, and biocompatibility and therefore, have the potential to be for bioconjugation applications. However, these reactions suffer from major drawbacks of slow reaction rate and poor bond stability under physiological conditions. In this regard, the work presented in this thesis focuses on designing novel bioconjugation reactions amenable under physiological conditions with tunable reaction kinetics and conjugation stability. The first part of the thesis presents different strategies of dynamic covalent reactions utilized for biomedical applications. In the next part, a detailed study related to the mechanism and catalysis of oxime chemistry was investigated in the presence of various catalysts. Aniline, carboxylate and saline were selective as target catalysts and their reaction kinetics were compared under physiological conditions (Paper I and II). Then we attempted to explore the potential of those chemistries in fabricating 3D hydrogel scaffolds for regenerative medicine application. A novel mild and regioselective method was devised to introduce an aldehyde moiety onto glycosaminoglycans structure. This involved the introduction of amino glycerol to glycosaminoglycans, followed by regioselective oxidation of tailed flexible diol without affecting the C2-C3 diol groups on the disaccharide repeating unit. The oxidation rate of the tailed flexible diol was 4-times faster than that of C2-C3 diol groups of native glycosaminoglycan. This strategy preserves the structural integrity of the glycosaminoglycans and provides a functional aldehyde moiety (Paper III). Further, different types of hydrazones were designed and their hydrolytic stability under acidic condition was carefully evaluated. The hydrazone linkage with the highest hydrolytic stability was utilized in the preparation of extracellular matrix hydrogel for delivery of bone morphogenetic proteins 2 in bone regeneration (Paper IV) and studied for controlled release of the growth factor (Paper III). In summary, this thesis presents a selection of strategies for designing bioconjugation chemistries that possess tunable stability and reaction kinetics under physiological conditions. These chemistries are powerful tools for conjugation of biomolecules for the biomedical applications.
96

Controlling the growth of nanoparticles produced in a highpower pulsed plasma

Gunnarsson, Rickard January 2017 (has links)
Nanotechnology can profoundly benefit our health, environment and everyday life. In order to make this a reality, both technological and theoretical advancements of the nanomaterial synthesis methods are needed. A nanoparticle is one of the fundamental building blocks in nanotechnology and this thesis describes the control of the nucleation, growth and oxidation of titanium particles produced in a pulsed plasma. It will be shown that by controlling the process conditions both the composition (oxidationstate) and size of the particles can be varied. The experimental results are supported by theoretical modeling. If processing conditions are chosen which give a high temperature in the nanoparticle growth environment, oxygen was found to be necessary in order to nucleate the nanoparticles. The two reasons for this are 1: the lower vapor pressure of a titanium oxide cluster compared to a titanium cluster, meaning a lower probability of evaporation, and 2: the ability of a cluster to cool down by ejecting an oxygen atom when an oxygen molecule condenses on its surface. When the oxygen gas flow was slightly increased, the nanoparticle yield and oxidation state increased. A further increase caused a decrease in particle yield which is attributed to a slight oxidation ofthe cathode. By varying the oxygen flow, it was possible to control the oxidation state of the nanoparticles without fully oxidizing the cathode. Pure titanium nanoparticles could not be produced in a high vacuum system because oxygen containing gases such as residual water vapour have a profound influence on nanoparticle yield and composition. In an ultrahigh vacuum system titanium nanoparticles without significantoxygen contamination were produced by reducing the temperature of the growth environment and increasing the pressure of an argon-helium gas mixture within whichthe nanoparticles grew. The dimer formation rate necessary for this is only achievable at higher pressures. After a dimer has formed, it needs to grow by colliding with a titanium atom followed by cooling by collisions with multiple buffer gas atoms. The condensation event heats up the cluster to a temperature much higher than the gas temperature, where it is during a short time susceptible to evaporation. When the clusters’ internal energy has decreased by collisions with the gas to less than the energy required to evaporate a titanium atom, it is temporarily stable until the next condensation event occurs. The temperature difference by which the cluster has to cool down before it is temporarily stable is exactly as many kelvins as the gas temperature.The addition of helium was found to decrease the temperature of the gas, making it possible for nanoparticles of pure titanium to grow. The process window where this is possible was determined and the results presented opens up new possibilities to synthesize particles with a controlled contamination level and deposition rate.The size of the nanoparticles has been controlled by three means. The first is to change the electrical potential around the growth zone, which allows for size (diameter) control in the order of 25 to 75 nm without influencing the oxygen content of the particles. The second means is by increasing the pressure which decreases the ambipolar diffusion rate of the ions resulting in a higher growth material density. By doing this, the particle size can be increased from 50 to 250 nm, however the oxygen content also increases with increasing pressure when this is done in a high vacuum system. The last means of size control was by adding a helium flow to the process where higher flows resulted in smaller nanoparticle sizes. When changing the pressure in high vacuum, the morphology of the nanoparticles could be controlled. At low pressures, highly faceted near spherical particles were produced. Increasing the pressure caused the formation of cubic particles which appear to ‘fracture’ at higher pressures. At the highest pressure investigated, the particles became poly-crystalline with a cauliflower shape and this morphology was attributed to a lowad atom mobility. The ability to control the size, morphology and composition of the nanoparticles determines the success of applying the process to manufacture devices. In related work presented in this thesis it is shown that 150-200 nm molybdenum particles with cauliflower morphology were found to scatter light in which made them useful in photovoltaic applications, and the size of titanium dioxide nanoparticles were found to influence the selectivity of graphene based gas sensors.
97

Spectroelectrochemical analysis of the Li-ion battery solid electrolyte interphase using simulated Raman spectra / Analys av anodens gränsskikt i litiumjonbatterier med spektroelektrokemi och simulerade Ramanspektra

Andersson, Edvin January 2020 (has links)
Lithium Ion Batteries (LIBs) are important in today's society, powering cars and mobile devices. LIBs consist of a negative anode commonly made of graphite, and a positive cathode commonly made from transition metal oxides. Between these electrodes are separators and organic solvent based electrolyte. Due to the high potential of LIBs the electrolyte is reduced at the anode. The electrolyte reduction results in the formation of a layer called the Solid Electrolyte Interphase (SEI), which prohibits the further breakdown of the electrolyte. Despite being researched for over50 years, the composition formation of the SEI is still poorly understood. The aim of this project is to develop strategies for efficient identification and classification of various active and intermediate components in the SEI, to, in turn, gain an understanding of the reactions taking place, which will help find routes to stabilize and tailor the composition of the SEI layer for long-term stability and optimal battery performance. For a model gold/li-ion battery electrolyte system, Raman spectra will be obtained using Surface Enhanced Raman Spectroscopy (SERS) in a spectroelectrochemical application where the voltage of the working gold electrode is swept from high to low potentials. Spectra of common components of the SEI as well as similar compounds will be simulated using Density Functional Theory (DFT). The DFT data is also used to calculate the spontaneity of reactions speculated to form the SEI. The simulated data will be validated by comparing it to experimental spectra from pure substances. The spectroelectrochemical SERS results show a clear formation of Li-carbonate at the SERS substrate, as well as the decomposition of the electrolyte into other species, according to the simulated data. It is however shown that there are several issues when modelling spectra, that makes it harder to correlate the simulated spectra with the spectroelectrochemical spectra. These issues include limited knowledge of the structure of the compounds thought to form on the anode surface, and incorrect choices in simulational parameters. To solve these issues, more work is needed in these areas, and the spectroelectrochemical methods used in this thesis needs to be combined with other experimental methods to narrow down the amount of compounds to be modelled. More work is also needed to avoid impurities in the electrolyte. Impurities leads to a thick inorganic layer which prohibits the observation of species in the organic layer.
98

Secondary Steel Metallurgy Slag Design and MgO-C Refractory Implications : Theoretical and Practical Considerations

Simon, Hellgren January 2019 (has links)
MgO-C based refractory materials, often used in secondary steel making, are exposed to variouswear mechanisms in its application. The wear could be divided into oxidative, chemical andabrasive categories, all behaving differently and all being influenced by different factors. Dueto the importance of minimizing material loss and to the environmental challenges to run asustainable industry, it is of interest to gain more knowledge of the behavior of the refractorymaterial in use. The present thesis work specifically investigated slag designed of the CaOSiO2-Al2O3-MgO (CSAM) system as well as the chemical and oxidative wear mechanisms ofthree different MgO-C based refractory materials from Höganäs AB, Halmstadverken, whichcontained 5, 10 and 12 wt% carbon (labeled T05, T10 and T12). Different CSAM slags weredesigned to meet certain process criteria such as MgO and CaO saturations and wereinvestigated through thermodynamic calculations using the FactSage software and throughlaboratory scaled slag smelting experiments. The oxidation effect on the refractory material wasalso studied through pre-heating simulations in chamber furnaces, similar to the pre-heating ofa re-built ladle furnace.The thermodynamic calculations made in FactSage 7.0, using the FactPS and FToxid databases, resulted in a few different slag designs with different properties. A few different slagsfulfilled the CaO and MgO saturation limits proposed by Höganäs AB and could be consideredto test experimentally for further evaluation. The simulations also showed trends on how theliquid viscosity behaved with different slag compositions and how the solids content changedwith temperature.The oxidation experiments were performed on the different MgO-C refractory types, where thebricks with 10% carbon also contained Al2O3 antioxidants. The experiments showed that themass loss during the pre-heating is greater for refractory with higher carbon content, withexception to T10, where the mass losses were measured to 3.76 – 4.01%, 1.06 – 1.28% and6.28 – 6.33% for T05, T10 and T12 respectively. Further, the oxidation depth of each materialwas measured to 9-10 mm, 2-3 mm and 2-5 mm for the T05, T10 and T12. The experimentsalso showed that T12 refractory in particular was very susceptible to abrasive wear after beingoxidized.The slag smelting experiments were carried out through two different methods, by melting slagin MgO-C crucibles and by melting pressed slag briquettes on top of refractory bricks. Theformer tests mainly showed that the methodology was not suitable for this type of refractorymaterial due to the crucibles cracking during the experiments. The latter experiments showedsome general behaviour of the different components in the slag, where Ca, Al and Fe stayednear the surface, and Si and Mg penetrated deeper. The spinel formation at the refractory surfacewas then concluded to be the reason for Al not penetrating deeper. Further it was concludedthat no significant difference in refractory dissolution was seen between slags with- and withoutMgO, other than possibly a small increase in refractory dissolution for the latter.
99

Investigating Particle Cracking in Single- and Polycrystalline Nickel-Rich Cathodes using In Situ Impedance Spectroscopy

Sjödin, Mattias January 2021 (has links)
State-of-the-art Li-ion cathode materials are based on LiMO2 (M=Ni, Mn, Co) layered transition metal oxides (denoted NMC) with Ni-rich composition because of their high specific capacity. Yet, these materials suffer from poor capacity retention due to crack formation during de-/lithiation cycling. Particle cracking leads to exposure of new electrode surface which leads to Li-inventory loss, increased side reactions, and electric disconnection. Quantification of the extent of cracking is therefore desirable, especially during in situ whilst cycling of the Li-ion cell. Herein, we evaluate and improve an analytical methodology based on electrochemical impedance spectroscopy (EIS) in order to estimate the changes in electrochemically active surface area of both poly- and single-crystalline Ni0.8Mn0.1Co0.1(NMC811) active materials. A transmission-line model (TLM) applied to both non-blocking and blocking electrode condition was utilized in order to deconvolute and interpret the acquired experimental data. Fits of the complex TLM equivalent-circuits to the impedance spectra was facilitated by developing a global stochastic iterative function based on local multivariate optimization. Impedance analysis during short- term cycling showed that the single-crystalline NMC811 suffered from less particle cracking and side reactions compared to polycrystalline NMC811, which was also confirmed from post-mortem gas adsorption analysis. A novel approach to estimate the extent of particle cracking in commercial Li-ion cells by utilizing an empirically strong positive correlation between the charge-transfer capacitance and resistance was proposed. The work presented herein demonstrates the unique prospects of the EIS methodology in the development and research of future rechargeable batteries
100

Synthesis and spectroscopic characterization of emerging synthetic cannabinoids and cathinones

Carlsson, Andreas January 2016 (has links)
The application of different analytical techniques is fundamental in forensic drug analysis. In the wake of the occurrence of large numbers of new psychoactive substances possessing similar chemical structures as already known ones, focus has been placed on applied criteria for their univocal identification. These criteria vary, obviously, depending on the applied technique and analytical approach. However, when two or more substances are proven to have similar analytical properties, these criteria no longer apply, which imply that complementary techniques have to be used in their differentiation. This work describes the synthesis of some structural analogues to synthetic cannabinoids and cathinones based on the evolving patterns in the illicit drug market. Six synthetic cannabinoids and six synthetic cathinones were synthesized, that, at the time for this study, were not as yet found in drug seizures. Further, a selection of their spectroscopic data is compared to those of already existing analogues; mainly isomers and homologues. The applied techniques were mass spectrometry (MS), Fourier transformed infrared (FTIR, gas phase) spectroscopy and nuclear magnetic resonance (NMR) spectroscopy. In total, 59 different compounds were analyzed with the  selected techniques. The results from comparison of spectroscopic data showed that isomeric substances may in some cases be difficult to unambiguously identify based only on their GC-MS EI spectra. On the other hand, GC-FTIR demonstrated more distinguishable spectra. The spectra for the homologous compounds showed however, that the GC-FTIR technique was less successful compared to GC-MS. Also a pronounced fragmentation pattern for some of the cathinones was found. In conclusion, this thesis highlights the importance of using complementary techniques for the univocal identification of synthetic cannabinoids and cathinones. By increasing the number of analogues investigated, the more may be learnt about the capabilities of different techniques for structural differentiations, and thereby providing important identification criteria leading to trustworthy forensic evidence.

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