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13 pages, 2207 KiB

Open AccessArticle

Characterization of Zr-Containing Dispersoids in Al–Zn–Mg–Cu Alloys by Small-Angle Scattering

by Mohammad Taha Honaramooz, Roland Morak, Stefan Pogatscher, Gerhard Fritz-Popovski, Thomas M. Kremmer, Thomas C. Meisel, Johannes A. Österreicher, Aurel Arnoldt and Oskar Paris

Materials 2023, 16(3), 1213; https://doi.org/10.3390/ma16031213 - 31 Jan 2023

Cited by 6 | Viewed by 1957

Abstract

The characterization of Zr-containing dispersoids in aluminum alloys is challenging due to their broad size distribution, low volume fraction, and heterogeneous distribution within the grains. In this work, small-angle X-ray scattering (SAXS) and small-angle neutron scattering (SANS) were compared to scanning electron microscopy [...] Read more.

The characterization of Zr-containing dispersoids in aluminum alloys is challenging due to their broad size distribution, low volume fraction, and heterogeneous distribution within the grains. In this work, small-angle X-ray scattering (SAXS) and small-angle neutron scattering (SANS) were compared to scanning electron microscopy (SEM) and transmission electron microscopy (TEM) regarding their capability to characterize Zr-containing dispersoids in aluminum alloys. It was demonstrated that both scattering techniques are suitable tools to characterize dispersoids in a multi-phase industrial 7xxx series aluminum alloy. While SAXS is more sensitive than SANS due to the high electron density of Zr-containing dispersoids, SANS has the advantage of being able to probe a much larger sample volume. The combination of both scattering techniques allows for the verification that the contribution from dispersoids can be separated from that of other precipitate phases such as the S-phase or GP-zones. The size distributions obtained from SAXS, SANS and TEM showed good agreement. The SEM-derived size distributions were, however, found to significantly deviate from those of the other techniques, which can be explained by considering the resolution-limited restrictions of the different techniques. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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17 pages, 6249 KiB

Open AccessArticle

Comparison of 2D and 3D Plasma Electrolytic Oxidation (PEO)-Based Coating Porosity Data Obtained by X-ray Tomography Rendering and a Classical Metallographic Approach

by Polina Karlova, Maria Serdechnova, Carsten Blawert, Xiaopeng Lu, Marta Mohedano, Domonkos Tolnai, Berit Zeller-Plumhoff and Mikhail L. Zheludkevich

Materials 2022, 15(18), 6315; https://doi.org/10.3390/ma15186315 - 12 Sep 2022

Cited by 7 | Viewed by 1688

Abstract

In this work, the porosity of plasma electrolytic oxidation (PEO)-based coatings on Al- and Mg-based substrates was studied by two imaging techniques—namely, SEM and computer microtomography. Two approaches for porosity determination were chosen; relatively simple and fast SEM surface and cross-sectional imaging was [...] Read more.

In this work, the porosity of plasma electrolytic oxidation (PEO)-based coatings on Al- and Mg-based substrates was studied by two imaging techniques—namely, SEM and computer microtomography. Two approaches for porosity determination were chosen; relatively simple and fast SEM surface and cross-sectional imaging was compared with X-ray micro computed tomography (microCT) rendering. Differences between 2D and 3D porosity were demonstrated and explained. A more compact PEO coating was found on the Al substrate, with a lower porosity compared to Mg substrates under the same processing parameters. Furthermore, huge pore clusters were detected with microCT. Overall, 2D surface porosity calculations did not show sufficient accuracy for them to become the recommended method for the exact evaluation of the porosity of PEO coatings; microCT is a more appropriate method for porosity evaluation compared to SEM imaging. Moreover, the advantage of 3D microCT images clearly lies in the detection of closed and open porosity, which are important for coating properties. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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22 pages, 5553 KiB

Open AccessArticle

Design and Evaluation of Orally Dispersible Tablets Containing Amlodipine Inclusion Complexes in Hydroxypropyl-β-cyclodextrin and Methyl-β-cyclodextrin

by Marian Novac, Adina Magdalena Musuc, Emma Adriana Ozon, Iulian Sarbu, Mirela Adriana Mitu, Adriana Rusu, Simona Petrescu, Irina Atkinson, Daniela Gheorghe and Dumitru Lupuliasa

Materials 2022, 15(15), 5217; https://doi.org/10.3390/ma15155217 - 28 Jul 2022

Cited by 8 | Viewed by 2443

Abstract

The development of new orally dispersible tablets containing amlodipine (AML) inclusion complexes in hydroxypropyl-β-cyclodextrin (HP-β-CD) and in methyl-β-cyclodextrin (Me-β-CD) was studied. The methods of obtaining amlodipine and the physical and chemical properties of the inclusion complexes using the two cyclodextrins was investigated separately. [...] Read more.

The development of new orally dispersible tablets containing amlodipine (AML) inclusion complexes in hydroxypropyl-β-cyclodextrin (HP-β-CD) and in methyl-β-cyclodextrin (Me-β-CD) was studied. The methods of obtaining amlodipine and the physical and chemical properties of the inclusion complexes using the two cyclodextrins was investigated separately. Solid inclusion complexes were obtained by three methods: kneading, coprecipitation, and lyophilization, at a molar ratio of 1:1. For comparison, a physical mixture in the same molar ratio was prepared. The aim of the complexation process was to improve the drug solubility. As the lyophilization method leads to a complete inclusion of the drug in the guest molecule cavity, for both used cyclodextrins, these types of compounds were selected as active ingredients for the design of orally dispersible tablets. Subsequently, the formulation of the orodispersible tablets containing AML-HP-β-CD and AML-Me-β-CD inclusion complexes and quality parameters of the final formulation were evaluated. The results prove that F1 and F4 formulations, based on silicified microcrystalline cellulose, which contains insignificant proportions of very small or very large particles, had the lowest moisture degree (3.52% for F1 and 4.03% for F4). All of these demonstrate their porous structure, which led to good flowability and compressibility performances. F1 and F4 formulations were found to be better to manufacture orally dispersible tablets. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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15 pages, 4634 KiB

Open AccessArticle

Experimental Investigation of the Tensile Behavior of Selected Tire Cords Using Novel Testing Equipment

by Paweł Bogusz, Danuta Miedzińska and Marcin Wieczorek

Materials 2022, 15(12), 4163; https://doi.org/10.3390/ma15124163 - 12 Jun 2022

Cited by 2 | Viewed by 2040

Abstract

Aramid and polyamide cords are used in a wide range of applications, particularly in the automotive industry (tire reinforcement) and textile industry for military and fireguard purposes. The problem of the reliable experimental study of tensile behavior of synthetic cords is considered in [...] Read more.

Aramid and polyamide cords are used in a wide range of applications, particularly in the automotive industry (tire reinforcement) and textile industry for military and fireguard purposes. The problem of the reliable experimental study of tensile behavior of synthetic cords is considered in this paper. In the available standards for synthetic cord testing, particularly ASTM D 885-03, the tensile test must result with the cord damage in the middle of gauge length, and the cords should be fixed in the machine clamps. The trial test gave damage near the clamps. We propose a novel testing stage mounted in the testing machine clamps to achieve the uniform tensile stress distribution in the gauge length of the measured cords. The results of the deformations were measured in two ways: using testing machine head displacement and a videoextensometer. Stress curves of four distinguished cords were evaluated and compared. The second method allowed to acquire results differing from the manufacturers’ data from 0.7% to 21.5%, which allowed for the conclusion that the designed test stand allows for obtaining reliable results for stretched cords. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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13 pages, 8386 KiB

Open AccessArticle

Surface Analysis of Fermented Wheat and Rice Starch Used for Coating Traditional Korean Textiles

by Hye Hyun Yu, Youngseo Lee, Yun-Sik Nam, Man-Ho Kim, Kang-Bong Lee and Yeonhee Lee

Materials 2022, 15(6), 2001; https://doi.org/10.3390/ma15062001 - 8 Mar 2022

Cited by 2 | Viewed by 2062

Abstract

Wheat and rice starches, traditionally used to stiffen fabric, become less contaminated and more antiseptic after fermentation for several years, thus enhancing their functional activity. In the present study, analytical techniques using particle size analysis, a gloss meter and a colorimeter were used [...] Read more.

Wheat and rice starches, traditionally used to stiffen fabric, become less contaminated and more antiseptic after fermentation for several years, thus enhancing their functional activity. In the present study, analytical techniques using particle size analysis, a gloss meter and a colorimeter were used to measure the physical properties of wheat and rice starches that had been fermented for 5 and 7 years, respectively. Their chemical contents and composition were determined by nutrient measurements and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The ToF-SIMS spectra and ion images showed that fermented starch contained more carbohydrate and less lipid than fresh starch. The surface morphologies of the fermented starch granules and starch-coated textiles were examined by scanning electron microscopy and compared with the surface morphologies of fresh starch granules. The fermented wheat and rice starch granules were smaller and more rounded with a lower level of N-containing compounds (proteins) and exhibited more antiseptic properties than fresh starch granules. The results showed that physical measurements and chemical analysis were simple and complementary techniques for investigating traditional Korean starch materials and textiles. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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24 pages, 2469 KiB

Open AccessArticle

The Art of Positronics in Contemporary Nanomaterials Science: A Case Study of Sub-Nanometer Scaled Glassy Arsenoselenides

by Oleh Shpotyuk, Adam Ingram, Catherine Boussard-Pledel, Bruno Bureau, Zdenka Lukáčová Bujňáková, Peter Baláž, Bohdan Mahlovanyi and Yaroslav Shpotyuk

Materials 2022, 15(1), 302; https://doi.org/10.3390/ma15010302 - 1 Jan 2022

Cited by 7 | Viewed by 1874

Abstract

The possibilities surrounding positronics, a versatile noninvasive tool employing annihilating positrons to probe atomic-deficient sub-nanometric imperfections in a condensed matter, are analyzed in application to glassy arsenoselenides g-As_xSe_100−x (0 < x < 65), subjected to dry and wet (in 0.5% [...] Read more.

The possibilities surrounding positronics, a versatile noninvasive tool employing annihilating positrons to probe atomic-deficient sub-nanometric imperfections in a condensed matter, are analyzed in application to glassy arsenoselenides g-As_xSe_100−x (0 < x < 65), subjected to dry and wet (in 0.5% PVP water solution) nanomilling. A preliminary analysis was performed within a modified two-state simple trapping model (STM), assuming slight contributions from bound positron–electron (Ps, positronium) states. Positron trapping in g-As_xSe_100−x/PVP nanocomposites was modified by an enriched population of Ps-decay sites in PVP. This was proven within a three-state STM, assuming two additive inputs in an overall trapping arising from distinct positron and Ps-related states. Formalism of x3-x2-CDA (coupling decomposition algorithm), describing the conversion of Ps-decay sites into positron traps, was applied to identify volumetric nanostructurization in wet-milled g-As-Se, with respect to dry-milled ones. Under wet nanomilling, the Ps-decay sites stabilized in inter-particle triple junctions filled with PVP replaced positron traps in dry-milled substances, the latter corresponding to multi-atomic vacancies in mostly negative environments of Se atoms. With increased Se content, these traps were agglomerated due to an abundant amount of Se-Se bonds. Three-component lifetime spectra with nanostructurally- and compositionally-tuned Ps-decay inputs and average lifetimes serve as a basis to correctly understand the specific “rainbow” effects observed in the row from pelletized PVP to wet-milled, dry-milled, and unmilled samples. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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16 pages, 7315 KiB

Open AccessArticle

High-Resolution Microstructure Characterization of Additively Manufactured X5CrNiCuNb17-4 Maraging Steel during Ex and In Situ Thermal Treatment

by Mihaela Albu, Bernd Panzirsch, Hartmuth Schröttner, Stefan Mitsche, Klaus Reichmann, Maria Cecilia Poletti and Gerald Kothleitner

Materials 2021, 14(24), 7784; https://doi.org/10.3390/ma14247784 - 16 Dec 2021

Cited by 3 | Viewed by 2297

Abstract

Powder and selective laser melting (SLM) additively manufactured parts of X5CrNiCuNb17-4 maraging steel were systematically investigated by electron microscopy to understand the relationship between the properties of the powder grains and the microstructure of the printed parts. We prove that satellites, irregularities and [...] Read more.

Powder and selective laser melting (SLM) additively manufactured parts of X5CrNiCuNb17-4 maraging steel were systematically investigated by electron microscopy to understand the relationship between the properties of the powder grains and the microstructure of the printed parts. We prove that satellites, irregularities and superficial oxidation of powder particles can be transformed into an advantage through the formation of nanoscale (AlMnSiTiCr) oxides in the matrix during the printing process. The nano-oxides showed extensive stability in terms of size, spherical morphology, chemical composition and crystallographic disorder upon in situ heating in the scanning transmission electron microscope up to 950 °C. Their presence thus indicates a potential for oxide-dispersive strengthening of this steel, which may be beneficial for creep resistance at elevated temperatures. The nucleation of copper clusters and their evolution into nanoparticles, and the precipitation of Ni and Cr particles upon in situ heating, have been systematically documented as well. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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15 pages, 3286 KiB

Open AccessArticle

Demonstration of Near Edge X-ray Absorption Fine Structure Spectroscopy of Transition Metals Using Xe/He Double Stream Gas Puff Target Soft X-ray Source

by Tomasz Fok, Przemysław Wachulak, Łukasz Węgrzyński, Andrzej Bartnik, Michał Nowak, Piotr Nyga, Jerzy Kostecki, Barbara Nasiłowska, Wojciech Skrzeczanowski, Rafał Pietruszka, Karol Janulewicz and Henryk Fiedorowicz

Materials 2021, 14(23), 7337; https://doi.org/10.3390/ma14237337 - 30 Nov 2021

Cited by 2 | Viewed by 2139

Abstract

A near 1-keV photons from the Xe/He plasma produced by the interaction of laser beam with a double stream gas puff target were employed for studies of L absorption edges of period 4 transitional metals with atomic number Z from 26 to 30. [...] Read more.

A near 1-keV photons from the Xe/He plasma produced by the interaction of laser beam with a double stream gas puff target were employed for studies of L absorption edges of period 4 transitional metals with atomic number Z from 26 to 30. The dual-channel, compact NEXAFS system was employed for the acquisition of the absorption spectra. L_1–3 absorption edges of the samples were identified in transmission mode using broadband emission from the Xe/He plasma to show the applicability of such source and measurement system to the NEXAFS studies of the transition metals, including magnetic materials. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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15 pages, 13211 KiB

Open AccessArticle

An In Situ Synchrotron Dilatometry and Atomistic Study of Martensite and Carbide Formation during Partitioning and Tempering

by Ernst Plesiutschnig, Mihaela Albu, David Canelo-Yubero, Vsevolod I. Razumovskiy, Andreas Stark, Norbert Schell, Gerald Kothleitner, Coline Beal, Christof Sommitsch and Ferdinand Hofer

Materials 2021, 14(14), 3849; https://doi.org/10.3390/ma14143849 - 9 Jul 2021

Viewed by 2771

Abstract

Precipitation hardened and tempered martensitic-ferritic steels (TMFSs) are used in many areas of our daily lives as tools, components in power generation industries, or in the oil and gas (O&G) industry for creep and corrosion resistance. In addition to the metallurgical and forging [...] Read more.

Precipitation hardened and tempered martensitic-ferritic steels (TMFSs) are used in many areas of our daily lives as tools, components in power generation industries, or in the oil and gas (O&G) industry for creep and corrosion resistance. In addition to the metallurgical and forging processes, the unique properties of the materials in service are determined by the quality heat treatment (HT). By performing a quenching and partitioning HT during an in situ high energy synchrotron radiation experiment in a dilatometer, the evolution of retained austenite, martensite laths, dislocations, and carbides was characterized in detail. Atomic-scale studies on a specimen with the same HT subjected to a laser scanning confocal microscope show how dislocations facilitate cloud formation around carbides. These clouds have a discrete build-up, and thermodynamic calculations and density functional theory explain their stability. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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13 pages, 26744 KiB

Open AccessArticle

Modification of Mechanical Properties of Expansive Soil from North China by Using Rice Husk Ash

by Mazahir M. M. Taha, Cheng-Pei Feng and Sara H. S. Ahmed

Materials 2021, 14(11), 2789; https://doi.org/10.3390/ma14112789 - 24 May 2021

Cited by 14 | Viewed by 3130

Abstract

The construction of buildings on expansive soils poses considerable risk of damage or collapse due to soil shrinkage or swelling made likely by the remarkable degree compressibility and weak shear resistance of such soils. In this research, rice husk ash (RHA) was added [...] Read more.

The construction of buildings on expansive soils poses considerable risk of damage or collapse due to soil shrinkage or swelling made likely by the remarkable degree compressibility and weak shear resistance of such soils. In this research, rice husk ash (RHA) was added to expansive soil samples in different quantities of 0%, 4%, 8%, 12%, and 16% by weight of soil to determine their effects on the plasticity index, compaction parameters, consolidation performance, and California bearing ratio (CBR)of clay soil. The results show that the use of RHA increases the effective stress and decreases the void ratio and coefficient of consolidation. Adding 16% RHA resulted in the greatest reduction in the hydraulic conductivity, void ratio, and coefficient of consolidation. The void ratio decreased from 0.96 to 0.93, consolidation coefficient decreased from 2.52 to 2.33 cm²/s, and hydraulic conductivity decreased from 1.12 to 0.80 cm/s. The addition of RHA improved the soil properties and coefficient of consolidation due to the high density and cohesiveness of RHA. The results of this study can be used to provide a suitable basis for the treatment of expansive soil to provide improved conditions for infrastructure construction. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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21 pages, 7018 KiB

Open AccessArticle

Thermal and Mechanical Characterization of Carbides for High Temperature Nuclear Applications

by Mattia Manzolaro, Stefano Corradetti, Michele Ballan, Riccardo Salomoni, Alberto Andrighetto and Giovanni Meneghetti

Materials 2021, 14(10), 2689; https://doi.org/10.3390/ma14102689 - 20 May 2021

Cited by 10 | Viewed by 2472

Abstract

In the facilities for the production of Radioactive Ion Beams (RIBs) according to the Isotope Separation On-Line (ISOL) technique, a production target is typically impinged by a high-power primary beam, generating radioactive isotopes for basic research and technological applications. With the aim to [...] Read more.

In the facilities for the production of Radioactive Ion Beams (RIBs) according to the Isotope Separation On-Line (ISOL) technique, a production target is typically impinged by a high-power primary beam, generating radioactive isotopes for basic research and technological applications. With the aim to guarantee an efficient extraction of the aforementioned isotopes, the production target must work in a high vacuum environment, at temperatures that are usually between 1600 °C and 2200 °C. Its main components are often characterized by intense temperature gradients and consequently by severe thermal stresses. Carbides are widely used for target manufacturing, and in this work a specific method for their thermal and mechanical characterization is presented and discussed. It is based on the comparison between experimental measurements and numerical simulations, with the introduction of the novel Virtual Thermoelastic Parameters approach for the structural verification procedure. High-performance silicon carbides (SiC) are taken as a reference to describe the method. Measured emissivity and thermal conductivity data are presented and discussed, together with the experimental estimation of material limitations for both temperature and stress fields. The aforementioned results can be promptly used for the design process of high-power ISOL targets. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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Review

Jump to: Research

24 pages, 7106 KiB

Open AccessReview

Analysis of Non-Metallic Inclusions by Means of Chemical and Electrolytic Extraction—A Review

by Shashank Ramesh Babu and Susanne Katharina Michelic

Materials 2022, 15(9), 3367; https://doi.org/10.3390/ma15093367 - 7 May 2022

Cited by 8 | Viewed by 2675

Abstract

Research on non-metallic inclusions is of critical importance, as they have a significant influence on the final properties of steel products. In this regard, the 3D analysis of inclusions isolated from steel samples allows for the accurate measurement of their chemical composition, without [...] Read more.

Research on non-metallic inclusions is of critical importance, as they have a significant influence on the final properties of steel products. In this regard, the 3D analysis of inclusions isolated from steel samples allows for the accurate measurement of their chemical composition, without the influence of the steel matrix, and detailed insights into their morphology. Inclusions can be extracted from the steel sample matrix using extraction methods followed by their measurement with scanning electron microscopy. Extraction methods can be broadly classified into chemical and electrolytic analyses. There have been numerous studies documenting the different extraction methods for the isolation of different inclusion types in a range of steels. The focus of this paper is to briefly review their developments over a century up until the present period. The most relevant methods and the corresponding steels and observed inclusions are also summarized in a table which could be a useful reference for researchers in this field. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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21 pages, 4675 KiB

Open AccessReview

Microwave Measurements of Electromagnetic Properties of Materials

by Jerzy Krupka

Materials 2021, 14(17), 5097; https://doi.org/10.3390/ma14175097 - 6 Sep 2021

Cited by 24 | Viewed by 4218

Abstract

A review of measurement methods of the basic electromagnetic parameters of materials at microwave frequencies is presented. Materials under study include dielectrics, semiconductors, conductors, superconductors, and ferrites. Measurement methods of the complex permittivity, the complex permeability tensor, and the complex conductivity and related [...] Read more.

A review of measurement methods of the basic electromagnetic parameters of materials at microwave frequencies is presented. Materials under study include dielectrics, semiconductors, conductors, superconductors, and ferrites. Measurement methods of the complex permittivity, the complex permeability tensor, and the complex conductivity and related parameters, such as resistivity, the sheet resistance, and the ferromagnetic linewidth are considered. For dielectrics and ferrites, the knowledge of their complex permittivity and the complex permeability at microwave frequencies is of practical interest. Microwave measurements allow contactless measurements of their resistivity, conductivity, and sheet resistance. These days contactless conductivity measurements have become more and more important, due to the progress in materials technology and the development of new materials intended for the electronic industry such as graphene, GaN, and SiC. Some of these materials, such as GaN and SiC are not measurable with the four-point probe technique, even if they are conducting. Measurement fixtures that are described in this paper include sections of transmission lines, resonance cavities, and dielectric resonators. Full article

(This article belongs to the Special Issue Advanced Techniques for Materials Characterization)

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