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EN
The reaction of alkalis with aggregate containing reactive forms of silica (ASR) plays a significant role in shaping the durability of concrete, as the strongly hygroscopic reaction products generated lead to internal stress, causing its expansion and cracking. This study presents an extended analysis of corrosive processes occurring in mortars with reactive natural aggregate from Poland, using computed tomography and scanning microscopy methods. Numerous cracks in the grains and the surrounding cementitious matrix were observed, indicating a high degree of advancement of corrosive processes. Over time, the proportion of pores with reduced sphericity increased, indicating ongoing degradation of the mortars. The usefulness of computed tomography in studying the progress of ASR was demonstrated. Scanning microscopy confirmed that the cause of mortar degradation is the formed ASR gel with a typical composition, located within the volume of reactive grains, cracks propagating into the cementitious matrix, and accumulated in air voids.
EN
There are two arsenical pyrite (As-FeS2mineralization zones cropping out in the Podwiśniówka and Wiśniówka Duża quarries where quartzites and quartzitic sandstones have been extracted for over a century. A large amount of pyrite in the Wiśniówka siliciclastics is unusual in the hard rock mining throughout the world. The pyritiferous beds contain a variety of REE-bearing minerals, including a crandallite series of aluminum-phosphate-sulfate (APS) minerals, e.g., predominant goyazite SrHAl3[(PO4)2(OH)6] with subordinate gorceixite BaHAl3[(PO4)2(OH)6] and very occasional crandallite CaHAl3[(PO4)2(OH)6]. By contrast, the other REE-phosphate minerals, e.g., xenotime YPO4, bur particularly monazite CePO4 occur in a lesser amount. Goyazite prevails somewhat in the Podwiśniówka beds whereas xenotime in the Wiśniówka Duża beds. Of the other REE-bearing minerals, bastnäsite REECO3(F,OH), florencite (REE)Al3(PO4)2(OH)6 and synchysite CaCe[CO3]2F occur in trace amounts. Interestingly, the quite common phosphate minerals, i.e., wavellite (Al.3[(OH,F)3|(PO4)2]×5H2O and variscite Al[PO4]×2H2O) are depleted in REEs with only Ce attaining 0.09 wt.% as documented by an electron-probe microanalysis. In contrast to quartzites/quartzitic sandstones, carbonaceous clayey-silty shales and bentonites/tuffites are distinctly enriched in REE-bearing minerals. This diversity is also mirrored in the mean total REE concentrations varying from 204 to 314 mg/kg, in clayey-silty shales and bentonites, attaining 457 mg/kg in some Podwiśniówka shale beds. Results of this and the previous petrographic, mineralogical and geochemical studies have indicated that REE-bearing minerals formed generally along with As-rich pyrite, nacrite/dickite and probably TiO2 polymorphs as a result of multiphase hydrothermal vent activity that took place in the Wiśniówka Late Cambrian sedimentary basin. This evidence is also backed up by the values of LREENASC/HREENASC (1.44–1.75) and Eu/EuNASC (1.24–1.30) coefficients in the clayey-silty shales. This positive Eu anomaly (31.20) points to the formation of REE-bearing minerals in a reducing environment.
EN
Estimating the direct radiative forcing (DRF) by air particles is challenging because of uncertainty in the morphology (shape and size), mixing states, and chemical properties of fine particulates. To improve numerically estimated optical and radiative properties, a region-specific database of the aforementioned physico-chemical properties (at individual particle level) is required. PM2.5 samples were examined using scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDS). SEM-EDS was utilized to investigate the differences in forms, morphology, and elemental composition of PM2.5 particles, as well as to relate them to a potential source as a cause of pollution and pollution emissions and transit from various polluted places. SEM micrographs identified a wide range of PM morphologies, including spherical, irregular, angular, cluster, flaky, rod-like, crystalline, and agglomerate structures, indicating natural and anthropogenic causes and creation. The sources of PM2.5 pollution episodes in Raipur were identified employing observed pollution levels and meteorological data, backward air mass trajectories, correlation, and PMF analysis. In addition, positive matrix factorization has been used to source-apportion the data and five significant source/pollution types including industrial emissions (37%), vehicular exhaust (13.8%), coal combustion (12.4%), ionic factor (11.3%), and crustal dust (25.5%) were detected. Using a backward trajectory analysis, the influence of air pollutant transmission on regional particle pollution was investigated. A significant connection between Fe-Mn, Mn-Ni, Ni-Al, and Cl- and NH4+ indicates that the contaminants share a similar source. It was revealed that unfavorable climatic circumstances, such as low wind speed, low humidity, low temperature, and surface layer inversions, increase the risk of large PM2.5 concentrations in the region.
EN
Stone has been used in architecture since Antiquity. The processes of its deterioration in different buildings have always been associated with natural processes of its weathering (physical, chemical, biological). However, this situation has changed over centuries. Currently, air pollution (mainly in urbanised areas) has a significant impact on the accelerated weathering of stone monuments. The research presented in this paper concerns the deterioration of stone facade of the 19th century building of the National Archive in Poznań, where the latest factor (contemporary air pollution) plays the greatest role. Based on the ICOMOS glossary, selected forms of deterioration were described and classified in macro and micro scales. For this purpose, optical and scanning microscopy and X-ray diffraction were used. As a result of the research, lichen species composition and secondary mineralisation in the black crust were identified. Elements, such as: barium, zinc, lead, and iron, which were detected on the black crust, were directly related to anthropogenic pollution caused mainly by combustion and low emissions.
EN
This paper evaluates the efficiency of metal recovery from printed circuit boards (PCBs) using two gravity separation devices: a shaking table and a cyclofluid separator. The test results were compared with the results obtained from previous research, where an electrostatic separation process was used for an identically prepared feed. The feed for the separators consisted of PCBs shredded in a knife mill at cryogenic temperatures. The separation efficiency and purity of the products were evaluated based on microscopic analysis, ICP-AES, SEM-EDS, XRD, and specific density. The yield of concentrates (valuable metals) obtained from the shaking table and the cyclofluid separator amounted to 25.7% and 18.9%, respectively. However, the concentrate obtained from the cyclofluid separator was characterised by much higher purity, amounting to ~88% of valuable metals, compared to ~72% for the shaking table. In both cases, middlings formed a significant share, their yield amounting to ~25%, with the share of valuable metals of ~15%. The yield of waste obtained from the shaking table and the cyclofluid separator were 42.6% and 52.5%, respectively. In both cases, as a result of the applied process, the waste was divided into two homogeneous groups differing in grain size and shape. The recovery of metals through gravity separation is possible, in particular, by using a shaking table. These processes can also be applied to separate waste (plastics) into two groups to be selectively processed to produce new materials in line with a circular economy.
EN
Since its discovery, the Morasko meteorite has been the subject of many studies. Among the publications summarising the mineralogical and geochemical characteristics of the Morasko meteorite, two monographs are worth mentioning by: Dominik (1976) and Muszyński et al. (2012), in which the essentialfeatures of the Morasko meteorite were presented. Since the first piece of the Morasko meteorite was to be explored, the analysis of mineral composition has been conducted with more and more specialised and sophisticated instrumental methods. As it is well known, the Morasko meteorite is classified into the group of iron meteorites IAB MG, and consists mainly of the crystalline Fe-Ni alloy in the form of two minerals: kamacite and taenite, accompanied by tetrataenite. A commonly found structure of the mineral composition of the Morasko meteorite, as regards other iron meteorites, are graphite-troilite nodules, which contain silicate and phosphate minerals. This paper presents a review ofresearch on the mineralogy and geochemistry of the Morasko meteorite, where a number of instrumental tests have been used, from microscopic observations to microchemical semiquantitative analyses using scanning electron microscopy (SEM-EDS), microchemical quantitative analyses using an electron microprobe (WDS), to the structural methods applying Raman spectroscopy. The results of microscopic, microchemical and microstructural investigations, which have included the outer layer of the meteorite known as a fusion crust, have been presented against the petrographic composition of the meteorite. Besides, the type of sediment attached to the outer meteorite layer was examined. The research, conducted on two dozen meteorite fragments, allowed distinguishing two different zones concerning mineralogy and geochemistry, and to determine microstructural changes within them, most probably created in the processes related to the moment of the meteorite impact.
EN
Sandstones are a commonly used stone in the architecture of Poznań. They are constantly affected by deterioration processes. This is mainly linked to pollution, which is a consequence of the city development. This is manifested, among others, by the emission of harmful substances from traffic routes, as well as the combustion of solid fuels in the city centre. The research is focused on the sandstone elevation of one of the monuments of the Royal-Imperial Route in Poznań - the current building of the University of Economics and Business in Poznań dated to the beginning of the 20th century. The research was carried out both -on a macro- and microscale. Taking into account the ICOMOS glossary (International Council on Monuments and Sites), the types of damage on the façade on a macroscale were classified. The most common problem was the black crust on the surface of stone panels. Thanks to the use of optical, scanning and cathodoluminescence microscopy, it was also possible to analyse various types of contaminants on a microscale that appear in the building elevation. As a result of the research, dust particles, metals such as lead, tin, zinc, iron, and sulphur and nitrogen compounds that were part of dust particles were found. Deterioration of the façade caused by soiling derived from traffic-related particulate matter, deposition of nitrates from exhaust and other emission sources may seriously impact natural building stones.
EN
The subject of the research was the Middle Miocene red algal limestone from the Włochy deposit, which is currently the only place of exploitation of the Pińczów Limestone representing a local type of the Leitha Limestone. The collected samples of this rock belong to the organodetric facies of diverse grain size and sorting of clastic material. Considering the proportions of characteristic skeleton remains, the composition of the coarse-grained organodetric facies is red algal-foraminiferalbryozoic, while of the fine-grained facies is foraminiferal-red algal. The cement of these rocks is predominantly sparite compared to micrite-clay matrix. A complement to petrographic studies was the chemical analysis and identification of mineral phases with X-ray diffraction. Moreover, physical and mechanical properties of samples were analyzed. Porosity of the rock was assessed in the polarizing and scanning microscope (SEM-EDS) observations, as well as with a porosimetric tests. The coarse-detrital limestone with a dominant binder in the form of intergranular cement is characterized by the apparent density sometimes exceeded 1.90 Mg/m3, while fine-grained limestone has the highest water absorbability (above 20%) and total porosity (about 40%). The above properties influenced high water absorption by capillarity, limiting the possibility of using limestone in places exposed to moisture. The observed relationship between the ultrasonic waves velocity and the uniaxial compressive strength gives the possibility of predicting the value of the latter parameter in the future. The limestones from Włochy deposit do not differ in quality from the previously used Pińczów Limestones, and their technical parameters predestine them for use as cladding material with insulating properties.
PL
Przedmiotem badań były środkowomioceńskie wapienie krasnorostowe ze złoża Włochy, jedynego obecnie miejsca eksploatacji wapieni pińczowskich, reprezentujących lokalny typ wapieni litawskich. Pobrane próbki tych skał reprezentują fację organodetrytyczną o zróżnicowanym uziarnieniu i wysortowaniu materiału okruchowego. Biorąc pod uwagę proporcje charakterystycznych szczątków szkieletowych, skład facji gruboziarnistej jest krasnorostowo-otwornicowo-mszywiołowy, zaś drobnoziarnistej – otwornicowo-krasnorostowy. Spoiwo tych skał stanowi cement sparytowy, przeważający nad matriks mikrytowo-ilastą. Uzupełnieniem obserwacji petrograficznych była analiza składu chemicznego i identyfikacja faz mineralnych przy pomocy dyfraktometrii rentgenowskiej (XRD). Ponadto wykonano badania właściwości fizycznych i mechanicznych. Porowatość skały oceniono na podstawie obserwacji w mikroskopie polaryzacyjnym i skaningowym (SEM-EDS) oraz w testach porozymetrycznych. Wapienie grubodetrytyczne z dominującym spoiwem w postaci cementu intergranularnego odznaczają się gęstością pozorną przekraczającą czasem 1,90 Mg/m3, podczas gdy drobnoziarniste mają najwyższą nasiąkliwość wagową (pow. 20%) i porowatość całkowitą (ok. 40%). Wpływa to na wysoką nasiąkliwość kapilarną, ograniczającą możliwości zastosowania wapienia w miejscach narażonych na zawilgocenia. Stwierdzona zależność pomiędzy prędkością fal ultradźwiękowych a wytrzymałością na ściskanie jednoosiowe daje możliwość prognozowania wartości tego ostatniego parametru w przyszłości. Wapienie ze złoża Włochy mają jakość podobną do innych wapieni pińczowskich eksploatowanych w przeszłości, a ich parametry techniczne predestynują je do zastosowania jako materiału okładzinowego o właściwościach izolacyjnych.
PL
Trzy piętnastowieczne witraże z klasztoru OO. Dominikanów w Krakowie: Tron Łaski, Maria ze sceny Zwiastowania i Chrystus z aniołem ze sceny Koronacji Marii były przedmiotem analiz technologii oraz stanu zachowania. W celu wyznaczenia składu chemicznego szkieł zastosowano trzy techniki analityczne: MA-XRF (makro-skaning fluorescencji rentgenowskiej), SEM-EDS (skaningowa mikroskopia elektronowa z mikroanalizatorem fluorescencji rentgenowskiej) i LA-ICP-MS (spektrometria mas z jonizacją próbki w plazmie indukcyjnie sprzężonej po ablacji laserowej). Na podstawie zawartości głównych składników szkłotwórczych oraz niektórych pierwiastków śladowych możliwa była identyfikacja szkieł w witrażach wykonanych przez ten sam warsztat. Badane szkła wykazały podobieństwa w zakresie zawartości krzemionki oraz proporcji tlenku potasu do tlenku wapnia.
EN
Three 15th century stained-glass panels The Throne of Grace, the Virgin Mary at the Annunciation and Christ and an Angel at the Coronation of the Virgin from the Dominican Monastery in Kraków were subjects of physicochemical analyses. MAXRF (macro X-ray fluorescence scanning), SEM-EDS (scanning electron microscope equipped with energy-dispersive X-ray spectrometry) and LA-ICP-MS (laser ablation inductively coupled plasma mass spectrometry) were utilized for determination of chemical composition of glass panes. Establishing of basic composition and analysis of trace elements allowed to compare panels, which are considered as made by the same stained-glass workshop. Analyses revealed similarities in the amount of silica and relation of potassium oxide to calcium oxide between glass panes.
PL
Przedstawiono wybrane rezultaty analizy składu pierwiastkowego na czynnej powierzchni ściernic impregnowanych węglem amorficznym po procesie szlifowania stopu Titanium Grade 2®, wykonanej z zastosowaniem spektroskopii dyspersji energii promieniowania rentgenowskiego (SEM-EDS). Uzyskane wyniki wskazują na skuteczne wprowadzenie impregnatu bezpośrednio do strefy styku aktywnych wierzchołków skrawających z materiałem obrabianym.
EN
In the paper the selected results of analysis of the state of amorphous carbon treated grinding wheel active surface after grinding of Titanium Grade 2® using SEM-EDS technique were presented. The obtained results indicate the effective input of impregnating substance directly into the contact zone between abrasive grains and workpiece surface.
EN
The subject of this study are polychromes in a tenement house in the Old Market Square, Poznan. The main aim of this research was to identify a palette of pigments used in the interior wall paintings. Cross-sections of polychromes, which are dated to the fifteenth century and later, were analysed. Petrographic analysis, especially in reflected light, electron microscopy (SEM-EDS) method, infrared imaging technique (FTIR-ATR) and Raman microspectroscopy were used. The following pigments were identified: minium, red ochre, litharge, massicot, orpiment, yellow ochre, malachite, chalk, lead white, lamp black and vine black.
EN
In many fields of science and technology, it is necessary to apply non-destructive methods of analysis. Such non-destructive methods include scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM/EDS) and X-ray photoelectron spectroscopy (XPS), and the results obtained with this set are often regarded as complementary. These methods were used in this study to research the chemical composition of the top layer of a model made with gold on a ceramic coating produced by the PVD technique on the surface of steel. The gold layer was ion sputtered until its complete removal and was studied by means of X-ray photoelectron spectroscopy and X-ray micro-analysis. It was found that the analytical data for an identical specimen obtained by SEM/EDS and XPS might differ significantly. This necessitates very careful consideration in treating these techniques as complementary, and during the interpretation of the results, one should take into account the physical essence of each method.
PL
W wielu dziedzinach nauki i techniki niezbędne jest zastosowanie nieniszczących metod analizy. Do takich metod należy skaningowa spektroskopia elektronów sprzężona z mikroanalizą rentgenowską (SEM/EDS) oraz rentgenowska spektroskopia fotoelektronów (XPS), a wyniki uzyskiwane za ich pomocą często są traktowane jako uzupełniające się. W pracy zastosowano te metody do badania składu chemicznego modelowej warstwy wierzchniej, utworzonej ze złota na podłożu powłoki ceramicznej wytworzonej techniką PVD na powierzchni stali. Warstwę złota trawiono jonowo aż do jej całkowitego usunięcia i badano za pomocą rentgenowskiej spektroskopii fotoelektronów oraz mikroanalizy rentgenowskiej. Stwierdzono, że dane analityczne dla identycznej próbki uzyskiwane metodami SEM/EDS oraz XPS mogą dość istotnie różnić się. Oznacza to konieczność dużej ostrożności przy traktowaniu tych technik jako komplementarne, podczas interpretacji wyników należy uwzględniać fizyczną istotę obydwu metod.
13
Content available remote Badania mechanizmu dehydratacji uwodnionego glinianu wapniowo-cyrkonowego
PL
W pracy przedstawiono wyniki badań składu fazowego oraz mikrostruktury zaczynu glinianu wapniowo-cyrkonowego (układ Ca7ZrAl6O18-woda) sezonowanego w warunkach otoczenia, a następnie poddanego obróbce termicznej w zakresie temperatur 100-900 °C. Wykorzystano następujące metody pomiarowe: XRD, FT-IR oraz SEM/EDS. Dehydratacja heksagonalnych hydratów C-A-H (C ≡ CaO, A ≡ Al2O3, H ≡ H2O), powstałych w zaczynie Ca7ZrAl6O18-woda sezonowanym w temperaturze otoczenia, przechodzi częściowo przez stadium pośrednie tworzenia się C3AH6 w warunkach odparowania wody fizycznie związanej i częściowego usunięcia wody chemicznie związanej, a następnie rozkładu hydratów do bezwodnych glinianów wapnia typu faz C5A3, C12A7 i C3A. Dodatkowo w badanym układzie stwierdzono obecność fazy o nieznanym dotąd składzie chemicznym, należącej do układu CaO-Al2O3-ZrO2, która utworzyła otoczkę na niezhydratyzowanych ziarnach Ca7ZrAl6O18, a także cyrkonian wapnia – CaZrO3.
EN
In this paper, the results of investigation of the phase composition and microstructure of hydrated calcium zirconium aluminate paste are presented. The paste was first cured at room temperature, and then additionally heat treated at a temperature located within a temperature range of 100-900°C. The XRD, FT-IR and SEM/EDS techniques were used for characterization of the hydrated and dehydrated samples. The dehydration process of hexagonal calcium aluminate hydrates C-A-H (C ≡ CaO, A ≡ Al2O3, H ≡ H2O) proceeded through a transitory stage of the C3AH6 formation due to evaporation of physically bonded water, and partial removal of chemically bonded one; as a result, anhydrous calcium aluminates, C5A3, C12A7 and C3A were formed. Additionally, both an unknown ternary compound belonging the CaO-Al2O3-ZrO2 system, forming dehydrated rings on the unhydrated core of Ca7ZrAl6O18 grains, and calcium zirconate, CaZrO3, were identified.
PL
Celem pracy było zbadanie wpływu temperatury na odporność na zużycie elementów pokrytych powłoką AlCrN. Powłokę wytworzono w procesie osadzania fizycznego z fazy gazowej (PVD) na tarczach wykonanych z węglika wolframu. Badania tribologiczne w ruchu ślizgowym ciągłym przeprowadzono z wykorzystaniem stanowiska badawczego T-21 produkcji ITeE–PIB. W wyniku przeprowadzonych badań stwierdzono, że odporność na zużywanie skojarzenia z powłoką AlCrN zależała od temperatury. Największe zużycie odnotowano w temperaturze pokojowej. Natomiast w 600°C intensywność zużywania powłoki była 4-krotnie mniejsza, a w 750°C 6-krotnie mniejsza niż w temperaturze pokojowej. Mechanizm wysokotemperaturowej odporności na zużywanie powłoki AlCrN polega na utworzeniu tlenkowej warstwy ochronnej. Przeprowadzone analizy składu warstwy wierzchniej wskazały na znacznie większą zawartość tlenu w śladzie tarcia niż poza śladem. W wysokiej temperaturze proces tarcia dodatkowo intensyfikował utlenianie, a ilość tlenu wzrastała wraz ze wzrostem temperatury.
EN
The aim of the study was to investigate the effect of temperature on the wear resistance of coated parts AlCrN. The coating was prepared in the physical vapour deposition process (PVD) on the discs made of tungsten carbide. The testing in sliding motion conditions was performed using T-21 tribotester manufactured by ITeE–PIB. The results showed that the wear resistance of the AlCrN coating depends on the temperature. The largest wear rate was obtained at room temperature. In contrast, at 600°C the intensity of wear of the coating was 4-fold lower, and 750°C, 6-fold lower than at room temperature. The mechanism of high wear resistance of AlCrN coating is based on creation of oxide protective layer. Conducted analysis of the composition of the surface layer showed a significantly higher content of oxygen in the wear track than the outside track. At high temperature, friction process further intensified oxidation and the amount of oxygen increased with increasing temperature.
PL
W artykule dokonano szczegółowej analizy stanu ściernicy impregnowanej nowym typem impregnatu (węglem amorficznym) po procesie szlifowania prostoliniowo-zwrotnego walcowych powierzchni wewnętrznych wykonanych ze stopu Titanium Grade 2. W celu dokładnej identyfikacji śladów zużycia takiej ściernicy wywołanego szlifowaniem przeprowadzono analizy z użyciem elektronowej mikroskopii skaningowej (SEM – ang. Scanning Electron Microscopy) i spektroskopii dyspersji energii promieniowania rentgenowskiego (EDS – ang. Energy-dispersive X-ray Spectroscopy). Podczas badań eksperymentalnych zastosowano nowoczesną aparaturę obserwacyjno-pomiarową, w której skład wchodziły dwa elektronowe mikroskopy skaningowe JSM-5500LV firmy JEOL Ltd., Japonia i stacja robocza Auriga CrossBeam firmy Carl Zeiss Microscopy GmbH, Niemcy oraz zaawansowany detektor EDS Octane plus firmy EDAX, Inc., USA. Przeprowadzone analizy SEM-EDS pozwoliły na określenie udziału procentowego oraz kształtu i rozmieszczenia zalepień będących skutkiem adhezji wiórów Ti do czynnej powierzchni ściernicy oraz określenie udziału na niej substancji impregnującej (węgla amorficznego) po procesie szlifowania.
EN
In this paper, a detailed analysis of the condition of the grinding wheel impregnated with a new type of impregnate (amorphous carbon) on the reciprocal internal cylindrical grinding process of Titanium Grade 2. In order to accurately identify of wear symptoms caused on the grinding wheel during grinding process, analyzes were performed using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) techniques. During the experimental research modern instruments of observation and measurement were used: two scanning electron microscopes (JSM-5500LV by JEOL Ltd., Japan and workstation Auriga CrossBeam by Carl Zeiss Microscopy GmbH, Germany) as well as advanced EDS detector (Octane plus by EDAX, Inc., USA). Conducted SEM-EDS analysis made it possible to determine the percentage, the shape and arrangement of cloggings resulting from adhesion of Ti chips to the grinding wheel active surface and to determine the share of an amorphous carbon after the grinding.
EN
Alkali-aggregate reaction is an expansive chemical reaction between the alkalis present in cement paste and minerals contained in aggregates. Mineral admixtures can mitigate the detrimental processes caused by this reaction. One of the minerals that reduce the effects of the alkali-aggregate reaction is natural zeolite. This study attempts to explain the process that takes place in the zone surrounding reactive gravel in the cement mortar made with an addition of natural zeolite. Mortar bar expansion tests were performed and a scanning electron microscope equipped with an energy-dispersive X-ray spectrometer was used to observe the paste-aggregate interfacial zone. The results confirmed the influence of the zeolite on the reduction in reactive aggregate-based mortar expansion. The microstructure of the aggregatepaste interfacial region was described and particular sub-zones varying in terms of calcium, sodium, potassium and silicon contents were determined.
EN
This work presents the metallographical observations of the chosen copper objects from the Late Middle Ages. Part of these studies is the analysis of metal relics from the Puck area conducted at the Faculty of Foundry, AGH-UST, in collaboration with the University of Warsaw. Medieval European cities were centers of trade and production of metal artifacts. Also in the Puck area, the manufacturing activities can be confirmed based on the metal findings. The aim of this study was to identify and systematize copper alloys used in the Late Medieval Period, on the basis of historic artifacts from Puck. The chemical composition analysis and microstructure observation were carried out. The research is at the first stage of an experiment of reconstructing the medieval alloys in order to study deeper their properties.
EN
In order to impart photo-catalytic properties to fibres, one can modify them by means of titanium dioxide. Such a modification should provide the best effectiveness with no deterioration in the basic properties of the fibres modified. Accordingly the modifiers should be deposited on the surface of fibres instead of adding them to the whole mass of the fibreforming polymer. To characterise polypropylene fibres (PP) modified with titanium dioxide doped with nano silver (TiO2/Ag), Raman micro-spectroscopy and SEM/EDS microanalysis were used. The combination of both techniques in the analysis of the fibre surface and cross-section allows qualitative and structural assessment of the distribution of titania modifier in the fibre.
PL
Do nadawania włóknom funkcji fotokatalitycznych stosuje się modyfikacje ditlenkiem tytanu. Modyfikacja taka powinna zapewnić najlepszą efektywność fotokatalityczną bez pogorszenia podstawowych właściwości modyfikowanych włókien. W związku z tym modyfikator powinien znajdować się na powierzchni włókien, a nie w całej objętości polimeru włóknotwórczego. Do oceny efektu modyfikacji włókien polipropylenowych (PP) ditlenkiem tytanu domieszkowanym srebrem (TiO2/Ag) zastosowano techniki mikro-spektroskopii Ramana oraz elektronowej mikroskopii skaningowej połączonej z mikroanalizą rentgenowską SEM/EDS. Połączenie obu technik do analizy powierzchni oraz przekroju poprzecznego włókien (PP) pozwoliło na ocenę jakościowego i strukturalnego efektu modyfikacji.
PL
Jednym z głównych zadań w badaniach obiektów zabytkowych jest konieczność wskazania materiałów oryginalnych i późniejszych uzupełnień, które często także mają charakter zabytkowy. Kolejne zadanie dotyczy określenia składu i budowy historycznych materiałów, rozpoznania techniki wykonania pierwotnego opracowania malarskiego. W artykule przedstawiono wstępne wyniki badań zabytkowej malatury. Wykorzystano metodę badań w mikroobszarze z zastosowaniem skaningowego mikroskopu elektronowego sprzężonego z energodyspersyjną mikrosondą elektronową EDS (SEM-EDS).
EN
One of the main tasks in the study of historic buildings is the need to identify the original materials and extensions, which often have historic character. The next task concerns the determination of the composition and structure of the historical, diagnosis technique to develop original paint. The article presents the preliminary results of paintings. Methods were used with the scanning electron microscope was equipped with an energy dispersive X-ray spectrometer (SEM-EDS).
20
Content available remote Analiza składu chemicznego i fazowego ceramicznych naczyń archeologicznych
PL
Celem badań przedstawionych w artykule była analiza składu chemicznego i fazowego ceramicznych naczyń archeologicznych. Do badań zastosowano skaningowy mikroskop elektronowy wraz z przystawką do mikroanalizy rentgenowskiej, fluorescencyjny spektrometr rentgenowski oraz dyfraktometr rentgenowski. Materiałem do badań były fragmenty ceramicznych naczyń archeologicznych typu Menkendorf – Szczecin z IX–XI wieku pochodzących z terenów obecnej Polski i Niemiec. Przy użyciu skaningowej mikroskopii elektronowej badaniom i obserwacjom poddane były gliniana osnowa oraz domieszki, co pozwoliło na ich analizę chemiczną. Badania przy użyciu spektrometru fluorescencyjnego pozwoliły na analizę składu chemicznego sproszkowanych fragmentów próbek, natomiast dyfraktometria rentgenowska ich składu fazowego. Badania składu chemicznego wykonane przy użyciu SEM–EDS wykazały obecność najczęściej występującej domieszki w postaci kwarcu. Badania spektrometrii fluorescencyjnej pokazały, że we wszystkich zbadanych próbkach zawartość Al2O3 jest zbliżona i wynosi (18-19)% wag., co świadczy, że do wyrobu naczyń użyto gliny plastycznej. Analizy te wykazały również obecność szeregu innych tlenków takich jak min. SiO2, Fe2O3, Na2O, K2O, CaO. Badania dyfrakcyjne potwierdziły we wszystkich próbkach obecność takich faz jak SiO2 (kwarc), NaAlSi3O8 (albit) i Al2O3 (korund).
EN
The aim of research presented in the article was to analyze the chemical and phase compositions of archaeological ceramic vessels. The studies used scanning electron microscopy coupled with X-ray microanalysis, an X-ray fluorescence spectrometer and an X-ray diffractometer. Pieces of IX-XI century ceramic archaeological vessels of the Menkendorf-Szczecin type originating from sites in present Poland and German were the test material. The clay matrix and admixtures were subjected to studies and observations by using scanning electron microscopy, which allowed chemical analysis in micro-areas to be performed. Studies using the fluorescence spectrometer allowed us to analyze the chemical composition of powdered portions of the samples. The analysis of phase composition of the powdered samples was performed by X-ray diffraction. The SEM-EDS studies showed the presence of the most common inclusion in the form of quartz. The fluorescence spectrometry measurements showed that the content of Al2O3 was similar and amounted to (18-19) wt% in all tested samples, indicating that the vessels have been manufactured from plastic clays. The XRF studies also showed the presence of a number of other oxides such as SiO2, Fe2O3, Na2O, K2O and CaO. The XRD studies confirmed the presence of SiO2 (quartz), NaAlSi3O8 (albite) and Al2O3 (corundum) in all samples.
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