|
|
Nové metody přípravy vzorků pro moderní rastrovací elektronovou mikroskopii
Ambrož, Ondřej ; Čermák, Jan ; Mikmeková, Šárka
Moderní rastrovací elektronové mikroskopy (SEM) jsou vybaveny velmi sofistikovaným detekčním systémem, který umožňuje detekovat signální elektrony současně pomocí několika různě umístěných detektorů. Tímto způsobem dochází k filtraci signálních elektronů podle energie a úhlu. Efektivní filtrace signálu v rastrovací elektronové mikroskopii současně s možností použití velmi nízkých dopadových energií primárního svazku vede k extrémní citlivosti této metody na kvalitu povrchu vzorku a jeho stav. Současné metalografické metody přípravy vzorků začínají být nedostatečné pro pokročilé zobrazování v moderních SEM instrumentech. Klasická příprava vzorků se ukazuje jako nevhodná zejména pro nízkonapěťovou rastrovací elektronovou mikroskopii. V práci budou prezentovány první výsledky experimentů vlivu běžných metod přípravy na stav povrchu a možnost odlišení jednotlivých fází TRIP oceli pomocí pokročilých technik elektronové mikroskopie a budou také nastíněny možnosti nových postupů využívajících například robotizace.
|
|
|
Artifacts and errors in EBSD mapping of retained austenite in TRIP steel
Mikmeková, Šárka ; Jozefovič, Patrik ; Ambrož, Ondřej
The present work aims to demonstrate artifacts and errors in visualization of retained austenite phase in TRIP steel by an electron back-scattered diffraction (EBSD) technique. Retained austenite phases size and shape obtained by the EBSD are directly compared with a real image of these phases acquired by means of an atomic force microscopy (AFM). The effect of the step size parameter used for the EBSD analysis on the retained austenite phase fraction and morphology is discussed in detail and quantified. Surface roughness as a barrier for the imaging of fine features situated on a specimen surface is demonstrated.
|
|
|
Apparatus for automatic chemical etching of metallographic samples
Ambrož, Ondřej ; Čermák, Jan ; Mikmeková, Šárka
The microstructure of steels after mechanical polishing is revealed only by the application of a suitable etchant. To achieve adequate optical or electron microscope images, the specimen surface must be free of any artifacts. Chemical etching can be defined as a controlled corrosion process. The metal of the investigated material passes as cations into the etchant solution during the chemical etching reaction. Chemical etching is usually performed manually either by immersing the sample in the etchant with simultaneous stirring or by swabbing with a lint-free cloth soaked in the etchant. It is also extremely important to debug the process of removing the sample from the bath and subsequent cleaning. It is recommended to wash the sample after removal from the etchant with water (distilled or demineralized) or alcohol (ethanol, methanol, or isopropyl alcohol) and dry it properly (depending on the etchant and the etched material). The main problem with these processes is the human factor, which significantly contributes to the already limited repeatability. All operation steps must be performed by properly trained personnel in the field of occupational safety because hazardous substances are handled. A high manual dexterity is also needed. Training a new employee is a long-term process. Moreover, keeping the exact etching time can be a challenge and one second can decide success. These problems become more serious in the case of using surface sensitive analytical method, such as a low energy scanning electron microscopy, due to the high spatial resolution and extreme surface sensitivity. We have developed an apparatus for automatic etching of metallographic samples of purpose to overcome all above-mentioned difficulties. The apparatus and results of the first experiments will be presented.
|
|
|
Microstructural classification of multiphase steels by advanced microscopy and image analysis techniques
Jozefovič, Patrik ; Materna, Jiří (oponent) ; Mikmeková, Šárka (vedoucí práce)
Austenitic stainless steels have found application in various sectors due to their characteristic properties. Metastable character of some of them, which allows martensitic transformation, is connected with possible risks in form of decrease of toughness. For revelation of martensitic phase in a microstructure of the austenitic stainless steel, techniques such as electron backscatter diffraction (EBSD) in scanning electron microscope (SEM) are used. However, the EBSD is time-consuming and it requires high quality of metallographic specimen preparation. Goal of this thesis is to find other techniques, which allow separation of the phases in metastable austenitic stainless steel in the SEM, as well as optimization of metallographic specimen preparation for needs of the SEM. After fulfilment of these goals, the thesis focuses on possibility of usage of the so-called deep learning for purpose of automated separation of phases in micrographs from the SEM. For this purpose, 4 artificial neural networks based on different architectures were trained and their results were compared.
|
|
|
Návrh automatizovaného procesu elektrolytického leštění vzorků pro elektronový mikroskop
Čermák, Jan ; Szabari, Mikuláš (oponent) ; Mikmeková, Šárka (vedoucí práce)
Tato diplomová práce se zabývá automatizací procesu elektrolytického leštění, které se pro-vádí jako poslední krok při přípravě metalografických vzorků určených pro pozorování v elektronovém mikroskopu. Byl vypracován kompletní návrh hardwaru jednoúčelového stroje, který zajišťuje automatickou přípravu až šesti vzorků na jedno vložení. Součástí řeše-ní bylo navržení manipulátoru pro manipulaci se vzorky společně s chemicky odolným držá-kem vzorků vhodným pro automatický provoz. Konstrukce celého stroje byla navržena s ohledem na bezpečnost obsluhy. Součástí práce je detailní 3D model zařízení a návrh apli-kace pro měření v prostředí LabVIEW. Je zde popsáno budoucí fungování stroje včetně po-pisu softwarového řešení pro ovládání stroje a odesílání dat o procesu pro každý vzorek do databáze v souladu s principy průmyslu 4.0. V závěru jsou formulovány dosažené výsledky a návrh dalších kroků nutných pro realizaci stroje.
|
|
|
Advanced metallographic techniques for aluminum and its alloys
Rychlý, David ; Gejdoš, Pavel (oponent) ; Mikmeková, Šárka (vedoucí práce)
Main goal of this thesis is to optimize the metallographic preparation process of aluminium for specific needs of a scanning electron microscopy (SEM). The SEM is highly sensitive to surface quality and conventional sample preparation methods used for an optical microscopy (OM) become insufficient. The thesis focuses on optimizing and finding novel metallographic methods fulfilling high requirements of the SEM imaging. It requires perfect quality surface without any damage, such as preparation artifacts and scratches. A pure aluminium has been selected as an experimental material. Conventional and advanced metallographic techniques were tested and the most promising techniques were optimized. Several surface finish techniques were examined in order to obtain a perfect quality surface, such as colloidal sillica polishing and electropolishing. The surface quality was examined by the OM, the low voltage SEM, and a confocal microscopy. Finally, the metallographic technique providing the aluminium surface with minimum defects is established.
|
|
|
Study of secondary phases in trip steel by advanced sem and afm techniques
Mikmeková, Šárka ; Ambrož, Ondřej ; Hegrová, J. ; Aoyama, T.
The paper aims to demonstrate a modern scanning electron microscope (SEM) as a powerful tool for visualization of the secondary phases in TRIP steel. The TRIP steel specimens prepared by various metallographic techniques were imaged by the SEM and the secondary phases presence was confirmed by an electron back-scattered diffraction (EBSD) technique. The chemical polishing by 5 % HF in H2O2 for 10 seconds results in selective etching for each individual phase, as confirmed by an atomic force microscopy (AFM) and hybrid AFM-in-SEM techniques. The phases are easily distinguishable in the SEM micrographs created by the low energy high take-off angle signal electrons. The proposed sample preparation technique together with special SEM imaging conditions enables us accurate analysis of distribution of secondary phases within the TRIP steel matrix and moreover, the retained austenite is distinguishable from the martensite phase.
|
|
|
Trip steel specimen preparation for advanced sem and EBSD
Ambrož, Ondřej ; Mikmeková, Šárka ; Hegrová, J. ; Aoyama, T.
Modern scanning electron microscopy (SEM) allows observations of specimens with high surface sensitivity. The surface sensitivity is significantly affected by the accelerating voltages. With the development of the scanning electron microscopy, the requirements for the surface quality of samples increase. Metallographic methods originally intended for light microscopy become insufficient. The problem occurs especially with multiphase materials having a fine-grained structure. The investigated TRIP steel consists of a ferritic-bainitic matrix, retained austenite and martensite phases. The sizes of the smallest phases are nanometer units. The volume of residual austenite was determined by X-ray diffraction. The basic preparation of all tested samples involved conventional metallographic grinding and very fine mechanical polishing. One sample was analysed in this state. Other samples were subsequently chemically polished, electropolished and chemical-mechanically polished. The specimens were observed in the SEM using a SE and a BSE detector at low energies immediately after the preparation. An EBSD was performed in the same areas to characterize the retained austenite. Topographical imaging by special AFM, integrated into the SEM, demonstrated that the mechanical polishing results in surface deformation and residual austenite is transformed. All other methods have their specifics and for modern sensitive SEM instruments it is necessary to optimize individual procedures.
|
|
|
Pokročilé metody přípravy vzorků TRIP ocelí a jejich zobrazování moderními technikami rastrovacího elektronového mikroskopu
Ambrož, Ondřej ; Mikmeková, Šárka
Vícefázové oceli, mezi něž patří i TRIP oceli, vynikají svými excelentními mechanickými vlastnostmi a nacházejí uplatnění v mnoha odvětvích, jako je například automobilový průmysl. Studium mikrostruktury takovýchto materiálů je velmi obtížné, především s ohledem na rozlišení jednotlivých fází. U současně vyvíjených TRIP ocelí, vyznačujících se přítomností nano-fází ve struktuře, běžné charakterizační techniky selhávají a vzniká poptávka po vývoji nových technik, které umožní precizní charakterizaci fází v nano- měřítku. V této práci bude demonstrován přínos moderní rastrovací elektronové mikroskopie pro charakterizaci jednotlivých fází ve vybrané TRIP oceli.
|
|
| |
host ::
RSS.