Mechanical Properties of Microstructural Components of Inorganic Materials

Disertační práce se zabývá studiem strukturních a mechanických vlastností anorganických materiálů. Cílem je nalezení jednotlivých fází ve zkoumaném materiálu a hlavně lokalizace (mechanicky) nejslabšího místa, jeho ovlivnění a následně výroba materiálu o lepších mechanických vlastnostech. Z důvodu velkého množství použitých metod je základní teorie vložena vždy na začátku příslušné kapitoly. Taktéž z důvodu značného množství výsledků jsou na konci kapitol uvedeny dílčí závěry. Práce je rozdělena na tři části, kdy první se zabývá seznámením s možnostmi modelování mikro-mechanických vlastností a provedením experimentů umožňujících posouzení rozsahu platnosti některého modelu. V druhé části je provedeno shrnutí současných možností indentačních zkoušek pro měření mechanických vlastností strukturních složek betonu a praktické zvládnutí metodiky vhodné k užití pro výzkum materiálů zkoumaných domovským pracovištěm. V třetí části je navržena metoda identifikace nejslabších článků struktury anorganických pojiv a její ověření na konkrétním materiálu zkoumaném na domovském pracovišti. V této dizertační práci jsou použity tyto metody: kalorimetrie, ultrazvukové testování, jednoosá pevnost v tlaku, nanoindentace, korelativní mikroskopie a rastrovací elektronová mikroskopie s energiově disperzním spektrometrem. Dílčími výsledky jsou kompletní charakterizace cementových materiálů, upřesnění stávajících poznatků a nalezení optimálního postupu pro charakterizaci. Hlavním výsledkem je inovativní přístup vedoucí k pozitivnímu ovlivnění materiálu.The doctoral thesis deals with study of structural and mechanical properties of inorganic materials. Goal is to find the weakest (mechanically) phases and interfaces of material. By affecting these structures it should be possible consequently produce a material with better mechanical properties. Due to the large amount of used methods the basic theory is discussed always in the beginning of relevant chapter. Similarly, due to the considerable amount of results every chapter includes partial conclusions. The work is divided in three parts. The first deals with the introduction of the possibilities of modeling micro-mechanical properties and performing of experiments that allow assessment of the scope of some model. In second part itis performed an overview of current possibilities of indentation tests for measuring mechanical properties of structural components of concrete and the practical managing of methods suitable for use for materials research examined at our faculty. In third part the method of identifying the weakest points in structure of inorganic binders is proposed and validation on the particular material examined at our faculty is performed. The methods used in this doctoral thesis are: calorimetry, ultrasonic testing, uniaxial compression, nanoindentation, correlative microscopy and scanning electron microscopy with energy dispersive spectrometer. Partial results are a complete characterization of cementitious materials, specification of existing knowledge and finding the optimal procedure for characterization. The main result is an innovative approach that leads to a positive effect on the material.

Local tests of mechanical properties of materials

Tato práce se zabývá studiem měření tvrdosti a mikrotvrdosti ve vztahu ke struktuře homogenních a heterogenních materiálů. V úvodní části práce je vysvětleno základní teoretické pozadí, tedy definice pojmů a popis principů měření tvrdosti, mikrotvrdosti, pevnosti v tahu, tlaku, ohybu a základní vyhodnocovací vztahy. Je podána stručná rešerše, poukazující na využitelnost uvedených principů v materiálovém inženýrství. Následuje popis experimentálních zařízení a přípravy vzorků. Jádrem práce jsou výsledky vlastních měření a vyhodnocení vztahů mezi nimi. Vyvrcholením práce je stanovení závislosti mechanických vlastností mezifázového rozhraní v geopolymerním materiálu v korelaci s gradientem chemického složení v této soustavě.This thesis deals with measurement of hardness and microhardness in relation to structure of homogeneous and heterogeneous materials. In the introduction basic theoretical background is commented, i.e. definitions, terminology, principles of measuring techniques for estimation of hardness, microhardness, tensile strength, compressive strength and bending strength. Follows a brief review of present research results focused on use of described principles in materials engineering. Then the experimental equipment and sample preparation is described. The crucial part of the thesis is summary of achieved results of original measurement and discussion of their relations to each other. Finally, the groundbreaking estimation is described, showing the correlation of chemical composition gradient and mechanical properties in interfacial zone of geopolymeric material.

Effect of Quench Environment on the Conversion Coatings on Magnesium Alloy AZ91

The aim of the study is to achieve fine microstructure of AZ91, due to the optimized heat treatment processes, which can be easily coated with a normal conversion process as phosphating. Determination of the influence of the AZ91 microstructure, mainly precipitates which are created using different cooling media during the heat treatment and definition of the best heat treatment process parameters are the main experimental sections of the work. The structure of the samples heat treated under different conditions was subsequently compared with the structure of the as cast state of AZ91. The morphology of the conversion coating was studied by scanning electron microscopy (SEM) and amount of individual elements in the deposited coating was determined by EDS analysis

The effect of heat-treatment on properties of Ni-P coatings deposited on AZ91 magnesium alloy

The present study reports the effect of phosphorus content in deposited electroless nickel (Ni–P) coatings, the heat treatment on the microhardness and its microstructural characteristics, and the influence of the temperature on the microstructure of the Mg alloy substrate during the heat treatment. The deposition of Ni–P coatings was carried out in the electroless nickel bath, and the resulting P content ranged from 5.2 to 10.8 wt.%. Prepared samples were heat-treated in the muffle furnace at 400 °C for 1 h after the coating deposition. The cooling of the samples to room temperature was proceeded in the air. For as-deposited and heat-treated samples, it was determined that with the increasing P content, the microhardness was decreasing. This may be caused by the changes in the structure of the Ni–P coating. The X-ray diffraction patterns of the as-deposited Ni–P coatings showed that the microstructure changed their nature from crystalline to amorphous with the increasing P content. The heat treatment of prepared samples led to the significant increase of microhardness of Ni–P coatings. All the heat-treated samples showed the crystalline character, regardless of the P content and the presence of hard Ni3P phase, which can have a positive effect on the increase of microhardness. The metallographic analysis showed changes of substrate microstructure after the heat treatment. The prepared coatings were uniform and with no visible defect

Effect of process conditions for the preparation of a manganese-based coating on the surface of AZ31 magnesium alloy

Manganese-based coatings on AZ31 magnesium alloy with Mg(OH)2 interlayer were prepared by hydrothermal reaction under different process conditions (temperature, time, and concentration). The harsh reaction conditions provided coatings with defects. These defects enabled the corrosive environment penetrated to the magnesium alloy which impaired the corrosion properties of AZ31 alloy. Optimal conditions included a temperature of 120 °C, 0.25 M MnCl2, and a reaction time of 1 h. The prepared coating was mainly composed of Mn3O4, which consisted of nanosized crystals of polyhedral shape. Potentiodynamic polarization measurements showed that the coating had very good corrosion resistance in 0.15 M NaCl. Future work will focus on the potential use of the manganese-based coating in biomedical applications. © 2023 Sciendo. All rights reserved

Improving the corrosion resistance of AZ31 magnesium alloy by preparing hydroxyapatite with a superhydrophobized surface

Magnesium and its alloys are promising materials that have potential mainly in the field of transport (e.g. automobile industry) and medicine (e.g. orthopedic implants). Their disadvantage is poor corrosion resistance, which limits their wider use in practice. Therefore, surface treatment by various methods is performed in order to improve corrosion protection. The preparation of a superhydrophobic coating is an interesting approach because the hydrophobic coating minimizes contact of the corrosion medium with the magnesium substrate. In this work, the hydrothermally prepared hydroxyapatite coating on AZ31 magnesium alloy was superhydrophobized by myristic acid. The prepared coatings were characterized by determining contact angle and surface analysis using a scanning electron microscopy with energy dispersive spectroscopy and Fourier transformed infrared spectroscopy. The corrosion resistance of modified surfaces was examined by potenciodynamic polarization in 3.5 % NaCl

Characterization of Electroless Ni–P Coating Prepared on a Wrought ZE10 Magnesium Alloy

Electroless low-phosphorus Ni–P coating was deposited on a wrought ZE10 magnesium alloy including an advanced pre-treatment of the material surface before deposition. Uniform Ni–P coating with an average thickness of 10 µm was formed by 95.6 wt % Ni and 4.4 wt % P. The content of Ni and P was homogeneous in the entire cross-section of the coating. Applying the Ni–P coating to the magnesium substrate, the surface microhardness increased from 60 ± 4 HV 0.025 to 690 ± 30 HV 0.025. Using the scratch test, it was determined that deposited Ni–P coating exhibits a high degree of adhesion to the magnesium substrate. Electrochemical corrosion properties of Ni–P coating were analyzed using the polarization tests in 0.1 M NaCl, while the deposited Ni–P coating showed an improvement of the corrosion resistance when compared to the ZE10 magnesium alloy. Using the scanning electron microscopy analysis, it was determined that the fine morphology of the deposited Ni–P coating did not contain visible microcavities. The absence of macrodefects due to the adequate pre-treatment before coating was reflected on the mechanism of the coated ZE10 degradation in a 0.1 M NaCl solution

The formation of feldspar strontian (SrAl2Si2O8) via ceramic route: Reaction mechanism, kinetics and thermodynamics of the process

The reaction mechanism, the equilibrium composition, the temperature range of stability of formed intermediates as well as the kinetics and thermodynamics of activated state during the formation of monoclinic strontium-aluminum-silicate feldspar stroncian (SrAl2Si2O8) via the ceramic route from the mixture of SrCO3, Al2O3 and SiO2 is described in this work. Strontian does not appear up to the temperature of 1150 degrees C and is the only stable phase at the temperature >= 1600 degrees C. Three independent reactions lead to two parallel reaction pathways, i.e. the formation of strontian from single or binary oxides (1) and with Sr-gehlenite as the intermediate (2). Since the reaction rate constants ratio is higher than one (k(1)/k(2) > 1), the first reaction route is favored according to the Wegscheider principle. The kinetics of chemical reaction of 1.5 order corresponding to the kinetic function F-2/3 ((1 - alpha)(-1/2) - 1) was determined as the rate determining the mechanism of formation of strontian. The integral and differential methods show that the process requires average apparent activation energy of 229.3 kJ mol(-1). The determined average value of frequency factor is 2.1 x 10(5) S-

The Effect of Crystallization and Phase Transformation on the Mechanical and Electrochemical Corrosion Properties of Ni-P Coatings

This paper deals with the study of the crystallization and phase transformation of Ni-P coatings deposited on AZ91 magnesium alloy. Prepared samples were characterized in terms of surface morphology and elemental composition by means of scanning electron microscopy with energy-dispersive spectroscopy analysis. The results of X-ray diffraction analysis and differential scanning calorimetry suggested that increasing the phosphorus content caused Ni-P coatings to develop an amorphous character. The crystallization of Ni was observed at 150, 250, and 300 °C for low-, medium- and high-phosphorus coatings, respectively. The Ni crystallite size increased with increasing temperature and decreasing P content. Conversely, the presence of the Ni3P phase was observed at a maximum peak of 320 °C for the high-phosphorus coating, whereas the crystallization of the Ni3P phase shifted to higher temperatures with decreasing P content. The Ni3P crystallite size increased with increasing temperature and increasing P content. An increase in microhardness due to the arrangement of Ni atoms and Ni3P precipitation was observed. The deposition of as-deposited Ni-P coatings led to an improvement in the corrosion resistance of AZ91. However, the heat treatment of coatings resulted in a deterioration in corrosion properties due to the formation of microcracks