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Spectroscopic techniques in the investigation of extraordinary medieval Polish coins : revealing the presence of hidden cores

Trela Krystian, Gójska Aneta Maria, Miśta-Jakubowska Ewelina A., Kelemen Mitja, Šmit Žiga, Kędzierski Adam, Garbacz-Klempka Aldona

Nukleonika

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2025

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Vol. 70, No. 1

19--27

EN

Spectroscopic techniques in the investigation of extraordinary medieval Polish coins : revealing the presence of hidden coresCross denars, frequently found in Polish hoards, were traditionally thought to be Ag coins with some Cu content. This study investigates the possibility of a hidden Cu core beneath the Ag or Ag–Cu surface of these coins. It raises questions about whether they were counterfeits or intentionally designed for mass production. Unlike Roman denarii, which revealed their cores when broken, the examination of cross denars without damage is challenging. Optical microscopy and microanalysis revealed differences in the composition of early medieval Polish coins, challenging the belief that cross denars were homogeneous Ag–Cu alloys. Detailed spectroscopic analyses, including energy-dispersive X-ray fluorescence (ED-XRF), scanning electron microscopy with energy- -dispersive X-ray spectroscopy (SEM-EDS), micro X-ray fluorescence (XRF), and microparticle-induced X-ray emission (-PIXE) measurements, were conducted. These analyses of two cross denars uncovered one composed of an Ag–Cu alloy and another manufactured by plating a Cu–Zn core with an Ag sheet. This suggests the need for further research in the history and technology of minting in Poland in the Early Middle Ages. It also prompts a reconsideration of the applicability of noninvasive X-ray techniques for archaeological examinations.

2

Silica diagenesis in Eocene carbonates of the Okçular Formation, Turkey : inferences from field observations and petrography

Yeşilot Kaplan Meryem

Geological Quarterly

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2025

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Vol. 69, No. 3

art., nr 30

EN

The silica diagenesis of limestones depends on the environmental conditions and the presence of a silica source. Microstructural features, cracking, porosity, crystal/grain size and the chemical composition of the limestones and chert nodules and layers in the Okçular Formation are parameters controlling silica diagenesis. Cherts are observed in three forms (1) chert nodules with/without a rim, (2) fractured cherts, and (3) layered cherts. Authigenic quartz crystals, chertified foraminifers, microlaminations in the limestones and the chert-limestone grain size relation indicate diagenetic replacement. There is a positive correlation between the size of the microquartz crystals and the colour of the cherts, according to fluid circulation, the trace element content, and the degree of silicification. As the size of microquartz crystals increases due to all these factors, the colour changes from brown to grey-black. Crack widening due to nodule growth, the generally parallel arrangement of chert nodules in carbonates to cracks, and the presence of diagenetic stylolites indicate that both tectonic and diagenetic fractures played a role in silicification. The presence of Cl, P, Ti, Mn and Mo in the chertified zones in limestones indicates inorganic silicification in a marine environment.

3

Structural and surface characterization of adsorbents applied in liquid chromatography

Lech-Przywara Regina, Galek Tomasz, Przywara Mateusz, Zapała Lidia, Zapała Wojciech

Advances in Science and Technology. Research Journal

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2025

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Vol. 19, no. 9

292--309

EN

A detailed analysis of the four commercial stationary phases often applied in liquid chromatography was performed using the following: SEM-EDS techniques and specific surface area and porosity analysis methods (multipoint BET, BJH, DH and DFT). The SEM-EDS results confirmed that the main component of all adsorbents examined is silica (SiO₂), while differences in oxygen content indicate varied approaches to surface modification, ranging from the strongly hydrophilic phase of TSK Gel Amide-80 to the hydrophobic Nucleodur C18 Gravity. Besides, the presence of trace amounts of metals may influence the additional analyte-adsorbent interaction of different nature. A comparison of specific adsorbent surface area data obtained using the multipoint BET method with the manufacturers values revealed significant discrepancies in the cases of TSK Gel Amide 80 and Nucleodur C18 Gravity, which may be the result of differences in pore accessibility and measurement methods. However, the Eurospher II 100-5 HILIC and Purospher STAR NH₂ phases showed good agreement with the manufacturers data. The porous structure of the phase studied shows significant differences: TSK Gel Amide 80 is characterized by mesopores with a uniform distribution, which favor the retention of larger molecules; Eurospher II 100-5 HILIC is microporous and selective for small, polar analytes; Nucleodur C18 Gravity has a structure typical of reversed phase materials; and Purospher STAR NH₂ exhibits the highest porosity, which favors the retention of large molecules, although it can also lead to the retention of undesirable analytes.

4

Pierwsze(?) polskie miejskie mikrometeoryty : analiza chemiczna i fazowa

Kajewski Wojciech, Durak Wojciech, Maciak Michał, Ziemniak Grzegorz

Przegląd Geologiczny

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2024

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Vol. 72, nr 10

508--516

EN

Micrometeorites are extraterrestrial particles smaller than 2 mm that fall on the surface of a planetary body, allowing them to be collected and investigated. In this study, we collected a 30 kg sample of sediment gathered on the rooftop of Wroclaw University, Poland. After separation and hand-picking, potentially extraterrestrial spherules were analysed using SEM-EDS and a Raman spectrometer. Nine spher¬ules were positively identified as micrometeorites. They are characterized by a chemical composition comparable to carbonaceous chondrites. Six of them represent the barred olivine type, and the remaining three are of the cryptocrystalline type. Five out of the nine spherules contain metallic beads that are characterized by variable contents of oxygen, iron, and nickel, while one of the grains, partly covered in iron oxide, exhibits morphological features suggesting that the metallic bead escaped from the silicate body. Raman spectroscopic analyses revealed that the cosmic spherules consist mainly of olivine and magnetite. Additional Raman analyses were performed on the cryptocrystalline spherule with two beads along its elongation, revealing a continuous shift of characteristic olivine Raman peaks. The ~820 cm-1and ~850 cm-1 Raman shift values near the heavier bead approach ~817 cm-1 and ~846 cm-1 towards the lighter one, which also corresponds with the change of the micrometeorite ’s black colour to a more greenish and translucent appearance near the lighter metallic bead. This suggests that at least surface crystallization of micrometeorites starts from a more forsteritic melt in the front, progressing towards more fayalitic compositions in the aerodynamic tail.

5

The use of computed tomography and scanning microscopy methods for assessing the alkaline reactivity of aggregate

Zapała-Sławeta Justyna

Bulletin of the Polish Academy of Sciences. Technical Sciences

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2024

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Vol. 72, nr 3

art. no. e149814

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.

6

A Glimpse into Raw Material Management in the Early Iron Age: Bronze Ingots from a Production Settlement in Wicina (Western Poland) in Archaeometallurgical Research

Garbacz-Klempka Aldona, Dzięgielewski Karol, Wardas-Lasoń Marta

Archives of Metallurgy and Materials

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2024

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Vol. 69, iss. 1

163--180

EN

Assessing the level of metallurgical and foundry technology in prehistoric times requires the examination of raw material finds, including elongated ingots, which served as semi-finished products ready for further processing. It is rare to find such raw material directly at production settlements, but Wicina in western Poland is an exception. During the Hallstatt period (800-450 BC), this area, situated along the middle Oder River, benefited from its favorable location in the heart of the Central European Urnfield cultures and developed networks for raw material exchange and bronze foundry production. Numerous remnants of casting activities, such as clay casting molds, casting systems, and raw materials, have been discovered at the Wicina settlement. This article aims to provide an archaeometallurgical interpretation of raw material management and utilization by prehistoric communities during the Early Iron Age. To achieve this, a collection of 31 ingots from the defensive settlement in Wicina, along with two contemporary deposits from Bieszków and Kumiałtowice, both found within a 20 km radius of the stronghold, were studied. Investigations were conducted using a range of methods, including optical microscopy (OM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (SEM-EDS), X-ray fluorescence spectroscopy (ED-XRF), powder X-ray diffraction (PXRD), AAS and ICP-OES spectrometer. The significance of ingots is examined in the context of increasing social complexity and the rising popularity of bronze products, which necessitated diversified production and a demand for raw materials with different properties and, consequently, different chemical compositions.

7

REE-bearing minerals in sediment-hosted stratiform pyrite mineralization zones of the Wiśniówka area (Holy Cross Mts., Poland)

Migaszewski Zdzisław M., Gałuszka Agnieszka, Zielińśki Grzegorz

Geological Quarterly

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2023

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Vol. 67, No. 2

art. no. 17

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.

8

Chemical and morphological characterization of PM2.5 samples collected over an urban industrial region Raipur, Chhattisgarh

Khobragade Pallavi Pradeep, Ahirwar Ajay Vikram

Acta Geophysica

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2023

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Vol. 71, no. 6

3057--3076

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.

9

Zróżnicowanie procesów deterioracji elewacji piaskowcowej XIX-wiecznego budynku Archiwum Państwowego w Poznaniu

Szczepaniak Małgorzata

Przegląd Geologiczny

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2021

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Vol. 69, nr 2

127--134

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.

10

Evaluation of the efficiency of metal recovery from printed circuit boards using gravity processes

Franke Dawid M., Suponik Tomasz, Nuckowski Paweł M., Dubaj Justyna

Physicochemical Problems of Mineral Processing

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2021

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Vol. 57, iss. 4

63--77

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.

11

Zastosowanie metod instrumentalnych w badaniach meteorytu Morasko

Muszyński Andrzej, Runka Tomasz, Gołębiewska Bożena, Michalska Danuta, Karwowski Łukasz

Przegląd Geologiczny

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2019

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Vol. 67, nr 3

156--158

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.

12

Niszczenie okładziny piaskowcowej w zabytkowym budynku Traktu Królewsko-Cesarskiego w Poznaniu

Szczepaniak Małgorzata, Rój Paulina

Przegląd Geologiczny

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2019

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Vol. 67, nr 9

717--727

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.

13

The effect of petrographic characteristics on the physical and mechanical properties of currently exploited Pińczów Limestones – a type of Leitha Limestone (Carpathian Foredeep, southern Poland)

Figarska-Warchoł Beata, Stańczak Grażyna

Gospodarka Surowcami Mineralnymi

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2019

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T. 35, z. 1

59--98

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.

14

Analiza składu chemicznego szkieł średniowiecznych trzech witraży z klasztoru oo. Dominikanów w Krakowie

Bernady E., Walczak M., Wilk D., Bulska E., Bernady E.

Szkło i Ceramika

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2018

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R. 69, nr 5

18--22

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.

15

Analiza stanu czynnej powierzchni ściernic impregnowanych węglem amorficznym po procesie szlifowania stopu Titanium Grade 2® z użyciem mikroskopii elektronowej i spektroskopii rentgenowskiej (SEM-EDS)

Nadolny K., Sienicki W., Wojtewicz M., Rokosz K., Kapłonek W., Wienecke M., Heeg J.

Mechanik

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2016

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R. 89, nr 8-9

1106--1107

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.

16

Identyfikacja pigmentów z zabytkowych polichromii we wnętrzach kamienicy nr 41 na Starym Rynku w Poznaniu

Filipiak M.

Przegląd Geologiczny

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2015

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Vol. 63, nr 7

418--425

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.

17

A methodology for identifying the chemical composition of the surface of solids using the XPS and SEM/EDS techniques

Bednarska A., Osuch-Słomka E., Grądkowski M.

Problemy Eksploatacji

|

2015

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no. 3

39--48

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.

18

Badania mechanizmu dehydratacji uwodnionego glinianu wapniowo-cyrkonowego

Madej D., Szczerba J.

Materiały Ceramiczne

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2015

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T. 67, nr 3

257--261

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.

19

Temperaturowa odporność na zużycie elementów z powłoką AlCrN

Michalak M., Michalczewski R., Osuch-Słomka E., Szczerek M.

Inżynieria Materiałowa

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2015

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Vol. 36, nr 6

468--472

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.

20

Analiza SEM-EDS stanu czynnej powierzchni ściernicy impregnowanej węglem amorficznym po procesie szlifowania prostoliniowo-zwrotnego walcowych powierzchni wewnętrznych ze stopu Titanium Grade 2

Nadolny K., Rokosz K., Kapłonek W., Wienecke M., Heeg J.

Inżynieria Maszyn

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2015

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R. 20, z. 1

78--88

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.