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This study aims to analyze the influence of process parameters used for hydrothermal synthesis of CaP coatings on their properties and to improve their corrosion resistance and biocompatibility compared to the substrat AZ31. The parameters monitored were deposition time, pH of the reaction mixture, and concentration of precursors in the reaction mixture. For the deposited CaP coatings on AZ31 magnesium alloy, the surface morphology and the number of structural defects were evaluated using scanning electron microscopy. Electrochemical corrosion properties were evaluated using polarization techniques in Hank’s solution. The results showed that the best properties were obtained for the sample prepared in a reaction mixture at 120 °C, pH 5 for a deposition time of 120 min, when the concentration of precursors in the reaction mixture was 0.30 mol/l Ca(NO3)2·4H2O and 0.28 mol/l NH4H2PO4. Under these conditions, the best electrochemical corrosion properties were achieved.

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.

An Fe-based coating was thermally sprayed onto the surface of AZ91 magnesium alloy via the High-Velocity-Oxygen-Fuel (HVOF) method. The thermally sprayed coating with a thickness of 530 ± 25 µm and a porosity of 0.7 ± 0.1% did not show any macrostructural defects and did not cause any degradation of the AZ91 alloy. Laser remelting of the surface layer of the sprayed coating resulted in the recrystallization of the structure and the disappearance of presented pores, splat boundaries, and other defects. This led to an increase in the hardness of the remelted layer from the original 535 ± 20 HV0.3 up to 625 ± 5 HV0.3. However, during the laser remelting at a laser power of 1000 W, stress cracking in the coating occurred. The tribological properties were evaluated by the ball-on-plate method under dry conditions. Compared to the uncoated AZ91 magnesium alloy, a higher value of friction coefficient (COF) was measured for the as-sprayed coating. However, there was a decrease in wear rate and weight loss. The remelting of the surface layer of the as-sprayed coating led to a further decrease in the wear rate and weight loss. Based on the obtained data, it has been shown that the application of laser-remelted thermally sprayed Fe-based coatings on AZ91 Mg alloy improves hardness and tribological properties compared to bare Mg alloy and as-sprayed Fe-based coatings.

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.

Humic acids are a heterogeneous mixture of organic compounds that are naturally found in water and soil. In recent years, there has been a growing interest in the application of green fertilizers containing humic acids in agricultural activities. Water-soluble fraction of humic acid (WSHA) can be released from these fertilizers and subsequently interact with metallic materials (e.g. steel) located in soils and waters. WSHA were leached from an aqueous suspension of humic acids isolated from South Moravian lignite. Corrosion tests were performed on a low-carbon steel using a potentiodynamic polarization test and electrochemical impedance spectrometry. Results suggest that corrosion was initially promoted due to the formation of complex compounds of water-soluble humic acids with released iron ions. After a long time, a positive effect of WSHA was observed as the corrosion resistance of low-carbon steel increased.

Pure Mg samples were prepared by powder metallurgy using the cold and hot compacting methods. Cold compacted pure Mg (500 MPa/RT) was characterized by 5% porosity and the mechanical bonding of powder particles. Hot compacted samples (100 MPa/400 °C and 500 MPa/400 °C) exhibited porosity below 0.5%, and diffusion bonding combined with mechanical bonding played a role in material compaction. The prepared pure Mg samples and wrought pure Mg were subjected to corrosion tests using electrochemical impedance spectroscopy. Similar material corrosion behavior was observed for the samples compacted at 500 MPa/RT and 100 MPa/400 °C; however, hot compacted samples processed at 500 MPa/400 °C exhibited longer corrosion resistance in 0.9% NaCl solution. The difference in corrosion behavior was mainly related to the different binding mechanisms of the powder particles. Cold compacted samples were characterized by a more pronounced corrosion attack and the creation of a porous layer of corrosion products. Hot compacted samples prepared at 500 MPa/400 °C were characterized by uniform corrosion and the absence of a layer of corrosion products on the specimen surface. Powder-based cold compacted samples exhibited lower corrosion resistance compared to the wrought pure Mg, while the corrosion behavior of the hot compacted samples prepared at 500 MPa/400 °C was similar to that of wrought material.

A sequential chemical extraction with a defined series of eluotropic organic solvents with an increasing polarity (trichloromethane < ethyl acetate < acetone < acetonitrile < n-propanol < methanol) was performed on peat-bog humic acid. Six organic fractions were obtained and subjected to a physicochemical characterization utilizing methods of structural and compositional analysis. Advanced spectroscopic techniques such as Attenuated Total Reflectance (ATR-FTIR), total luminescence, and liquid-state 13C NMR spectrometry were combined with elemental analysis of the organic fractions. In total, the procedure extracted about 57% (wt.) of the initial material; the individual fractions amounted from 1.1% to 19.7%. As expected, the apolar solvents preferentially released lipid-like components, while polar solvents provided organic fractions rich in oxygen-containing polar groups with structural parameters closer to the original humic material. The fraction extracted with acetonitrile shows distinct structural features with its lower aromaticity and high content of protein-like structural motifs. The last two—alcohol extracted—fractions show the higher content of carbohydrate residues and their specific (V-type) fluorescence suggests the presence of plant pigment residues. The extraction procedure is suggested for further studies as a simple but effective way to decrease the structural complexity of a humic material enabling its detail and more conclusive compositional characterization.

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.

The corrosion behavior of duplex Ni-P coatings deposited on AZ91 magnesium alloy was studied. The electroless deposition process of duplex Ni-P coating consisted in the preparation of low-phosphorus Ni-P coating (5.7 wt.% of P), which served as a bond coating and high-phosphorus Ni-P coating (11.5 wt.% of P) deposited on it. The duplex Ni-P coatings with the thickness of 25, 50, 75 and 100 µm were deposited on AZ91 magnesium alloy. The electrochemical corrosion behavior of coated AZ91 magnesium alloy was investigated by electrochemical impedance spectroscopy and potentiodynamic polarization method in 0.1 M NaCl. Obtained results showed a significant improvement in the corrosion resistance of coated specimens when compared to uncoated AZ91 magnesium alloy. From the results of the immersion tests in 3.5 wt.% NaCl, 10% solution of HCl and NaOH and 5% neutral salt spray, a noticeable increase in the corrosion resistance with the increasing thickness of the Ni-P coating was observed.

Cílem bakalářské práce bylo studium sorpčních vlastností a fyzikálně-chemická charakterizace huminových kyselin před a po adsorpci. Byly provedeny sorpční experimenty na methylenové modři a rhodaminu 6G. Adsorpční izotermy byly získány pomocí UV/Vis spektrometrie. K vyhodnocení experimentálních dat byla využita Langmuirova izoterma. Standard HK izolované z Leonarditu byl charakterizován pomocí elementární a termogravimetrické analýzy, dále pak za použití infračervené spektrometrie s Fourierovou transformací, analyzátoru povrchu částic a v neposlední řadě i potenciometrickou titrací., Bachelor thesis deals with a sorption properties and physical-chemical characterization of humic acids before and after the adsorption. Sorption experiments with a methylene blue and a rhodamin 6G were performed. Adsorption isotherms were obtain via UV/VIS spectrometry. The Langmuir isotherm was used to evaluate the experimental data. Standard of HA isolated from Leonardite was characterized by an elemental and thermogravimetric analysis, by a Fourier-transform infrared spectroscopy, a surface area analysis and also by a potentiometric titration.

Předložená práce se zabývá studiem huminových látek (HL) izolovaných z vermikompostovaného přírodního odpadu pomocí spektrometrických metod. Hlavním cílem bakalářské práce je studium fyzikálně-chemických vlastností huminových látek za pomocí moderních instrumentálních technik, jako jsou molekulová absorpční spektrometrie v ultrafialové a viditelné oblasti elektromagnetického záření (UV/Vis), infračervená spektrometrie s Fourierovou transformací (FTIR), dále pak elementární analýza (EA), termogravimetrická analýza (TGA) a emisní spektrometrie s indukčně vázaným plazmatem (ICP OES). V teoretické části je vypracována rešerše zaměřená na základní informace o HL, kde je popsáno jejich rozdělení i struktura a v neposlední řadě jejich využití v oblasti medicíny, průmyslu či ekologii. Též jsou popsány některé metody, které jsou využívány za účelem studia HL. Nezbytnou součástí práce byla izolace huminových a fulvinových kyselin z vermikopostovaného přírodního odpadu. Z naměřených UV/Vis spekter byly vypočítány absorpční koeficienty, které sloužily k následné charakterizaci HK a FK. FTIR spektra byla využita k určení funkčních skupin studovaných HL. Využitím elementární analýzy byl stanoven obsah biogenních prvků a na základě termogravimetrické analýzy byl určen celkový obsah vlhkosti a popela. Obsah stopového množství studovaných prvků byl stanoven za pomoci ICP-OES., This bachelor thesis deals with the study of humic substances isolated from vermicompost natural waste through spectrometric methods. The aim of this thesis is to study physicochemical properties of the humic substances through modern instrumental techniques such as molecular absorption spectroscopy in the ultraviolet and visible regions of electromagnetic radiation (UV/Vis), infrared spectroscopy with Fourier transformationn (FTIR), elemental analysis (EA), thermogravimetric analysis (TGA) and inductively coupled plasma emission (ICP OES). A research focused on basic information about the humic substances was developed in the theoretical part. A description about their distribution or structure was made and also their utilization in medicine, industry or ecology. Then, methods, which are used for study of the humic substances, were described as well. An essential part of the thesis was isolation of humic and fulvic acid from the vermicompost natural waste. Absorption coefficients were calculated from the measured UV/VIS spectrum which served to following characterization of HK and FK. FTIR spectrum was used to determination of functional groups of studied HL. An area of biogenic elements was specified using the elementary analysis. Total amount of studied trace elements was determined with with the help of ICP-OES.

Tato bakalářská práce se zabývá vlivem hyaluronanu s různou molekulovou hmotností na korozní chování hořčíkové slitiny AZ31 v prostředí fyziologického roztoku. Pro elektrochemické testy byly využity metody potenciodynamická polarizace (PDP) a elektrická impedanční spektroskopie (EIS). Povrchová a mikroskopická analýza byla provedena pomocí rastrovacího elektronového mikroskopu (SEM) a energiově disperzní spektrometrie (EDS). Pro charakterizaci korozního roztoku a povrchu slitiny AZ31 byly využitý ponorné testy., This bachelor’s thesis deals with the influence of hyaluronan with different molecular weight on the corrosion properties of magnesium alloy AZ31 in the environment of physiological solution. Potentiodynamic polarization (PDP) and electrical impedance spectroscopy (EIS) methods were used for electrochemical tests. Surface and microscopic analysis were performed using scanning electron microscope (SEM) and energy dispersive spectrometry (EDS). Immersion tests were used to characterize the corrosion solution and the surface of the AZ31 alloy.

Bakalářská práce se zabývá vlivem koncentrace glukosy na korozní chování hořčíkové slitiny AZ31 v prostředí fyziologického roztoku 0,9% NaCl. Teoretická část stručně shrnuje využití hořčíku a jeho slitin v medicínských aplikacích a nabízí náhled do současného stavu poznání vlivu glukosy na korozi těchto materiálů. V experimentální části bylo využito potenciodynamické měření a elektrochemická impedanční spektroskopie (EIS) pro sledování elektrochemického chování slitiny AZ31 ve fyziologickém roztoku v přítomnosti různých koncentrací glukosy. Analýza povrchu slitiny po korozi byla provedena pomocí rastrovacího elektronového mikroskopu (SEM) a energiově disperzní spektroskopie (EDS). Korozní prostředí bylo analyzováno měřením konduktivity, pH, emisní spektrometrií s indukčně vázaným plazmatem (ICP-OES) a kapalinovou chromatografií s vodivostním detektorem. Výsledky ukázaly, že glukosa v závislosti na koncentraci zhoršuje korozní odolnost slitiny AZ31 v 0,9% NaCl. V korozním prostředí byly identifikovány tři organické kyseliny, z nichž největší zastoupení má glukonová kyselina., This bachelor thesis deals with the influence of glucose concentration on corrosion behaviour of magnesium alloy AZ31 in saline solution. The theoretical part briefly summarises the use of magnesium and its alloys in biomedical applications and offers insight into the current state of knowledge of the effect of glucose on corrosion of these materials. In the experimental part, potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) were used to evaluate the electrochemical behaviour of AZ31 alloy in saline solution with varying concentrations of glucose. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to characterise post-corrosion surface of the alloy. The corrosion environment was analysed by measurement of conductivity, pH, inductively coupled plasma atomic emission spectroscopy (ICP-OES) and liquid chromatography with conductivity detector. Results showed that glucose, depending on concentration, impairs corrosion resistance of AZ31 alloy in 0.9% NaCl. Three organic acids were identified in the corrosion environment, of which gluconic acid is the most abundant.

Předmětem bakalářské práce byla příprava a charakterizace (morfologická a chemická) povlaků na bázi vrstvených podvojných hydroxidů (LDH) s yttriem na hořčíkové slitině AZ31 pro zlepšení korozní odolnosti slitiny. Povlaky byly připraveny za mírných a hydrotermálních podmínek a syntéza byla podpořena termodynamickými předpoklady. Korozní odolnost slitiny AZ31 s povlaky byla popsána potenciodynamickými měřeními a srovnána s čistou slitinou AZ31. Následoval popis morfologického a prvkového složení skrze SEM-EDS analýzu a potvrzení vzniku struktur, vypozorovaných touto metodou, bylo provedeno skrze FTIR analýzu. Nejlepším povlakem připraveným za mírných podmínek byl vzorek připravený při 90 °C po 24 h s koncentrací yttria 0,05 M a za hydrotermálních podmínek to byl povlak připravený při 120 °C po 30 h s koncentrací yttria 0,075 M. SEM-EDS a FTIR analýza neprokázala vznik MgY-LDH, nýbrž vznik Mg(OH)2. Yttrium bylo v povlacích minoritně zastoupeno, kde se mohlo nacházet, např. ve formě Y(OH)3. Bylo prokázáno, že yttrium má pozitivní vliv na přípravu povlaků ve srovnání se vzorkem připraveným bez yttria za stejných reakčních podmínek., The subject of the bachelor thesis was the preparation and characterization (morphological and chemical) of coatings based on layered double hydroxides (LDH) with yttrium on AZ31 magnesium alloy to improve the corrosion resistance of the alloy. The coatings were prepared under mild and hydrothermal conditions and the synthesis was supported by thermodynamic assumptions. The corrosion resistance of the AZ31 alloy with coatings was described by potentiodynamic measurements and compared with the pure AZ31 alloy. This was followed by a description of the morphological and elemental composition through SEM-EDS analysis, and confirmation of the formation of the structures observed by this method was performed through FTIR analysis. The best coating prepared under mild conditions was a sample prepared at 90 °C for 24 h with a yttrium concentration of 0,05 M and under hydrothermal conditions it was a coating prepared at 120 °C for 30 h with a yttrium concentration of 0,075 M. SEM-EDS and FTIR analysis did not show the formation of MgY-LDH but the formation of Mg(OH)2. Yttrium was minorly represented in the coatings where it could be present, e.g. as Y(OH)3. Yttrium was shown to have a positive effect on the preparation of the coatings compared to the sample prepared without yttrium under the same reaction conditions.