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Abstract

In the paper, which can be treated as a continuation of research intended to identify the time period when the Rotunda of St. Nicholas in Przemyśl had been built, we made another attempt to define the period of the church’s construction based on the current state of the art and with the use of precise research equipment. Our study was aimed at defining the structures of the building’s material obtained via chemical and crystalline composition analysis of collected mortar samples. We also attempted to define the site of the quarry from where the material used to build the church had been procured from, using tools to assess their chemical and crystalline compositions. We identified the composition of the samples via in situ and laboratory testing (instrumental analyses). The findings allowed us to determine the chemical and crystalline composition of mortars and the chemical and crystalline composition of stone and to compare it with other dated buildings.
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Authors and Affiliations

Marek Gosztyła
1
ORCID: ORCID
Krystian Sikorski
1
ORCID: ORCID

  1. Rzeszów University of Technology, Faculty of Civil and Environmental Engineering and Architecture
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Abstract

W artykule zbadano możliwość wykorzystania popiołów lotnych klasy C (otrzymywanych w wyniku spalania węgla brunatnego w kotle pyłowym) i F (otrzymywanych w wyniku spalania węgla kamiennego metodą konwencjonalną) jako substratów do syntezy materiału zeolitowego z grupy filipsytu. W tym celu przeprowadzono szereg syntez hydrotermalnych z wykorzystaniem reagentów takich jak wodorotlenek sodu (NaOH) oraz bromek tetrapropyloamoniowy (TPABr). W wyniku reakcji otrzymano docelowy materiał zeolitowy, zarówno z popiołu klasy C, jak i F. Otrzymane produkty syntezy, jak też popiołowe substraty reakcji, poddano charakterystyce chemicznej i mineralogicznej. Badania wykazały, że popiół lotny powstały z węgla brunatnego i kamiennego może być substratem w reakcjach syntez zeolitu, jakim jest filipsyt. Analiza porównawcza dyfraktogramów rentgenowskich produktów z obu typów popiołów wykazała, że lepszym substratem jest popiół klasy C otrzymywany w wyniku spalania węgla brunatnego w kotle pyłowym (w reakcji syntezy otrzymano lepiej wykształcone formy zeolitowe). W pracy dokonano także analizy literaturowej potencjalnych kierunków zastosowania filipsytu w inżynierii i ochronie środowiska. Na podstawie zweryfikowanych danych stwierdzono, iż dalszym kierunkiem badań będzie analiza możliwości wykorzystania otrzymanych materiałów jako potencjalnych sorbentów amoniaku.
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Authors and Affiliations

Rafał Panek
Magdalena Wdowin
Piotr Kunecki
Justyna Cader
Dorota Czarna
Jarosław Madej
Patrycja Lipiec
Wojciech Franus
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Abstract

The paper is concerned with comparing the methods for determining the ferrite content in castings from duplex stainless steels. It uses Schaeffler diagram, empirical formula based calculation, image analysis of metallographic sample, X-ray diffraction and measurement with a feritscope. The influence of wall thickness of the casting on the ferrite content was tested too. The results of the experiments show that the casting thickness of 25 or 60 mm does not have a significant effect on the measured amount of ferrite. The image analysis of metallographic sample and the measurement with the feritscope appear to be the most suitable methods. On the contrary, predictive methods, such as Schaeffler diagram or empirical formula based calculation are only indicative and cannot replace the real measurements. X-ray diffraction seems to be the least suitable measuring method. Values of ferrite content measured in such a way often deviated from the values measured by image analysis and with feritscope.

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Authors and Affiliations

V. Kaňa
V. Pernica
A. Zadera
V. Krutiš
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Abstract

The subject of the paper is structural stability of the Zn-26 wt.% Al binary alloys doped with 2.2 wt.% Cu or 1.6 wt.% Ti addition. The structural stability of Zn-Al alloys with increased Al content is connected with stability of solid solution of zinc in aluminium α', which is the main component of these alloys microstructure. Such a solution undergoes phase transformations which are accompanied, among others, by changes in dimensions and strength properties. The structural stability of the ZnAL26Cu2.2 and ZnAl26Ti1.6 alloys was investigated using XRD examinations during long term natural ageing after casting, as well as during long term natural ageing after super-saturation and quenching. On the basis of the performed examinations it was stated that small Ti addition to the binary ZnAl25 alloy, apart from structure refinement, accelerates decomposition of the primary α' phase giving stable structure in a shorter period of time in comparison with the alloy without Ti addition. Addition of Ti in amount of 1.6 wt.%, totally replacing Cu, allows obtaining stable structure and dimensions and allows avoiding structural instability caused by the metastable ε−CuZn4 phase present in the ZnAl26Cu2.2 alloy.

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Authors and Affiliations

W. Krajewski
P. Zak
J. Orava
A. Greer
P. Krajewski
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Abstract

ZnO thin layers were deposited on p-type silicon substrates by the sol-gel spin-coating method and, then, annealed at various temperatures in the range of 573–873 K. Photoluminescence was carried out in the temperature range of 20–300 K. All samples showed two dominant peaks that have UV emissions from 300 nm to 400 nm and visible emissions from 400 nm to 800 nm. Influence of temperature on morphology and chemical composition of fabricated thin layers was examined by XRD, SEM, FTIR, and Raman spectroscopy. These measurements indicate that ZnO structure is obtained for samples annealed at temperatures above 573 K. It means that below this temperature, the obtained thin films are not pure zinc oxide. Thus, annealing temperature significantly affected crystallinity of the thin films.

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Authors and Affiliations

M. Sypniewska
R. Szczesny
P. Popielarski
ORCID: ORCID
K. Strzalkowski
B. Derkowska-Zielinska
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Abstract

In this study, a new chemically modified cellulose polymer-capped ZnO nanopowder prepared by hydrothermal method using chemically modified cellulose polymer as capping agent was successfully reported. The structural characteristics of CMC-capped ZnO nanopowder was reported by FTIR, XRD, SEM and EDX studies. XRD results revealed crystallographic properties like crystal composition, phase purity and crystallite size of the prepared CMC-capped ZnO nanopowder and average size calculated by Debye Scherrer formula as 14.66 nm. EDX studies revealed that the presence of elemental compositions of capping agent in the nanopowder samples. The optical characterization of the CMC-capped ZnO nanopowder was studied using UV absorption (λmax = 303 nm) and PL spectroscopy (λex = 295 nm). The average crystal diameter and grain size were calculated by effective mass approximation formula and compared with XRD findings that agreed well and verified CMC capped ZnO with particle size of 193 nm. Thus, the promising optical characteristics shown by the synthesized CMC capped ZnO nanopowders exposes its potential usage in bio-medical fields.
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Authors and Affiliations

R. Jagadeeswari
1
P. Selvakumar
2
ORCID: ORCID
V. Jeevanantham
2
ORCID: ORCID
R. Saravanan
1

  1. Department of Chemistry, KPR Institute of Engineering And Technology, Coimbatore-641407, Tamilnadu, India
  2. Department of Chemistry, Vivekanandha College of Arts And Sciences for Women, Tiruchengode-637205, Tamilnadu, India
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Abstract

In this paper, detailed characterization of the oxide scale, grown on the Inconel 686 coating after high-temperature oxidation at 650°C in ashes from waste incineration power plant was performed. Phase composition, morphology, microstructure and chemical composition of the oxide scale were investigated using XRD and SEM analysis. Mechanisms of formation and growth of oxide scales were examined, resulting in the insights into oxidation kinetics. Results revealed presence of NiO in the outermost layer of the oxide scale. At the bottom of oxide scale, CrNi2O4 spinel layers were formed due to the increasing concentration of Cr. In the middle area of oxide scale, due to higher concentration of Cr and lower amount of Ni, the Cr2NiO4 spinel is formed. The innermost layer was composed of Cr2O3.
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Authors and Affiliations

M. Solecka
1
ORCID: ORCID
B. Rutkowski
2
ORCID: ORCID
A. Kopia
2
ORCID: ORCID

  1. Institute of Metallurgy and Materials Science, Polish Academy of Sciences, 25 Reymonta Str., 30-059 Krakow, Poland
  2. AGH University of Science and Technology, Faculty of Metals Engineering and Industrial Computer Science, Al. A. Mickiewicza 30, 30-059 Kraków, Poland
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Abstract

In this paper, study the preparation of Y-Fe alloy by reduction-diffusion process, which is novel technique for producing an alloy from its ores directly at different temperatures. From this work, investigates the particles size and morphology structure of alloy by X-Ray Diffraction (XRD), Energy dispersive-X-ray analyzer (EDAX) and Scanning Electron Microscope (SEM) respectively. Here study the thermodynamics of property of system such as Gibbs free energy and reaction kinetics of system respectively. The Vibrating Sample magnetometer (VSM) is used to study the magnetic properties of alloy such as cocerviety, saturation magnetization and retentivity.

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Authors and Affiliations

Marimuthu Ilayaraja
L. John Berchmans
Sankara Raman Sankaranarayan
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Abstract

In the present work, Hydroxyapatite synthesis was carried out using hydrothermal method with calcium nitrate tetrahydrate (Ca(NO 3) 2.4H 2O) and fosfor pentaoksit (P 2O 5) as precursors. For the hydrothermal method, constant reaction temperature (180°C) and different reaction times (6 hours, 12 hours, 18 hours and 24 hours) were determined. The samples produced were divided into two groups. Four samples were not heat treatment; four samples were heat treatment at 700°C for 1 hour. The obtained products were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) techniques, X-ray diffraction (XRD) and UV-Vis spectrometer. SEM photos showed that the Hydroxyapatite powders produced are in the form of the agglomerate. According to EDS results, Hydroxyapatite samples are of high purity. XRD’s findings confirm that the diffraction peaks correspond to the pure phase of Hydroxyapatite. A general decrease was observed in the energy band gap of the samples with increasing hydrothermal reaction time.
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Authors and Affiliations

Nida Kati
1
ORCID: ORCID
Sermin Ozan
1
ORCID: ORCID
Tülay Yildiz
1
ORCID: ORCID
Mehmet Arslan
1
ORCID: ORCID

  1. Fırat Unıversity, Faculty of Technology, Metallurgical and Materials Engineering Department, 23200, Elazığ, Turkiye
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Abstract

Carbon steel is one of the most widely used alloys in many industries, however, its use is limited by its low corrosion resistance. Depositing a layer of phosphate on its surface improves the corrosion resistance as well as other properties, such as wear resistance, adhesion etc. Accordingly, preliminary studies demonstrated that carbon steel coated with phosphate layers can be used in the manufacture of carabiners for various fields: civil engineering, oil industry etc. Whereas, to demonstrate their capacity to operate in severe conditions related to fire rescue and extinguishing operations, it is necessary to evaluate the thermal behaviour of these materials. Thus, the main goal of this paper is to study the behaviour at high temperatures of three different types of phosphate layers deposited on carbon steel surface, by STA analysis. Also, the paper aims to study the formation of different phosphate layers by determining the types of compounds formed after the completion of the phosphating process, by XRD analysis.
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Authors and Affiliations

D.-P. Burduhos-Nergis
1
ORCID: ORCID
C. Bejinariu
1
ORCID: ORCID
A.M. Cazac
1
ORCID: ORCID
A.V. Sandu
1
ORCID: ORCID
P. Vizureanu
1
ORCID: ORCID

  1. "Gheorghe Asachi” Technical University of Iasi, Faculty of Materials Science and Engineering, 41 “D. Mangeron” Street, 700050, Iasi, Romania
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Abstract

Zinc is present in electric arc furnace dust (EAFD) mainly in two basic minerals, namely as franklinite ZnFe2O4 and/or zincite ZnO. While zincite is relatively reactive and easily treatable, franklinite is considerably refractory, which causes problems during EAFD processing. In this work EAFD containing 18.53% Zn was leached in water solution of ammonium carbonate. This leaching solution selectively leaches zincite, while franklinite is refractory and stable against leaching in this case. The temperature dependence of zinc leaching from EAFD was studied and the activation energy EA was determined by two methods: 1.) classically based on zinc chemical analyses from the leaching solution and 2.) by using of X-Ray diffraction qualitative phase analyses of leaching residues. The determined values of activation energies 37.41 and 38.55 kJmol–1 match perfectly, which show the excellent possibility of using X-Ray diffraction toward the study of leaching kinetics at properly chosen experimental conditions. The important result is the determination of the amount zincite and franklinite in EAFD, which is not possible by using of classical chemical methods.
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Authors and Affiliations

T. Havlik
G. Maruskinova
A. Miskufova
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Abstract

The aim of these studies was to obtain single phase cubic modification of Li7La3Zr2O12 by mechanical milling and annealing of La(OH)3, Li2CO3 and ZrO2 powder mixture. Fritsch P5 planetary ball mill, Rigaku MiniFlex II X-ray diffractometer, Setaram TG-DSC 1500 analyser and FEI Titan 80-300 transmission electron microscope were used for sample preparation and investigations. The applied milling and annealing parameters allowed to obtain the significant contribution of c-Li7La3Zr2O12 in the sample structure, reaching 90%. Thermal measurements revealed more complex reactions requiring further studies.

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Authors and Affiliations

D. Oleszak
B. Kurowski
T. Pikula
M. Pawlyta
M. Senna
H. Suzuki
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Abstract

Equal-channel angular pressing (ECAP) was used as a technique for severe plastic deformation (SPD) on Al alloy AA3004. This technique produced fully dense materials of refined grain structure to sub-micrometer dimensions and advanced mechanical properties. The ECAP processing of samples was conducted as 1 to 4 passes through the die at room temperature. We present the results of the studied homogeneity evolution with the ECAP treatment. Furthermore, a Scanning Electron Microscope (SEM) was used for examination of the microstructure changes in samples undergone from 1 to 4 passes. The microhardness-HV increased upon each ECAP pass. The resulting micro-hardness evolution was attributed to crystalline microstructure modifications, such as the d-spacing (studied by X-ray Diffraction-XRD) depending on the number of ECAP pressings. The microcrystalline changes (grain refining evaluated from the Scanning Electron Microscopy – SEM images) were found to be related to the HV, following the Hall-Petch equation.

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Authors and Affiliations

N. Izairi
F. Ajredini
A. Vevecka-Pfiftaj
P. Makreski
M.M. Ristova
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Abstract

Nano technology is an emerging field of interest for civil engineering application. Among the nano materials presently used in concrete, nano-silica possess more pozzolanic nature. It has the capability to react with the free lime during the cement hydration and forms additional C-S-H gel giving strength, impermeability and durability to concrete. Present paper investigates the effects of addition of nano silica in normal strength concrete. Three types of nano-silica in the form of nano suspension having different amount of silica content have been investigated. Mix design has been carried out by using particle packing method. X-Ray diffraction (XRD) analysis has been carried out to find the chemical composition of control concrete and nano modified concrete. Further, experimental investigations have been carried out to characterize the mechanical behaviour in compression, tension and flexure. It has been observed that the addition of nano-silica in normal strength concrete increased the compressive strength and decreased the spilt tensile strength and flexural strength. Also, Rapid chloride permeability test (RCPT) has been conducted to know the chloride permeability of control concrete, nano modified concrete, and nano coated concrete. It has been observed that the chloride permeability is less for nano coated concrete.

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Authors and Affiliations

S. Gopinath
P.Ch. Mouli
A.R. Murthy
N.R. Iyer
S. Maheswaran
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Abstract

The article presents the results of research concerning to AlCu4MgSi alloy ingots produced using horizontal continuous casting process. The presented research was focused on the precise determination of phase composition of the precipitates formed during the solidification of ingots and the analysis of their thermal stability. In order to assess the morphology of precipitates in the AlCu4MgSi alloy, data obtained by using a computer simulation of thermodynamic phenomena were compiled with results obtained using advanced research techniques, i.e. High-temperature X-ray diffraction (HT-XRD), SEM-EDS, Thermal and derivative analysis (TDA) and Glow discharge optical emission spectroscopy (GD OES). SEM observations and analysis of chemical composition in micro-areas showed that the precipitates are mainly intermetallic θ-Al2Cu and β-Mg2Si phases, and also presence of Al19Fe4MnSi2 intermetallic phase was confirmed by X-ray diffraction studies. Based on the prepared Thermo-Calc simulation data, high-temperature X-ray diffraction measurements were conducted.

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Authors and Affiliations

P.M. Nuckowski
M. Kondracki
T. Wróbel
ORCID: ORCID
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Abstract

In the presented work, the conditions of the high-temperature and mechanochemical method for the synthesis of compound Sm 5VO 10 and their influence on its physicochemical properties were studied. The following methods were used for the study: X-ray powder diffraction (XRD), differential thermal analysis (DTA), infrared spectroscopy (FTIR), ultraviolet and visible light spectroscopy (UV–VIS–DRS), scanning electron microscopy (SEM-EDX), and laser beam diffraction spectrometry (LDS). Based on the results, it was determined that the compound Sm 5VO 10 is thermally stable in air atmospheres up to 1475 °C, crystallises in a monoclinic system, and its structure is made up of oxygen VO 4 and SmO 8 polyhedra. The estimated energy gap value for nanometric, mechanochemically obtained Sm 5VO 10 was about 3.20 eV, and for the microcrystalline, obtained with the high-temperature method, was about 2.75 eV. The established physicochemical characterisation of Sm 5VO 10 initially showed that the compound could find potential applications, e.g. as a photocatalyst for water purification or as a component of new optoelectronic materials.
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Authors and Affiliations

Kamil Kwiatkowski
1
ORCID: ORCID
Mateusz Piz
1
ORCID: ORCID
Elżbieta Filipek
1
ORCID: ORCID

  1. West Pomeranian University of Technology in Szczecin, Faculty of Chemical Technology and Engineering, Piastów 42, 71-065 Szczecin, Poland
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Abstract

The paper aims to show a search method for optimal conditions of 3A, 13X, ZSM-5 zeolite thermal regeneration after adsorption from a liquid water-isopropanol mixture. Comparative TGA-DTG results for heating of wet zeolites with different structure and hydrophobicity showed characteristic effects corresponding to the optimal temperature of zeolite regeneration. The consequences of overheating and collapse of the 3A, 13X, ZSM-5 zeolite structure at temperatures of 850, 900, 1000 °C, respectively, were recorded with XRD method. Moreover, XRD and NIR/DRS tests of loaded and regenerated zeolite samples showed interaction of adsorbate and co-adsorbed water with adsorbent and revealed influence of adsorption and regeneration processes on the adsorbent structure. Investigations of the regeneration of the zeolite 3A bed after adsorption of water from the isopropanol solution in the temperature swing adsorption (TSA) process were carried out by heating the bed with inert gas at 250 °C and different purge gas streams in the range of 1.68–2.40 kg/h. Four stages of wet bed regeneration were distinguished, which corresponded to the effect observed during TGA-DTG tests. For each stage, the specific demand for purge gas and energy was determined depending on the gas stream and its minimum value of 2.16 kg/h was indicated.
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Authors and Affiliations

Piotr Tabero
1
ORCID: ORCID
Elżbieta Gabruś
2

  1. West Pomeranian University of Technology in Szczecin, Faculty of Chemical Technologyand Engineering, Department of Inorganic and Analytical Chemistry, Piastów 42, 71-065 Szczecin, Poland
  2. West Pomeranian University of Technology in Szczecin, Faculty of Chemical Technology and Engineering, Department of Chemicaland Process Engineering, Piastów 42, 71-065 Szczecin, Poland
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Abstract

The Matmata region, located in the south of Gabès (Tunisia), experienced significant damage during the floods of the Beni zelten wadi on November 11, 2017. These floods, exacerbated by the steep slopes and underlying soil conditions, led to the occurrence of debris flows, posing a threat to road infrastructure. The generation of debris flows is closely linked to intense rainfall events that surpass the soil capacity to retain water. To gain insights into the behaviour of the soil samples, various characteristics were analysed, including texture, clay mineralogy, grain size distribution, and Atterberg limits. The results showed that the mean liquid limit values ranged from 38% to 62%, while the mean plasticity index of the materials in the landslide-prone areas varied from 18% to 27.9%. These findings indicate presence of clay formations and highlight a significance of the increased soil clay content as contributing factors to landslide development. The X-ray Diffraction analysis revealed that gypsum, quartz, phyllosilicate and calcite minerals were the most abundant minerals identified in the soil samples. This work shows the importance of clay mineral and geotechnical parameters of the soils in the occurrence of landslides and predicting debris flows occurrences in the Matmata region.
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Authors and Affiliations

Hassen Bensalem
1 2
Soulef Amamria
3
Mohamed Sadok Bensalem
3
Claudia Meisina
4
Noureddine Hamdi
1 2

  1. Higher Institute of the Sciences and Techniques of Waters of Gabes, University of Gabes,6072 Zrig Gabès, Tunisia
  2. Laboratory of composite materials and clay minerals, National Center for Research in Materials Science Borj Cedria (CNRSM), B.P. 73‑8020 Soliman, Tunisia
  3. Faculty of Sciences Gabes,University of Gabes, 6072 Hatem BETTAHER Erriadh city Gabes, Tunisia
  4. Department of Earth and Envirnmontal Sciences, University of Pavia, 27100 Via Ferrata 9 Pavia, Italy
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Abstract

The aim of the paper is the residual stress analysis of AlSi10Mg material fabricated by selective laser melting (SLM). The SLM technique allows to product of complex geometries based on three-dimensional model, in which stiffness and porosity can be precisely designed for specific uses. As the studied material, there were chosen solid samples built in two different directions: parallel (P-L) and perpendicular (P-R) to the tested surface and cellular lattice built in perpendicular direction, as well. In the paper, for the complex characterization of obtained materials, the phase analysis, residual stress and texture studies were performed. The classical non-destructive sin2ψ method was used to measure the residual stress measurements.

The final products, both solid sample and cellular lattice, have a homogeneous phase composition and consist of solid solution Al(Si) (Fm-3m) type, Si (Fd-3m) and Mg2Si (Pnma). The obtained values of the crystallite size are in a range of 1000 Å for Al(Si), 130-180 Å for Si phase. For Mg2Si phase, the crystallite sizes depend on sintering process, they are 800 Å for solid samples and 107 Å for cellular lattice. The residual stress results have the compressive character and they are in a range from –5 to –15 MPa.

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Authors and Affiliations

M. Karolus
J. Maszybrocka
A. Stwora
G. Skrabalak
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Abstract

The present work comprises the development of Al6061/nano Al2O3 composites with 0 to 4 weight percent in steps of 0.5 wt. % of nano alumina particles by using ultrasonic assisted stir casting. Casted samples were subjected to heat treatment and hot forging. Further forged and heat-treated gear blanks of nano Al2O3 (0 to 3.0 weight %) reinforced nanocomposites were machined to make spur gears for the wear test. The results have shown that nano Al2O3 reinforcement in the Al6061 matrix with heat treatment and forging improves the hardness and compressive strength up to 3.5 wt. %, after that, it starts decreasing because of the agglomeration of nano alumina particles. SEM results reveal grain refinement of the pure alloy after reinforcement. Removal of porosity and voids observed after forging operation. Wear resistance increasing with incorporation of Al2O3 nanoparticles in base alloy, reinforcement wt. %, precipitation hardening and hot forging also improves wear resistance and mechanical properties. These composites have widespread applications in gear, brake discs, crankshaft, clutch plates, pistons, and other components of automobiles and aircraft structures.
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Authors and Affiliations

Rajesh Purohit
1
M.M.U. Qureshi
1
Ashish Kumar
1
ORCID: ORCID
Abhishek Mishra
1
R.S. Rana
1

  1. Mechanical Engineering Department, MANIT, Bhopal, India-462003

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