[pt] Limas de NiTi Profile® 25/.04 após sua usinagem não recebem tratamento superficial de polimento gerando pontos concentradores de tensão conseqüente áreas de trinca e fraturas. Avaliou-se o efeito de diferentes condições superficiais de limas endodônticas na resistência à torção. Foram avaliadas e caracterizadas por Microscopia Eletrônica de Varredura dezoito limas rotatórias de NiTi Profile® 25/.04. Utilizou-se 6 limas que não foram submetidas a tratamento químico (Grupo I), 6 limas tratadas com Ácido Nítrico 8% e Ácido Fluorídrico 4% em solução durante 2 minutos (Grupo II) e 6 limas tratadas com a mesma solução porém em tempo de 2 minutos e trinta segundos (Grupo III). Analisaram-se as limas com e sem tratamento superficial carregadas em ensaio de torção e suas fractografias em Microscopia Eletrônica de Varredura. As variáveis avaliadas foram torque aplicado no momento da fratura e ângulo máximo de rotação até a fratura. Os valores obtidos nos ensaios mecânicos referentes ao ângulo máximo de rotação e torque máximo foram analisados estatisticamente através do teste estatístico T-student. Os resultados obtidos permitem concluir que houve diferença estatisticamente significante quanto aos valores de torque máximo entre o Grupo II e Grupo III e ângulo máximo entre os Grupos I e III. / [en] NiTi Profile® 25/.04 files do not undergo surface polishing treatments after machining, and therefore exhibit local stress concentrators and, consequently, areas of cracking and fractures. The effect of different surface conditions on the torsional strength of endodontic files were evaluated. 18 NiTi Profile® 25/.04 rotary files were examined by scanning electron. A group of 6 files (Group I) were not subjected to any chemical treatment, another group of 6 (Group II) were treated for 2 minutes using a solution of 8% Nitric Acid, 4% Flouridic Acid, and a further 6 (Group III) were treated with the same solution fot 2.5 minutes. All the file, with and without treatment, were loaded in a torsion test and fractography of the samples was undertaken by scanning electron microscopy. The variables investigated were, torque at fracture and maximum angle of rotation at fracture. The results obtained in these mechanical tests were subjected to a statistical analysis utilizing the T-Student test. It can be concluded from these results that there was a statistically significant difference between the maximum torque results for groups II and III, and between the maximum angle results for groups I and III.

Packages are the means of preservation, distribution and convenience of use for food, medicine and other consumer products. Package opening is becoming complicated in many cases because of cutting cost in design and production of opening techniques. Introduction of new package opening technique, material or geometry for better opening experience, forces new design measurements which require a large number of prototype developments and physical testing. In order to achieve more rapid and accurate design, Finite Element Method (FEM) Simulations are widely used in packaging industries to compliment and reduce the number of physical testing. The goal of this work is to develop the building blocks towards complete package opening simulation. The study focuses on testing and simulation of shear fracture and shear delamination of packaging materials. A modified shear test specimen was developed and optimized by finite element simulation. Test method was validated for High-density polyethylene (HDPE) and Polypropylene (PP). The developed method has been accepted by international standards organization ASTM. Based on linear elastic fracture mechanics, a geometry correction factor of shear fracture toughness for the proposed specimen was derived. The study concluded that, for ease of opening, HDPE is a more favorable material for screw caps than PP. When performing the experiment with the shear specimen to find essential work of fracture, the ligament length should be varied between twice of the thickness and half of the width of the specimen ligament. Multi-layered thin laminate of Low-density polyethylene (LDPE) and aluminum (Al), also known as Al/LDPE laminate, is another key object addressed in this study. Continuum and fracture testing of individual layers provided the base information and input for numerical modeling. The propagation of an interfacial pre-crack in lamination in Al-LDPE laminate was simulated using several numerical techniques available in the commercial FEM solver ABAQUS, and it was concluded that using the combination of VCCT technique to model the interfacial delamination and coupled elasto-plastic damage constitutive for Al and LDPE substrates can describe interfacial delamination and failure due to necking. It was also concluded that the delamination mode in a pre-crack tip is influenced by the ratio of fracture energy release rate of mode I and II. To address the challenge in quantifying shear energy release rate of laminate with very thin substrate, a convenient test technique is proposed. Additionally, scanning electron microscopic study provided useful information on fractured and delaminated surfaces and provided evidence that strengthened the conclusions of this work. The proposed test methods in this work will be crucial to measure the shear mechanical properties in bulk material and thin substrates. Laminates of Al and LDPE or similar material can be studied using the developed simulation technique which can be effectively used for decision support in early package development.

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Cílem diplomové práce je popsat oxidaci nanotrubic sulfidu wolframičitého za zvýšených teplot v přítomnosti vodní páry. Na jejich povrchu se nejprve vytvoří nanočástice oxidu wolframu, ze kterých potom vyrůstají nanodráty. Na základě in-situ experimentů v rastrovacím elektronovém mikroskopu je navržen mechanismus reakce a ten je zjednodušeně popsán analyticky. Ukazuje se, že elektronový svazek má zásadní vliv na reakci.

Tato Diplomová práce se zabývá povrchovou analýzou nanokompozitní folie polyetherimidu (PEI) vyztuženého exfoliovanými grafitickými nanodestičkami (xGnP). Analyzovány byly take vzorky nevyztužené PEI folie a samostatné nanodestičky. Vzorky nanokompozitu a PEI folie byly plazmaticky leptány s využitím argonového plazmatu po dobu 1, 3 a 10 hod. Skenovací elektronová mikroskopie (SEM) byla použita pro charakterizaci samostatných nanodestiček rozptýlených na křemíkovém substrátu, původních či leptaných vzorků PEI folie a nanokompozitu. Nanodestičky byly identifikovány při povrchu leptané nanokompozitní folie. Mikroskopie atomárních sil (AFM) byla použita pro zobrazení povrchové topografie separovaných nanodestiček a odkrytých destiček při povrchu leptaného kompozitu. Povrchová drsnost (střední kvadratická hodnota, vzdálenost nejnižšího a nejvyššího bodu) leptaného nanokompozitu narůstala s prodlužující se dobou leptání. Akustická mikroskopie atomárních sil (AFAM) byla použita pro charakterizaci elastické anizotropie leptaných kompozitních vzorků. Nanoindentační měření umožnila charakterizaci lokálních mechanických vlastností PEI a nanokompozitních folií.

This graduation theses in introduction deals with principle and problems of electron signal detection in scanning electron microscopy and charging of insulating specimens in SEM. The experimental part of the thesis describe the methods of qualification and quantification of insulating specimen charging effect observed in environmental scanning electron microscope through the use of ionisation and scintillation detector in dependence on water vapour pressure in specimen chamber. The goal of the thesis is formation of the methodics useful to evaluate charging effect at insulating specimens observing and on the basis of measuring, determine optimal conditions for insulating specimen observation with ionisation and scintillation detector.

This thesis is interested in new materials for lithium – ion batteries. Two different samples were investigated, one intercalation and one conversion cathode material. The theoretical part is focused to the structure of cells, their advantages and disadvantages compared to other secondary batteries. Also other materials used in batteries are described. The practical part describes the preparation of cathode materials for subsequent testing by scanning elektron microscopy and thermogravimetric analysis. In conclusions two different materials were evaluated and compared with each other.

This master's thesis deals with study of the injected charge contrast mechanism of doped semiconductors by using the ultra – high vacuum scanning low electron energy microscope (UHV SLEEM). The aims of this work were to explain the injected charge contrast mechanism, to ability of this contrast mechanism to map the dopant density quantitatively and to identify the influencing factors.

This diploma thesis deals with preparation and characterization of aqueous solutions of polyvinyl alcohol suitable for electrospinning. In the theoretical part method of electrospinning is described, including parameters which influence this process. Literary research also includes a chapter about rheology, which deals with the rheological properties of polymers, specifically PVA. The experimental part describes the preparation and rheological study of of aqueous solutions of polyvinyl alcohol, which were then spun. The morphology of prepared nanofibers was studied by using scanning electron microscopy (SEM). The effect of molecular weight, the solvent, concentration of solution, rheological properties, electrical conductivity and surface tension on the spinability, diameter and morphology of nanofibers is discussed.

<p>U ovom radu prikazani su rezultati ispitivanja termičkih, mehaničkih, električnih i optičkih karakteristika kvazibinarnih halkogenida iz sistema Bi-As2S3. Na osnovu termičkih merenja analizirana je kinetika kristalizacionih i predkristalizacionih procesa i utvrđen je mehanizam dekompozicije za različite sastave dobijenih stakala. Primenom impedansne spektroskopije kvantitativno su ocenjeni doprinosi relaksacionih procesa na pojedinim temperaturama u ukupnoj polaraziciji za stakla sa 5 i 7 at.% Bi. Na osnovu merenja Raman spektroskopije identifikovane su nastale strukturne jedinice i konstatovana pojava nanofazne separacije u staklima sa 1.5 i 3 at.% Bi. Mehanička merenja ispitivanih halkogenida različitog sastava ukazala su na povećanje Vickers-ove tvrdoće sa povećanjem udela primesnih atoma. Na osnovu procenjene vrednosti modula elastičnosti ustanovljeno je da uzorak sa 5 at.% Bi odlikuje najgu&scaron;će atomsko pakovanje. Merenja električnih karakteristika u jednosmernom režimu (DC) pokazala su da je udeo lokalizovanih stanja u ukupnom mehanizmu provođenja značajan samo za manje koncentracije primesnih atoma, a da za veće koncentracije dominantan faktor postaju preskoci između delokalizovanih stanja. Skok u provodljivosti za nekoliko redova veličine kod sastava sa složenijom strukturom protumačen je kao posledica fazne separacije. Rezultati&nbsp; ACmerenja dobijeni za sastav sa 5 at.% Bi ukazali su da je u mernom frekventnom intervalu i dalje dominantan mehanizam termičke aktivacije nosilaca naelektrisanja. Kod sastava sa maksimalnim sadržajem Bi uočena je promena provodljivosti u funkciji frekvencije na svim temperaturama, a dobijeni rezultati su u skladu sa postavkama modela korelisanih preskoka barijere (CHB model).</p> / <p>This paper presents the results of investigation ofthermal, mechanical, electrical and optical propertiesof quasibinar chalcogenides from the system Bi-As2S3.&nbsp;Kinetics analysis of softening and crystallizationprocesses was done on the basis of thermalmeasurements, as well the analysis of decompositionmechanism for different compositions of obtainedglasses. The application of impedance spectroscopy enabled quantitative description of relaxation process contributions at selected temperatures in the overallpolarization for the samples with 5 and 7 at.% Bi.&nbsp;Based on measurements of Raman spectroscopy identification of structural units in the investigated chalcogenides was made, as well as the appearance of&nbsp;nano-scale phase separation in the glasses with 1.5 and 3 at.% Bi. Mechanical measurements pointed to the increase of the Vickers hardness with increase of&nbsp;doping atoms content. &nbsp;Based on the estimated value of the modulus of elasticity it was found that the sample &nbsp;with 5 at.% Bi is characterized by the densest atomic&nbsp;arrangement. Measurements of the electrical properties in dc regime (DC) pointed out that the share of localized states in the whole mechanism of conduction&nbsp;is significant only for the smaller concentrations of doping atoms. For the samples with higher concentrations dominant &nbsp;factor in conductivity are transitions between delocalized states. The jump in conductivity by few orders of magnitude, noticed for&nbsp;the compound with heterogeneous structure was interpreted as a consequence of micro-scale phase&nbsp; separation. Results of&nbsp; ACmeasurements for the&nbsp; composition with 5 at.% Bi showed that the mechanism of thermal activation of charge carriers is&nbsp;still dominant in the measured frequency range. For&nbsp;&nbsp; the composition with the maximum content of Bi changes in conductivity versus frequency were observed at all temperatures, and the results were interpreted in accordance with the model of correlated hopping over the barrier (CHB).</p>