Electron Probe Microanalysis Results Research Articles

Insight into the Cationic Charge Distribution in U1-y-zPuyAmzO2±x Mixed Oxides.

Uranium-plutonium mixed oxides, containing few mol % of Am, are currently studied as fuel for Sodium Fast Reactors. The study of the O/M ratio of these fuels is of main interest, as its variation can induce issues for reactor safety. For this purpose, four U1-y-zPuyAmzO2±x samples (0.235 ≤ y ≤ 0.39 and 0.005 ≤ z ≤ 0.02) were studied using electron probe microanalysis (EPMA), X-ray powder diffraction (XRD), and X-ray absorption spectroscopy (XAS) experiments. EPMA analyses revealed a homogeneous matrix phase with few U- and Pu-rich agglomerates. A matrix phase of fluorite structure (face-centered cubic), as well as a small contribution of a UO2 phase of the same structure, was evidenced for all of the samples by XRD. The O/M ratios of the (U,Pu)O2±x matrix were calculated based on the obtained lattice parameters. XANES experiments highlighted the simultaneous presence of U5+ and Pu3+/Am3+ for all of the samples, indicating a charge compensation mechanism even for stoichiometric samples. Based on the EPMA and XRD results, it was evidenced that this coexistence of U4+, U5+, Pu3+, Pu4+, and Am3+ was not originating from the U- and Pu-rich agglomerates. It was found to be rather a peculiarity of the U1-y-zPuyAmzO2±x matrix phase, discussed with the help of thermodynamic calculations performed on the U-Pu-Am-O system.

Characterizing oxidation, thickness, and composition of metallic glass thin films with combined electron probe microanalysis and X-ray photoelectron spectroscopy

Metallic glass thin films (MGTFs) are a recently developed class of alloy coatings with potential applications ranging from biomedical devices to electrical components. Their tribological performance in service conditions is dictated by MGTF bulk composition but can be limited by the native oxide surface that inevitably forms upon exposure to atmosphere. Surface oxidation, thickness, and composition of ZrCuNiAl MGTFs were characterized using a combination of X-ray photoelectron microscopy (XPS) and electron probe microanalysis (EPMA). MGTF samples with nominal thicknesses of 50, 500, and 1500 nm were sputtered onto Si and SiN wafer substrates within a high vacuum deposition chamber and their amorphicity was confirmed by X-ray diffraction. XPS depth profiling identified the thin film composition and showed that the surface oxide was dominated by a mixed layer of mostly ZrO2, a little oxidized Al, and some metallic Zr. EPMA X-ray intensities were acquired as a function of beam energy to excite characteristic X-rays from different depths of the MGTFs and reconstructed using open-source thin film analysis software BadgerFilm, to determine the composition and thickness of sample layers. EPMA results constrain the composition to be Zr54Cu29Al10Ni7 within 0.7 at. % variation and total thicknesses to be 49, 470, and 1546 nm. Using the oxide composition identified from XPS depth profiling as an input for BadgerFilm analysis, EPMA results indicate the surface oxidation layer on each of the thin film samples was 6.5 ± 1.1 nm thick and uniform across a 0.25 mm region of the film.

Alteration mineralogy, characteristics and shortwave infrared spectroscopy of white mica in the Zijinshan ore field, Fujian Province: Implications for porphyry Cu prospecting

The Zijinshan ore field is situated in the southeastern part of China. in which contains the large Zijinshan high-sulfidation Cu-Au deposit, the Luoboling porphyry Cu-Mo deposit, the Yueyang low-sulfidation Au-Ag deposit, the Longjiangting and the Wuziqilong tansitional Cu deposit, and the Xi’nan porphyry Cu-Mo prospect. Debates on genetic relationship among these deposits, especially the relationship between the Zijinshan Cu-Au deposit and the adjacent Luoboling deposit is a question of importance for further exploration in this ore field. In this contribution, the alteration mineralogy, alteration texture, zonation and mineral chemistry, in combination with shortwave infrared spectroscopy (SWIR) analysis of white mica were used to help focus exploration and assessment of hydrothermal deposits in the Zijinshan ore field.In this study, diaspore-pyrophyllite alteration zone, chlorite-sericite alteration zone and propylitic alteration zone were first identified in the deep drill core of the Zijinshan Cu-Au deposit, which gives way upward to quartz-alunite-kaolinite zone, quartz-alunite zone and the silicic alteration zone. In the Xi’nan Cu-Mo prospect, diaspore-pyrophyllite alteration zone was first recognized in the shallow level with the chlorite-sericite alteration zone and propylitic alteration zone in the deeper level. Andalusite- sericite ± diaspore alteration zone was first recognized in the upper part of the Luoboling Cu-Mo deposit and the deeper part of the Wuziqilong Cu deposit. It indicates that a pervasive occurrence of diaspore -pyrophyllite ± andalusite alteration zones in the Zijinshan ore field, which may potentially represent a transitional environment between the top of porphyry alteration zones and the base of advanced argillic alteration zones. Minerals of the white mica group are extensively distributed in various alteration zones of the Zijinshan ore field. The SWIR analysis of white mica indicated that the wavelength position of the Al-OH (∼2,200 nm; wAlOH) absorption feature increases gradually from the shallow kaolinite-dickite alteration zone to the deep potassic alteration zone. In the advanced argillic alteration zones, the range of wAlOH values of white mica is less than 2205 nm. Conversely, in the porphyry alteration zones, it always exceeds 2205 nm. It is evident that the andalusite-sericite alteration zone with higher wAlOH values (average of 2203 nm) is always proximal to the porphyry mineralization, which may act as indicators for deep porphyry prospecting. The results of electron probe microanalysis (EPMA) reveal that the early enrichment of Mg and depletion of Fe in white mica can be attributed to the preferential incorporation of Fe into iron oxides and iron sulfides in the potassic and propylitic alteration zones. Overall, there is a negative correlation between wAlOH and Al, while wAlOH exhibits a positive correlation with the sum of Fe + Mg + Mn. The distribution characteristics of alteration zones and the variation patterns of the wAlOH of white mica indicate that there are probably several paleo-thermal centers in the deep parts of the Zijinshan ore field, located respectively in the deep parts of the Xi’nan Cu-Mo prospect and the deep part of the Zijinshan Cu-Au deposit and the deep parts of the Wuziqilong Cu deposit, and the latest seems to be more fertile and deserves further exploration.

Structural changes in trajectories of platinum sphere migration via laser illumination

In this study, metal spheres in glass were manipulated via heating using continuous-wave laser illumination. Metals are doped into the trajectory and selective compositional changes in the glass are observed. Meanwhile, the glass structure is modified via rapid heating and quenching. The structure of silica glass modified via platinum sphere migration was examined. Results of electron probe microanalysis confirm the presence of platinum in all trajectories, regardless of its low reactivity with silica glass. Elemental analysis reveals the precipitation of platinum nanoparticles in the trajectories at low migration speeds. Raman and infrared spectrum analyses reveal an increase in the fictive temperature, which increases with the migration velocity. Further, the etching rate increases with the sphere velocity. This study demonstrates that the structure of glass can be locally modified via platinum sphere migration, which depends on the sphere migration velocity.

Geochemical Characteristics of Garnet from Zinc–Copper Ore Bodies in the Changpo–Tongkeng Deposit and Its Geological Significance

The Changpo–Tongkeng tin polymetallic deposit in Dachang, Guangxi, is a world-class, superlarge, polymetallic tin deposit consisting of lower skarn zinc–copper ore bodies and upper tin polymetallic ore bodies. Garnet is the main gangue mineral in the skarn zinc–copper ore bodies and has a granular texture. Based on hand specimens and microscopic observations, the existing garnet can be divided into two generations: an early generation (Grt I) and a late generation (Grt II). The results of electron probe microanalysis (EPMA) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) in situ microanalysis show that the contents of SiO2 and CaO in the garnets from the two generations present limited variations, while the FeOT and Al2O3 contents vary significantly, indicating the grossular–andradite solid solution series (Gro29–82And12–69). Compared with Grt I (Gro72And25), Grt II (Gro39And59) is Fe-enriched and oscillatory zoning is developed. The total rare earth element (REE) contents in the two generations of garnet are relatively low, showing light rare earth element (LREE) depletion and heavy rare earth element (HREE) enrichment patterns. Grt II has higher REE content than Grt I and exhibits significant negative Eu anomalies (δEu = 0.18–0.44). The contents and variation characteristics of the major and trace elements in the two generations of garnet suggest that there were variable redox conditions and water/rock ratios in the hydrothermal system during the crystallization process of garnet. In the early stage, skarnization was in a relatively closed and low-oxygen fugacity system, with hydrothermal diffusion metasomatism being dominant, forming homogeneous Grt I lacking well-developed zoning. In the late stage of skarnization, the oxygen fugacity of the ore-forming fluids increased, with infiltration metasomatism being dominant, forming Grt II with well-developed oscillatory zoning. The contents of Sn, As, W, In, and Ge in the garnets are relatively high and increase with the proportion of andradite. Sn in zinc–copper ore bodies mainly exists in the form of isomorphic substitution in garnet, which may be the main reason for the lack of tin ore bodies during the skarn stage. This paper compares the trace element contents in garnets from domestic skarn deposits. The results indicate that the Sn content and δEu in garnet can be used to evaluate the tin-forming potential of skarn deposits.

Corrosion protection of folic acid and lauric acid modified films prepared by anodic oxidation on WE43 magnesium alloys

The corrosion protection of folic acid (FA) and lauric acid (LA) modified films prepared by anodic oxidation on WE43 magnesium alloys was particularly evaluated by scanning electron microscopy (SEM), electron probe microanalysis (EPMA), static contact angle (CA) and electrochemical tests. The combined results of SEM and EPMA showed that both FA and LA penetrated into the cavities and cracks to repair the defects of the anodic films. The polarization resistance of the FA-modified films increased by 1.56 × 105 Ω cm2 and the LA-fmodified films showed the largest value (6.36 × 106 Ω cm2). They improved by two and three orders of magnitude compared with the substrate, which objectively revealed the excellent corrosion resistance capacity of the modified films on measurement results level. The CA results indicated that the obtained anodic films modified by LA were hydrophobic. Furthermore, the process of the organic modification sealing and the corrosion protection mechanism of the anodic films modified by FA and LA were discussed.

An investigation into the reverse transformation of ferrite to austenite during friction stir processing of a duplex low-density steel

The reverse transformation of ferrite-to-austenite during friction stir processing of a duplex lightweight steel resulted in an abrupt decrease of the ferrite volume fraction within the stirred zone. This was explained in terms of diffusion-governed phenomena from the thermodynamic points of view. However, owing to the recorded thermal history of the process and the low exposure time at the maximum temperature, the probability of shear assisted diffusion was considered. The fraction of high angle and low angle boundaries within the stirred zone was extremely higher than those observed in thermomechanically affected zone or heat affected zone. These high/low angle boundaries acted as preferred diffusion paths and provided a proper condition to increase the lattice diffusion. The results of electron probe micro-analysis indicated that the alloying elements remained relatively un-partitioned in long range order. In addition, the grains were arbitrarily sheared towards the shear surface/ direction and volume fraction of shear texture component was substantially higher than that of recrystallization texture component. The above observations suggest that the abrupt drop in the ferrite content at the vicinity of the rotating tool in the shear layer may be also induced by shear assisted massive transformation.

Hunting the Datable Garnet using the LA‐ICP‐MS U‐Pb Method: Predicting Garnet U Concentration, based on Major and Minor Elements

AbstractGarnet occurs in a wide range of rock types, from mantle peridotites to granites, from eclogites to skarns. In recent years, garnet LA‐ICP‐MS (Laser Ablation Inductively Coupled Plasma Mass Spectrometry) U‐Pb dating has provided a powerful solution for retrieving the ages of rock formations, but successful dating is often prohibited by the low concentration of U. However, the concentration of U, a trace element of garnet, is unknown prior to the LA‐ICP‐MS analysis. In this study, we propose that the U concentration in garnet can be predicted by the contents of major and minor elements, which can be quantitatively obtained by EPMA (electron probe microanalysis). Using a supervised machine learning method (neural network), a model is trained to discriminate U‐rich (>2 ppm) and U‐poor (<2 ppm) garnets, based on EPMA results. Results of cross validation shows that the model has an average accuracy of ∼92% and is a powerful tool in detecting datable U‐rich garnet. To facilitate the use of the discriminator, it is programmed as a stand‐alone Microsoft Excel spreadsheet (HighUGarnet) and users directly paste the molar proportions of garnet end members into it and obtain the discrimination result.

Zr3Mn3Sn4Ga: a new hexagonal Ti6Sn5-type quaternary intermetallic

The discovery of a new quaternary intermetallic compound of composition Zr3Mn3Sn4Ga during a survey of the Zr–Mn–Sn–Ga phase diagram is reported. Single-crystal X-ray diffraction reveals that the new compound crystallizes in a hexagonal lattice (space group P63/mmc, No. 194). The analysis of single-crystal X-ray diffraction data indicates that the atomic arrangement is an ordered variant of the high-temperature hexagonal Ti6Sn5 crystal structure. From a simple geometry point of view, the unit cell consists of GaZr3 octahedra chains and Mn chains growing along the sixfold symmetry axis c. The Mn chains are stacked within the ab basal plane in a kagome geometry, with large interatomic distances. The possible slight levels of Sn/Ga and Zr/Mn mixed occupancy based on additional results of electron probe microanalysis and single-crystal neutron diffraction are discussed. It is noteworthy that this compound is the first quaternary intermetallic discovered in this structure and the first Ti6Sn5 derivative bearing a magnetic metal, namely Mn, in the 6g position, which may give rise to interesting physical properties.

A Comparative Study on Microstructure and Properties of Ultra-High-Speed Laser Cladding and Traditional Laser Cladding of Inconel625 Coatings.

In this study, ultra-high-speed laser cladding (UHSLC) and traditional low-speed laser cladding (LSLC) were employed to prepare high-quality Inconel625 coatings on 27SiMn substrates. UHSLC has cladding speeds of 30 m/min, which are 15 times faster than those of LSLC, and it produces a much greater cladding efficiency, which is 13.9 times greater than LSLC. The microstructure of the Inconel625 coatings was investigated in detail utilizing field emission scanning electron microscopy (FESEM) and electron probe microanalyzer (EPMA). According to the FESEM results, UHSLC Inconel625 coatings have more refined crystals than LSLC Inconel625 coatings. Nevertheless, the EPMA results indicate that the UHSLC Inconel625 coatings exhibit much more severe elemental segregation. Moreover, the hardness, wear and corrosion resistance of Inconel625 coatings are significantly enhanced by increasing the laser cladding speed. Furthermore, the reasons for the differences in microstructure and properties of Inconel625 coatings prepared by UHSLC and LSLC were clarified by finite element simulation. UHSLC technique is, therefore, more suitable for preparing Inconel625 coatings on 27SiMn steel surfaces than LSLC.

Structure, segregation and properties of high-alloy Al – Ti – V – Ni alloys

Using optical and electron scanning microscopy, as well as electron probe microanalysis and X-ray diffraction analysis, the authors looked at the structure, segregation and properties (hardness HRA, microhardness HV) of high-alloy Al – Ti – V – Ni alloys. It was established how the structure tends to change and how elements of the structural components of the studied alloys (1–5) tend to distribute as a function of V and Ni concentration. Using electron probe microanalysis, the structural conponents of the studied alloys were identified depending on V and Ni concentration. 1. The initial alloy 1 sees vanadium aluminide Al3(V, Ti) solidify from Al – Ti – V – Ni (wt. %: 24.6 V, 0 Ni), as well as alloyed vanadium carbide. The former solidifies as grey-coloured grains with a minimum size of 25 μm and serves as the base phase, whereas tha latter comes in a spiky shape (<25 μm). A blackish-coloured mixture of Al + Al3Ti + Al21V2 solidifies last. 2. Alloy 2 sees nickel aluminide Al3Ni solidify from Al – Ti – V – Ni (17 wt. % V, 7.2 wt. % Ni) as fine-grained light-coloured inclusions against a background of vanadium aluminate Al2(V, Ti), which is the key structural component of the alloy. Together with the above phases, alloyed titanium carbide (Al, Ti, V)3C forms in the alloy as compact grey-coloured grains. A phase mixture of Al + + Al3Ni + Al3Ti + Al21V2 solidifies last. 3. The following phases solidify in alloys 3–5 from Al – Ti – V – Ni (0–10.7 wt. % V; 13.5–23.8 wt. % Ni): β'-phase – a solid solution of Ni in nickel aluminide AlNi, which comes as fine-grained white-coloured inclusions against a background of nickel aluminide Al3Ni, which is the base phase. The next phase includes compact dark-grey grains of titanium carbide Ti2C. Alloys 4–5 see a new phase form – a complex alloyed titanium aluminide Al3(Ti, V, Ni), which consists of dark-grey oblong-shaped crystals. A phase mixture of Al + Al3Ni + Al3Ti + Al21V2 solidifies last. Even though the stoichiometry of the identified phases fails to match the results of electron probe microanalysis, the results of X-ray diffraction analysis confirms the presence of the key structural components in the studied alloys.This research was carried out using the equipment of the Applied Materials Science Centre at the Pacific National University. It was funded by the Ministry of Education and Science of the Russian Federation under Gove rnmental Assignment No. FEME-2020-0010.

Age-related changes in cationic compositions of human cranial base bone apatite measured by X-ray energy dispersive spectroscopy (EDS) coupled with scanning electron microscope (SEM).

One of the most common scientific methods to study the chemical composition of bone matter is energy-dispersive X-ray spectroscopy (EDS). However, interpretation of the data obtained can be quite complicated and require a thorough understanding of bone structure. This is especially important when evaluating subtle changes of chemical composition, including the age-related ones. The aim of current study is to create a method of processing the obtained data that can be utilized in clinical medicine and use it to evaluate the age evolution of bone chemical composition. To achieve this goal, an elemental composition of 62 samples of cadaver compact bone, taken from the skull base (age: Me = 57.5; 21/91(min/max); Q1 = 39.5, Q3 = 73.75), was studied with EDS. We used the original method to estimate the amount of Mg2+ cations. We detected and confirmed an increase of Mg2+ cation formula amount in the bone apatite, which characterizes age-related resorption rate. Analysis of cation estimated ratio in a normative bone hydroxylapatite showed an increase of Mg2+ amount (R = 0.43, p = 0.0005). Also, Ca weight fraction was shown to decrease with age (R=-0.43, p = 0.0005), which in turn confirmed the age-dependent bone decalcification. In addition, electron probe microanalysis (EPMA) and X-ray diffraction analysis (XRD) were performed. EDS data confirmed the EPMA results (R = 0.76, p = 0.001). In conclusion, the proposed method can be used in forensic medicine and provide additional data to the known trends of decalcification and change of density and crystallinity of mineral bone matter.

Genesis of Chaoshan skarn Au deposit, Tongling, eastern China: Insights from mineral geochemistry

Skarn Au deposits are particularly developed along Middle and Lower Yangtze River region, eastern China, but gold behavior and genesis of the skarn Au deposits remain unclear. Whole-rock geochemical, sulfur isotopic and in-situ mineralogical data from the mineralized alteration stages of Chaoshan skarn Au deposit in Tongling region are systemically investigated to reveal Au distribution and precipitation, and useful information for ore-forming process. The altered rocks and ores in the Chaoshan deposit have total REE contents of 7.81–226 ppm and show LREE enrichment patterns with weak negative to positive Eu (δEu = 0.71–2.24) anomalies. Electron probe microanalysis results indicate that garnet and pyroxene of the Chaoshan deposit are grossular-andradite and diopside-hedenbergite series, respectively. In situ elemental compositions of the euhedral pyrite analyzed show that invisible Au is mainly of lattice-bound Au+ in As-bearing pyrite. The studied pyrite samples also have high Co/Ni (mainly >1) and Se/Tl (>10) ratios, highly variable Pb and As contents, low Se content (<5.00 ppm), low Tl/Pb and Sb/Pb ratios, and relatively consistent sulfur isotopic compositions (5.0–8.3 ‰). The distinctly geochemical characteristics indicate that the Chaoshan skarn Au mineralization was likely derived from a magmatic-hydrothermal system. A comprehensive discriminant analysis shows that the Au precipitation and enrichment of the Chaoshan deposit are a result of boiling-induced trace element fractionation resulted from fluid boiling during the skarn formation process.

Electron probe microanalysis of the elemental composition of phytoliths from woody bamboo species.

Electron probe microanalysis (EPMA) is promising for accurately determining elemental components in micro-areas of individual phytolith particles, interpreting compositional features and formation mechanisms of phytoliths in plants, identifying archeological and sedimental phytolith. However, the EPMA method of analyzing mounted slide phytoliths has not well been defined. In this study, we attempted different EPMA methods to determine the elemental compositions of phytoliths in mounted slides. Direct analysis of carbon (DAC) with other elements in phytolith could obtain abnormally high total values and carbon values. The method of carbon excluded in measuring elements (non-carbon analysis (NCA)) was feasible to obtain elemental compositions in phytolith. The NCA method was conducive to obtain the factual elemental compositions of an individual phytolith (morphotype) when the carbon content of phytolith was relatively low. The EPMA results of phytoliths from 20 bamboo species (three genera) showed that phytolith was dominantly composed of SiO2 but also included low contents of diverse other elements. The EPMA of phytoliths can provide the elemental composition of micro-areas of an individual phytolith particle. The elemental compositions of phytolith varied with their morphotypes, the genera and ecotype of bamboos. The EPMA of elemental compositions in phytoliths is a potential tool to study the formation mechanism of phytoliths, plant taxonomical identification, archaeological and paleoenvironmental reconstruction.

Effects of processing parameters and heat treatment on the microstructure and magnetic properties of the in-situ synthesized Fe-Ni permalloy produced using direct energy deposition

The present work investigated the correlations between heat treatment and the microstructure and magnetic properties of the in situ alloyed Fe-50%Ni samples manufactured using laser-based direct energy deposition under different production conditions. The samples with high relative density were directly synthesized from the pure Fe and Ni elemental powders. In addition, a fine FCC microstructure with relatively elongated grains in the building direction was observed in the as-print samples. After applying short-time heat treatment, the grain morphology remained unchanged, while the grain size and microhardness were slightly increased and decreased, respectively. This also caused the reduction in internal residual stresses and, subsequently, partial stress relaxation in the microstructure. According to the electron probe microanalysis results, the simultaneous Fe and Ni depletion/enrichment formed during the in-situ alloying was practically decreased after applying short time heat-treatment, resulting in the significant improvement of magnetic properties, as compared to the as-built ones. The maximum magnetization, coercivity, and curie temperature of ~170 emg/g, 1.8 Oe, and 530 °C, respectively, were obtained in the optimum processed sample, which were significantly higher than those of other soft magnetic permalloys produced by additive manufacturing methods.

Effects of composition and growth parameters on phase formation in multicomponent aluminum garnet crystals.

The effects of composition on the phase formation of multicomponent garnet crystals grown via directional solidification by the micro-pulling-down method are studied. A relatively wide range of rare-earth (RE) average ionic radii (AIR) is explored by formulating ten compositions from the system (Lu,Y,Ho,Dy,Tb,Gd)3Al5O12. Crystals were grown at either 0.05 or 0.20 mm min-1. The hypothesis is that multicomponent compounds with large AIR will form secondary phases as the single-RE aluminum garnets formed by larger Tb3+ or Gd3+; this will result in crystals of poor optical quality. Crystals with large AIR have a central opaque region in optical microscopy images, which is responsible for their reduced transparency compared to crystals with small AIR. Slow pulling rates suppress the formation of the opaque region in crystals with intermediate AIR. Powder and single-crystal X-ray diffraction and electron probe microanalysis results indicate that the opaque region is a perovskite phase. Scanning electron microscopy and energy dispersive spectroscopy measurements reveal eutectic inclusions at the outer surface of the crystals. The concentration of the eutectic inclusions increases with increasing AIR.

Mineralogical and Chemical Changes after Reduction Roasting of Xinjiang Iron Ore, China

The mineralogical and chemical changes in Chinese Xinjiang iron ore containing impurities, lead, and zinc as a result of reduction roasting were studied via chemical analysis, optical microscopy, X-ray fluorescence (XRF), electron probe microanalysis (EPMA), and energy-dispersive spectroscopy (EDS). Analysis showed that hematite was the main iron-bearing mineral, with small amounts of magnetite and iron silicate; lead impurities were mainly lead oxide and lead–iron alum, while zinc oxide was the main zinc impurity. X-ray fluorescence analysis for raw samples indicated the presence of quartz, hematite, magnetite, chlorite, calcite, and dolomite. The results of the analysis of roasted samples showed an increase in hematite at temperatures of 750 °C and 950 °C, while the elemental iron increased at a temperature of 1200 °C, along with the conversion of galena to lead oxide and sphalerite to zinc oxide, with a stable quartz ratio. The chemical analysis of the raw sample showed that the TFe grade of the sample was 47.04%, while the contents of harmful Pb and Zn impurities were 0.39% and 0.30%, respectively, both of which exceed the index (less than 0.10%) required by the iron industry for raw materials. The content of harmful sulfur impurities was also high, at 1.19%, which needs to be eliminated or reduced. The results of EPMA and EDS analysis of pre-roasting raw samples showed that chemical compositions vary in different locations in the hematite, magnetite, sphalerite, and galena micro-zones. It has also been observed that quartz is mostly diffused with magnetite and hematite, and sulfur appears in small quantities in most regions. The analysis after roasting showed that the percentages of lead, zinc, and sulfur impurities decreased by a large rate. It is clear that the roasting process plays a major role in removing impurities such as sulfur, which appears in a small percentage after the roasting process, and also helps in oxidizing the impurities of lead and zinc, which helps in removing them.

NEW DATA ON THE CRYSTAL-CHEMISTRY OF METAMICT MINERALS FROM THE VELYKA VYSKA SYENITE MASSIF (UKRAINIAN SHIELD)

The structural properties and composition of metamict minerals, namely allanite, chevkinite, and britholite, occurring as inclusions in allanite from feldspar syenites of the Velyka Vyska massif (Korsun-Novomyrgorod pluton, Ukrainian Shield) were investigated by X-ray diffraction and electron probe microanalysis (EPMA). The age of the syenites is 1.7-1.8 Ga, which corresponds to their formation ages within the Ukrainian Shield. X-ray analysis shows that of the original samples of chevkinite and allanite give a broad diffraction peak between 16—28° 2Θ as well as Bragg reflections in the region of the most intense reflections of semimetamict allanite and britholite, indicating the metamict state of chevkinite and the semimetamict state of allanite. The content of radioactive Th found in the chevkinite (0.25-0.33 apfu) is higher compared to its amount in allanite (0.024-0.033 apfu). Calculated unit-cell parameters of the chevkinite and allanite samples showed that their structures underwent significant changes after annealing. There is a slight distortion of the chevkinite unit cell related to a decrease in the a and an increase in b and c edges. A decrease in b and the increase in c in the allanite is caused by a redistribution of cations in the structure and an oxidation of iron, Fe2+ → Fe3+, during heating. Thereby the stability of the allanite structure decreases and it ultimately breaks down. The structural sites A and A2 in chevkinite and allanite are mainly occupied by REEs of the cerium group. The amount of Y is minor. The substitution mechanism А2(REE)3+ + М3М2+ → А2Са2+ + М3М3+(allanite) and M2Fe3+ + M3,4Ti4+↔ M2Fe2+ + M3,4Nb5+ (chevkinite) occur. The M2 site in the structure of chevkinite and M3 in allanite contain more Fe2+ than Fe3+. This leads to a weakening of the bonds in their structures, and a stepwise breakdown and partial or total metamictization of their structures. The britholite inclusions in allanite belong to the Y variety. They were probably formed much later than allanite and chevkinite in the Velyka Vyska massif. According to the EPMA results, namely BSE-images and REE content determinations, allanite and chevkinite formed almost simultaneously.

Sintering, microstructure, and mechanical properties of vitrified bond diamond composite

The demand for high-performance grinding wheels is gradually increasing due to rapid industrial development. Vitrified bond diamond composite is a versatile material for grinding wheels used in the backside grinding step of Si wafer production. However, the properties of the vitrified bond diamond composite are controlled by the characteristics of the diamond particles, the vitrified bond, and pores and are very complicated. The main objective of this study was to investigate the effects of SiO2–Na2O–B2O3–Al2O3–Li2O–K2O–CaO–MgO–ZrO2–TiO2–Bi2O3 glass powder on the sintering, microstructure, and mechanical properties of the vitrified bond diamond composite. The elemental distributions of the composite were analyzed using electron probe micro-analysis (EPMA) to clarify the diffusion behaviors of various elements during sintering.The results showed that the relative density and transverse rupture strength of the composite sintered at 620 °C were 91.7% and 126 MPa, respectively. After sintering at 680 °C, the glass powder used in this study exhibited a superior forming ability without an additional pore foaming agent. The relative density and transverse rupture strength of the composite decreased to 48.2% and 49 MPa, respectively. Moreover, the low sintering temperature of this glass powder protected the diamond particles from graphitization during sintering, as determined by X-ray diffraction and Raman spectrum. Furthermore, the EPMA results indicate that Na diffused and segregated at the interface between the diamond particles and vitrified bond, contributing to the improved bonding. The diamond particles can remain effectively bonded by the vitrified bond even after fracture.

Fabrication, Structure, and Thermal Properties of Mg-Cu Alloys as High Temperature PCM for Thermal Energy Storage.

This work studied the thermophysical properties of Mg-24%Cu, Mg-31%Cu, and Mg-45%Cu (wt.%) alloys to comprehensively consider the possibility of using them as thermal energy storage (TES) phase change materials (PCMs) used at high temperatures. The microstructure, phase composition, phase change temperatures, and enthalpy of these alloys were investigated by an electron probe micro analyzer (EPMA), X-ray diffraction (XRD), and differential scanning calorimetry (DSC). The XRD and EPMA results indicated that the binary eutectic phase composed of α-Mg and Mg2Cu exists in the microstructure of the prepared Mg–Cu series alloys. The microstructure of Mg-24%Cu and Mg-31%Cu is composed of α-Mg matrix and binary eutectic phases, and Mg-45%Cu is composed of primary Mg2Cu and binary eutectic phases. The number of eutectic phases is largest in Mg-31%Cu alloy. The DSC curves indicated that the onset melting temperature of Mg-24%Cu, Mg-31%Cu, and Mg-45%Cu alloys were 485, 486, and 485 °C, and the melting enthalpies were 152, 215, and 91 J/g. Thermal expansion and thermal conductivity were also determined, revealing that the Mg–Cu alloys had a low linear thermal expansion coefficient and high thermal conductivity with respect to increasing temperatures. In conclusion, the thermal properties demonstrated that the Mg–Cu alloys can be considered as a potential PCM for TES.