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At least 811 records · Page 45

Residual glass and crystalline phases in a barium disilicate glass–ceramic

Investigations about the presence of residual glass are scarce, despite its fundamental role in the crystallization kinetics and luminescent properties of barium disilicate glass–ceramics (BaO·2SiO{sub 2}–BS{sub 2}) with a quasi-stoichiometric composition. Non-isothermal (DTA/DSC) experiments have demonstrated that BS{sub 2} presents a polymorphic transformation, where the h-BS{sub 2} (monoclinic structure) phase is completely transformed in l-BS{sub 2} (orthorhombic structure) at temperatures higher than 1020 °C (10 °C/min). In this study, BS{sub 2} monolithic samples were heat-treated at 1000 °C (BS2-10) and 1100 °C (BS2-11) in a DSC furnace at a heating rate of 10 °C/min. In addition, the crystalline and amorphous phases were characterized and quantified by Transmission Electron Microscopy (TEM) and X-ray Diffraction (XRD) experiments, respectively. Although the complete polymorphic transformation from h-BS2 to l-BS2 was achieved at 1100 °C, our results demonstrated that BS2-11 contains a minor, albeit not negligible, amount of residual glass. - Highlights: • The crystalline and amorphous phases in a barium disilicate glass were characterized and quantified by XRD and TEM. • The BS2-10 sample was constituted by two main crystalline phases, which consists of 2 polymorphic forms: h-BS2 and l-BS2. • The orthorhombic BS2 phase (l-BS2) was predominant at 1100 °C. • The complete polymorphic transformation from h-BS2 to l-BS2 was achieved at 1100 °C. • Nevertheless, our XRD and TEM results demonstrated that BS2-11 contains a minor amount of residual glass.

36 MATERIALS SCIENCE↗

Characterization of ZnAl cast alloys with Na addition

This study was aimed at evaluating the microstructural change and thermal, electrical and mechanical properties with the addition of Na to eutectic ZnAl alloys. Solders based on eutectic ZnAl containing 0.2 to 3.0 (wt.%) of Na were developed for high temperature solder. Differential scanning calorimetry (DSC) measurements were performed to determine the melting temperatures of the alloys. Thermal linear expansion and electrical resistivity measurements were performed over − 50 °C to 300 °C and 30 °C to 300 °C temperature ranges, respectively. The microstructure of the specimens was analyzed using scanning (SEM) and transmission electron microscopy (TEM) techniques. Chemical microanalysis was performed by energy-dispersive X-ray spectroscopy (EDS) on SEM and TEM. The precipitates of NaZn{sub 13} were confirmed by X-ray diffraction (XRD) measurements and selected area electron diffraction (SAED) techniques. The addition of Na to eutectic ZnAl alloy increased the electrical resistivity and reduced the coefficient of thermal expansion; however, the melting point did not change. The mechanical properties, strain and microhardness increased with Na content in alloys. - Highlights: • High temperature soldering materials of ZnAl with Na were designed and characterized. • Precipitates of NaZn{sub 13}were observed and confirmed using TEM and XRD. • Addition of Na to eutectic ZnAl cussed increased mechanical properties. • NaZn{sub 13} caused increased electrical resistivity and microhardness, and reduced the CTE.

36 MATERIALS SCIENCE↗

Oxidation controlled phase composition of FeCo(Zr) nanoparticles in CaF{sub 2} matrix

Results of the study of oxidised (FeCoZr){sub x}(CaF{sub 2}){sub 100−x} films in a wide composition range (30 ≤ x ≤ 74 at.%) sintered at oxygen pressures P{sub O} = 4.3 and 9.8 mPa with X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray absorption spectroscopy (XAS), {sup 57}Fe Mössbauer spectroscopy (MS), and vibrating sample magnetometry (VSM) are reported. A “crystalline metallic core–amorphous oxide shell” structure of nanoparticles (NPs) in films oxidised at lower P{sub O} = 4.3 mPa is observed in TEM images. A combined use of XRD, MS and XAS techniques provides identification of NP phase composition evidencing α-FeCo(Zr) core of the variable content depending on x and a complex oxide shell including amorphous α-Fe{sup 3+}{sub 2}O{sub 3} together with Co{sup 2+}{sub 1−y}Fe{sup 2+}{sub y}O at low x (30–36 at.%). Full oxidation of NPs at higher P{sub O} = 9.8 mPa is indicated by TEM, XRD, MS and XAS patterns evidencing the formation of “crystalline Co{sup 2+}{sub 1−y}Fe{sup 2+}{sub y}O core–amorphous α-Fe{sup 3+}{sub 2}O{sub 3} shell” structure. Progressive oxidation of NPs with decreasing x at P{sub O} = 4.3 mPa as well as with P{sub O} increase is followed by variation of average centre shifts < δ > obtained from deconvoluted {sup 57}Fe Mössbauer spectra. Magnetometry measurements of films sintered at P{sub O} = 4.3 mPa reveal an effect of exchange bias confirming “ferromagnetic metallic core–antiferromagnetic oxide shell” structure of NPs. The results show that phase composition of oxide shells is governed both by concentration of oxygen available during synthesis and on the x. Schemes of progressive NP oxidation with identified phase composition as a function of P{sub O} and x values are proposed. - Highlights: • A selective oxidation of Fe in Fe–Co nanoparticles, NPs, is revealed. • Oxidation controlled composition of Fe–Co NPs in CaF{sub 2} matrix is determined. • “Metallic core–amorphous oxide shell”-like NPs are obtained at low oxygen pressure. • “Crystalline core–amorphous shell” oxide structures appear at high oxygen pressure. • A scheme of phase occurrence and structure of nanoparticles is proposed.

36 MATERIALS SCIENCE↗

A transmission Kikuchi diffraction study of cementite in a quenched and tempered steel

This is the first transmission Kikuchi diffraction (TKD) study to report the indexing of nano-sized cementite as distinct structures and its orientation relationship with the body-centered cubic matrix in a quenched and tempered steel. Crystallographic analysis via TKD and selected area diffraction returned the well-known Bagaryatskii and Isaichev orientation relationships. However, the indexing of nano-sized cementite via TKD was sensitive to the thickness of the electron transparent region such that TEM remains the most precise method to characterise such precipitates. - Highlights: • Nano-sized cementite in a QT steel has been investigated by TKD and TEM. • Cementite has been indexed as distinct structures via TKD. • Crystallographic analysis returned the Bagaryatskii and Isaichev ORs. • Success of TKD is sensitive to the thickness of the electron transparent region. • TEM remains the most precise technique to characterise nano-sized precipitates.

36 MATERIALS SCIENCE↗

Synthesis and microstructure characterization of Ni-Cr-Co-Ti-V-Al high entropy alloy coating on Ti-6Al-4V substrate by laser surface alloying

Ni-Cr-Co-Ti-V-Al high-entropy alloy coating on Ti-6Al-4V was synthesized by laser surface alloying. The coating is composed of a B2 matrix and (Co, Ni)Ti{sub 2} compounds with few β-Ti phases. Focused ion beam technique was utilized to prepare TEM sample and TEM observations agree well with XRD and SEM results. The formation of HEA phases is due to high temperature and rapid cooling rate during laser surface alloying. The thermodynamic parameters, ΔH{sub mix}, ΔS{sub mix}and δ as well as Δχ, should be used to predict the formation of the BCC solid solution, but they are not the strict criteria. Especially when Δχ reaches a high value (≥ 10%), BCC HEA will be partially decomposed, leading to the formation of (Co, Ni)Ti{sub 2} compound phases. - Highlights: •Preparing HEA coating on Ti-6Al-4V by laser surface alloying is successful. •The synthesized HEA coating mainly consists of BCC HEA and (Co, Ni)Ti{sub 2} compounds. •FIB technology was used to prepare the sample for TEM analysis. • ΔH{sub mix}, ΔS{sub mix}and δ as well as Δχ, should be all used to predict the formation of solid solution.

36 MATERIALS SCIENCE↗

Effect of processing parameters on the formation of C{sub f}/LAS composites/Ag−Cu−Ti/TC4 brazed joint

C{sub f}/LAS composites were successfully jointed to TC4 alloy with Ag−Cu−Ti filler by vacuum brazing. The interfacial microstructure of TC4/C{sub f}/LAS composites joints was characterized by employing scanning electron microscope (SEM), energy dispersive spectrometer (EDS), X-diffraction (XRD) and transmission electron microscopy (TEM). The determination of the thin interfacial reaction layer (TiSi{sub 2} + TiC layer) was realized by TEM. The effect of holding time on the interfacial microstructure and shear strength were investigated. With the increasing holding time, the thickness of diffusion layer, Ti{sub 3}Cu{sub 4} layer, and TiSi{sub 2} + TiC layer increased obviously, on the contrary, that of Ti−Cu intermetallic compound layers decreased gradually. Besides, blocky Ti{sub 3}Cu{sub 4} phase was coarsened when the joint was brazed at 890 °C for 20 min, which deteriorated the mechanical properties of the joint dramatically. The interfacial evolution of TC4/C{sub f}/LAS composites joint and the formation of TiSi{sub 2}, TiC, Ti{sub 3}Cu{sub 4}, TiCu and Ti{sub 2}Cu phases were expounded. The maximum shear strength of 26.4 MPa was obtained when brazed at 890 °C for 10 min. - Highlights: •The thin interface reaction layer was determined to be TiSi{sub 2} + TiC layer by TEM. •Holding time had influence on the interfacial microstructure and joint properties. •Microstructural evolution mechanism and reactions of brazed joints were expounded.

36 MATERIALS SCIENCE↗

Optimization of SEM-EDS to determine the C–A–S–H composition in matured cement paste samples

Microanalysis of characteristic X-rays in the SEM is a powerful method to assess the chemical composition of phases in cement pastes, in particular the calcium silicate hydrate containing aluminium (C–A–S–H). Nevertheless, many variables may influence the results obtained, due mainly to the intimate mixing of C–A–S–H with other hydrate phases and the susceptibility of this phase to damage by the electron beam. In this study the effect of various acquisition parameters was examined, along with methods to determine an “average” C–A–S–H composition. The results acquired in the SEM were compared with the analysis of the same samples in the TEM, where phases can be analyzed without intermixing. A simple method was used to obtain compositions from SEM based analysis that are very close to those which can be obtained in the TEM. - Highlights: •The intermixing of phases is the limiting factor in the analysis of C–A–S–H composition by SEM-EDS •Guidelines to limit beam damage and properly analyze C–A–S–H composition by SEM-EDS are given •SEM-EDS and TEM-EDS give similar results when proper data treatment is made.

36 MATERIALS SCIENCE↗

Characterizing dislocation configurations and their evolution during creep of a new 12% Cr steel

Highlights: • Applicability of different techniques to characterize particular dislocation configuration. • XRD models in combination with TEM and EBSD to measure the dislocation density. • Substructure evolution during creep of a new 12% Cr steel is discussed. - Abstract: In this research, different types of dislocations are characterized and quantified in a newly developed 12% Cr steel in as-received as well as in crept conditions. X-ray diffraction (XRD) patterns are analyzed using three different models. The dislocation densities are determined employing the Convolution Multiple Whole Profile (CMWP) fitting, the analysis of the asymptotic part of the X-ray line profile (Groma's method), and the Rietveld refinement coupling Popa's and Williamson-Smallman approaches. CMWP method is used to measure the internal dislocation density inside the subgrains consisting of mobile and dipole dislocations, and the results show good agreement with Transmission Electron Microscopy (TEM) measurements. Groma's method is used to evaluate the total dislocation density, with results comparable to those obtained from the combination of Electron Backscatter Diffraction (EBSD) and TEM. Rietveld method gives the internal dislocation density or mobile dislocation density depending on the model chosen. The experimentally determined results such as creep strain, dislocation densities and subgrain size are compared with theoretical predictions and they are found in good agreement.

36 MATERIALS SCIENCE↗

Information depth in backscattered electron microscopy of nanoparticles within a solid matrix

Highlights: • Backscattered electron microscopy was used for reliable determination of nanoparticle density and sizes within Al alloys • Backscattered electron information depth was determined as a function of nanoparticle size from Monte Carlo simulations • Unlike transmission electron microscopy, the method is non-destructive and allows analyzing large sample areas • Good agreement with transmission electron microscopy data shows that our method is suitable for nanocomposite materials - Abstract: Measuring the dimensions and number density of nanoparticles dispersed in a solid matrix is usually accomplished via transmission electron microscopy (TEM) which suffers from high cost, low throughput, and small analytical volume. In comparison, scanning backscattered electron microscopy is inexpensive, requires little sample preparation, and allows for the analysis of large sample areas. However, the information depth is usually not known precisely and depends on several factors such as the composition of the nanoparticles and the matrix as well as the size of the nanoparticles, hindering the reconstruction of the actual size distribution and three-dimensional number density. Here we present a method to estimate the information depth for spherical nanoparticles of different sizes in order to accurately determine size distribution and number density. The approach is based on Monte Carlo simulation of electron trajectories in the material and analysis of the obtained backscattered electron signal-to-noise-ratio. Our experimental results are compared to those obtained via TEM and good agreement is demonstrated; this shows that TEM can be replaced by scanning electron microscopy for studying nanocomposites in many cases.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

The effect of finish rolling temperature and tempering on the microstructure, mechanical properties and dislocation density of direct-quenched steel

Highlights: • The effect of thermomechanical treatment and tempering on direct-quenched steel has been studied. • Dislocation density of direct-quenched and tempered martensite is evaluated using both TEM and Williamson-Hall method. • Statistical analysis has been performed to study the effect of different factors on toughness of direct-quenched martensite. - Abstract: A unique batch tempering treatment for industrial scale direct-quenched steel coils has been studied using laboratory simulations. The tempering treatment was non-isothermal with slow heating to 570 °C and slow cooling to simulate the tempering of large steel coils. The paper presents the effect of finishing rolling temperature (FRT) relative to the non-recrystallization temperature (T{sub NR}) and the effect of long time tempering on the microstructure, dislocation density and mechanical properties of direct-quenched coiled strips. Conditioning austenite below the recrystallization stop temperature resulted in a finer effective grain size distribution, which correlated strongly with the impact toughness of the final product. Furthermore low finish rolling temperature resulted in partially ferritic microstructures while higher finishing rolling temperatures led to mixtures of bainite and martensite. Dislocation densities determined with TEM and XRD showed somewhat different trends regarding the effect of tempering: intra-lath dislocation density, as measured with TEM, showed a statistically significant drop in only one case, while XRD analysis indicated a drop in all cases. Furthermore, no significant correlation between finishing rolling temperature and dislocation density existed in XRD studies. The XRD results indicate that the decrease in dislocation density corresponds to about 100 MPa lower dislocation strengthening. However, precipitation hardening and potential internal micro stress relief compensates this as yield strength remains unchanged or even increases during tempering.

36 MATERIALS SCIENCE↗

Cyclic plastic deformation behaviour of a directionally solidified nickel base superalloy at 850 °C: Damage micromechanisms

Highlights: • Isothermal LCF life of CM 247 DS is reduced using R = 0 instead of R = −1. • Reduction in LCF life is significant at lower values of Δε/2. • Reduction in fatigue life is attributed to the development of sustained mean stress. • Sustained mean stress prevents the slip transfer from γ-channels to γ′-precipitates. • Sustained mean stress promotes dislocation network formation and looping. - Abstract: Dislocation based deformation micromechanisms during low cycle fatigue deformation of nickel base superalloy CM 247 DS LC at 850 °C was investigated by conducting fatigue tests employing constant strain amplitudes for strain ratio (R) values of 0, −1 and carrying out extensive SEM and TEM examinations. Cyclic life of the alloy reduces for all fatigue tests conducted employing R = 0 in comparison with R = −1 owing to sustained mean stress developed during fatigue at R = 0. TEM examinations confirmed that sustained mean stress developed during low strain amplitude fatigue test (Δε/2 = 0.5%) using R = 0 condition prevented slip transfer from γ-channels to γ′-precipitates and resulted in the formation of dislocation substructures such as networks, nodes etc. and also promoted dislocation looping around γ′-precipitates. Lower fatigue life at R = 0 is mainly attributed to the development of these types of substructures, which promotes strain localization in both intra as well intergranular regions. Whereas, in specimen fatigue tested (Δε/2 = 0.5%) using R = −1 condition, shearing of γ′-precipitates by APB coupled dislocation and formation of stacking faults were observed. The formation and nature of stacking faults were analysed using weak beam imaging technique. Stacking fault formed during fatigue tests using R = −1 condition matured to micro-twins when Δε/2 value was increased to 0.8%. The mechanism of formation of these microtwins is discussed in detail. SEM based microstructural and fractographic examinations revealed that mean stress induced creep effect resulted in intergranular crack initiation and grain boundary cavitation during fatigue tests under R = 0 condition and therefore verified the facts revealed in TEM studies.

36 MATERIALS SCIENCE↗

High resolution microstructural, chemical studies and localized burnup analysis in an irradiated U–10Zr metallic fuel

This study involves high resolution characterization of a sodium bonded solid uranium (U)-10 wt% zirconium (Zr) metallic fuel irradiated in Fast Flux Test Facility (FFTF). The fuel centerline temperature during irradiation was estimated to be around 675 °C with the peak burnup 13.1 atomic percent. Samples for transmission electron microscopy (TEM) and atom probe tomography (APT) were prepared from different regions/zones in the fuel cross section radially to elucidate the microstructural changes and chemical redistribution of solute elements as well as fission products during irradiation experiment. TEM results indicate the irradiation in fast flux testing leads to the formation of extensive Zr-rich precipitates with varying sizes in the U–Zr fuel matrix. APT analysis performed to investigate redistribution of Zr, U and fission products along the radial direction of fuel pin showed Zr-rich precipitates entrapping the fission products in higher concentration as compared to the α-U phases. Here, the local burnup ( 235 U depletion) is found to be consistent, calculated by quantification of 235 U, 236 U and 238 U isotopes from mass spectrum obtained from APT along the radial direction. Zr-rich precipitation and its implication on fuel constitutional redistribution are discussed based on SEM, TEM and APT results.

APT↗

Preparation, characterization, and photocatalytic studies on anatase nano-TiO{sub 2} at internal air lift circulating photocatalytic reactor

Graphical abstract: The micro morphological structure of the nano-TiO{sub 2} particles was also observed with TEM, as shown in figure. The TEM images clearly exhibited the homogeneous microstructure of particles with a size of around 10–15 nm. - Highlights: • Nano-TiO{sub 2} was prepared by complex techniques of sol–gel, micro-emulsion and solvent thermal. • The size of TiO{sub 2} was nano level and uniformity. • Nano-TiO{sub 2} exhibited high photo-catalytic activity at internal air lift circulating reactor. • The best nano-TiO{sub 2} dosage was obtained. - Abstract: Anatase nano-titania (TiO{sub 2}) powder was prepared by using a sol–gel process mediated in reverse microemulsion combined with a solvent thermal technique. The structures of the obtained TiO{sub 2} were characterized by TG-DSC, XRD, TEM. The photocatalytic decomposition of methylene blue (MB) on nano-TiO{sub 2} was studied by using an internal air lift circulating photocatalytic reactor. The results show that the anatase structure appears in the calcination temperature range of 400–510 °C, while the transformation of anatase into rutile takes place above 510 °C. The homogeneous microstructure of nano-TiO{sub 2} particles was obtained with a size of around 10–15 nm. In the photocatalytic performance, degradation process follows pseudo first order kinetics with different dosages of photocatalyst and initial MB concentrations and optimal TiO{sub 2} dosage is 0.1 g/L with neutral medium.

36 MATERIALS SCIENCE↗

Synthesis and structure of high-quality films of copper polyphthalocyanine – 2D conductive polymer

Graphical abstract: - Highlights: • 2D polymers show a big promise for science and technology. • We develop a new procedure for the direct synthesis of copper polyphthalocyanine. • We obtain reliable experimental data on the CuPPC structure. • With the support of quantum chemical calculations we describe electronic structure of CuPPC. - Abstract: Copper polyphthalocyanine (CuPPC), a 2D conjugated polymer, is a promising material for electronics and photovoltaics, but its applications were hindered by a poor processability. We propose an experimental approach, by which thin films of CuPPC, can be directly synthesized in a chemical vapor deposition (CVD) set-up at mild temperature (420 °C). High polymerization degree and high crystallinity of the films were confirmed by TEM, FTIR and UV–vis studies. From XRD and TEM electron diffraction, we conclude that the polymer has AA layer stacking with the inter-layer distance of 0.32 nm. The assignment of X-ray and TEM diffraction patterns was based on quantum-chemical calculations. Based on the latter, we also discuss electronic structure and conclude that CuPPC is rather a semi-metal than semi-conductor.

36 MATERIALS SCIENCE↗

Characterization, antioxidant and cytotoxicity evaluation of green synthesized silver nanoparticles using Cleistanthus collinus extract as surface modifier

Graphical abstract: The figure is the TEM image of green synthesized silver nanoparticles from Cleistanthus collinus. In this investigation we have used the poisonous plant as a reducing and capping agent. This is a first time data to synthesis the metal nanoparticles using poisonous plant. - Highlights: • A hitherto unreported venomous plant mediated AgNPs synthesis. • The particle size is observed in the range of 20–40 nm. • Surface morphology of the well-dispersed silver nanoparticles is studied using SEM and TEM. • Crystalline nature of AgNPs is confirmed by X-ray diffraction analysis. • Antioxidant activities of green synthesized AgNPs are tested in vitro. - Abstract: We report, here a simple green method for the preparation of silver nanoparticles (AgNPs) using the plant extract of Cleistanthus collinus as potential phyto reducer. The synthesized AgNPs were characterized by UV–vis spectra, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The obtained results confirmed that the AgNPs were crystalline in nature and the morphological studies reveal the spherical shape of AgNPs with size ranging from 20 to 40 nm. The in vitro antioxidant activity of AgNPs showed a significant effect on scavenging of free radicals. The cytotoxicity study exhibited a dose-dependent effect against human lung cancer cells (A549) and normal cells (HBL-100), the inhibitory concentration (IC{sub 50}) were found to be 30 μg/mL and 60 μg/mL respectively. The in vivo histopathology of mouse organs proved that AgNPs does not possess toxic effect and can be extensively applied in biomedical sciences.

36 MATERIALS SCIENCE↗

Electronic structure, magnetic and structural properties of Ni doped ZnO nanoparticles

Highlights: • XRD, and HR-TEM results show the single phase nature of Ni doped ZnO nanoparticles. • dc magnetization results indicate the RT-FM in Ni doped ZnO nanoparticles. • Ni L{sub 3,2} edge NEXAFS spectra infer that Ni ions are in +2 valence state. • O K edge NEXAFS spectra show that O vacancy increases with Ni doping in ZnO. - Abstract: We report structural, magnetic and electronic structural properties of Ni doped ZnO nanoparticles prepared by auto-combustion method. The prepared nanoparticles were characterized by using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, and dc magnetization measurements. The XRD and HR-TEM results indicate that Ni doped ZnO nanoparticles have single phase nature with wurtzite lattice and exclude the presence of secondary phase. NEXAFS measurements performed at Ni L{sub 3,2}-edges indicates that Ni ions are in +2 valence state and exclude the presence of Ni metal clusters. O K-edge NEXAFS spectra indicate an increase in oxygen vacancies with Ni-doping, while Zn L{sub 3,2}-edge show the absence of Zn-vacancies. The magnetization measurements performed at room temperature shows that pure and Ni doped ZnO exhibits ferromagnetic behavior.

36 MATERIALS SCIENCE↗

Green synthesis and characterization of graphene nanosheets

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.

36 MATERIALS SCIENCE↗

Structure and properties of Pb(Lu{sub 1/2}Nb{sub 1/2})O{sub 3}–0.2PbTiO{sub 3} relaxor ferroelectric crystal

Graphical abstract: The relaxor state of the crystal was demonstrated by the dielectric behavior. - Highlights: • PLN–0.2PT ferroelectric crystal was obtained by the TSSG technique. • The super-lattice reflections were identified by XRD and TEM results. • The PLN–0.2PT crystal is a typical relaxor ferroelectric. - Abstract: Ferroelectric crystal Pb(Lu{sub 1/2}Nb{sub 1/2})O{sub 3}–0.2PbTiO{sub 3} (PLN–0.2PT) was successfully obtained by a top-seed solution growth technique. At room temperature the symmetry was orthorhomic according to X-ray diffraction (XRD). The super-lattice reflections were identified by XRD and transmission electron microscope (TEM). The micro-domain structure was detected by TEM. The temperature dependence of the dielectric constant (ϵ′) shows a typical relaxor behavior. The temperature dependence of coercive electric field and remnant polarizations were investigated, which also shows the relaxor feature.

36 MATERIALS SCIENCE↗