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At least 1,387 records · Page 77

Electron microscopy study of the microstructure of Ni–W substrate surface

The surface microstructure of Ni–W alloy tapes, which are used as substrates to form films of high-temperature superconductors and photovoltaic devices, has been studied. Several samples of a Ni{sub 95}W{sub 5} tape (Evico) annealed under different conditions were analyzed using scanning electron microscopy, energy-dispersive X-ray microanalysis, electron diffraction, and electron energy-loss spectroscopy. NiWO{sub 4} precipitates are found on the surface of annealed samples. The growth of precipitates at a temperature of 950°C is accompanied by the formation of pores on the surface or under an oxide film. Depressions with a wedge-shaped profile are found at the grain boundaries. Annealing in a reducing atmosphere using a specially prepared chamber allows one to form a surface free of nickel tungstate precipitates.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

An investigation of wear behaviors of different Monel alloys produced by powder metallurgy

In the present study, wear behaviors of Monel 400, Monel 404, Monel R-405 and Monel K-500 alloys produced by Powder Metallurgy (P/M) method were investigated. These compounds prepared from elemental powders were cold-pressed (600 MPa) and then, sintered at 1150°C for 2 hours and cooled down to the room temperature in furnace environment. Monel alloys produced by the P/M method were characterized through scanning electron microscope (SEM+EDS), X-ray diffraction (XRD), hardness and density measurements. In wear tests, standard pin-on-disk type device was used. Specimens produced within four different Monel Alloys were tested under 1ms{sup −1} sliding speed, under three different loads (20N, 30N and 40N) and five different sliding distances (400-2000 m). The results show that Monel Alloys have γ matrix and that Al{sub 0,9}Ni{sub 4,22} intermetallic phase was formed in the structure. Also, the highest hardness value was measured with the Monel K-500 alloy. In wear tests, the maximum weight loss according to the sliding distance, was observed in Monel 400 and Monel 404 alloys while the minimum weight loss was achieved by the Monel K-500 alloy.

36 MATERIALS SCIENCE↗

Neutron absorption of Al-Si-Mg-B{sub 4}C composite

Al-Si-Mg-B{sub 4}C composites containing 2-8 wt% of B{sub 4}C were prepared by stir casting technique. Homogenization treatment was carried out at temperatures of 540°C for 4 houra and followed by ageing at 180°C for 2 houra. Microstructure and phase identification were studied by scanning electron microscopy (SEM) and X-ray diffraction (XRD) respectively. Neutron absorption study was investigated using neutron source Am/Be{sup 241}. The result indicated that higher B{sub 4}C content improved the neutron absorption property. Meanwhile homogeneity of the composite was increased by ageing processes. This composite is potential to be used as neutron shielding material especially for nuclear reactor application.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Evolution of the substructure of a novel 12% Cr steel under creep conditions

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used to the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.

36 MATERIALS SCIENCE↗

Polyethylene glycol (PEG) assisted size-controlled SnO{sub 2} nanoparticles by sol-gel process

Tetragonal phase tin oxide (SnO{sub 2}) nanoparticles have been synthesized by sol–gel method using SnCl{sub 4}.5H{sub 2}O and polyethylene glycol (PEG) of different concentration. The phase, size and purity of the final products are characterized by X-ray diffraction (XRD). The morphology is confirmed by scanning electron microscopy (SEM) analysis. There exists relationship between the concentration of PEG and particle size of SnO{sub 2} nanoparticles. Increase in concentration of PEG caused the reduction of particle size of tin oxide nanoparticles. The results suggest that the concentration of PEG plays a significant role in determining the size of SnO{sub 2} nanoparticles synthesized via this method. The optical property of the product has been explored by Ultraviolet (UV-visible) and Fourier Transform Infrared (FTIR) spectroscopic techniques.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

A mild calcium carbonate treatment improves moisture resistance and mechanical/interfacial properties of jute and hemp fibers

Natural fibers are attractive, sustainable reinforcements, but often exhibit high moisture uptake and weak bonding with polymer matrices. In this study, jute and hemp were treated by immersion in aqueous calcium carbonate (CaCO3) suspensions (10–40?wt.%, 1.5?h, room temperature) and were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), moisture sorption testing, single-fiber tensile testing, and bundle pull-out testing. SEM showed granular CaCO3 deposition on fiber surfaces, with particulates bridging surface voids and microcracks. At 40 wt.% CaCO3, equilibrium moisture uptake decreased to ~5% (hemp) and ~3% (jute), while tensile strength increased to ~904 MPa (hemp) and ~960 MPa (jute). Apparent interfacial shear strength from pull-out testing increased up to ~1.35 MPa (hemp) and ~0.56 MPa (jute). These results indicate that CaCO3 deposition is a mild, scalable surface treatment that improves moisture resistance, fiber tensile strength, and interfacial load transfer relevant to semi-structural composite applications, including interior and secondary automotive components.

Calcium carbonate treatment↗

Hydrothermal synthesis of highly crystalline ZnO nanorod arrays: Dependence of morphology and alignment on growth conditions

Highly oriented zinc oxide nanorod were successfully grown on seeded p-type silicon substrate by hydrothermal methode. The morphology and the crystallinty of ZnO c-axis (002) arrays were systematically studied using field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD) methods. The effect of seed layer pre-annealing on nanorods properties was explained according to the nucleation site of ZnO nanoparticles on silicon substrate. In addition, the variation of the equal molarity of zinc nitrate hexahydrate and hexamine concentrations in the reaction vessel play a crucial role related to the ZnO nanorods.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Slags as Evidence for Copper Mining above Casaccia, Val Bregaglia (Central Alps)

Slags from the remote Mota Farun locality above Casaccia (Val Bregaglia, Swiss Alps) have been analyzed with scanning electron microscopy, X-ray powder diffraction and microfocus synchrotron X-ray diffraction to determine mineralogical composition and microstructures. Non-magnetic slag samples are largely composed of euhedral and dendritic iron-rich olivine in a glassy matrix. Locally there are zones with globular inclusions rich in bornite ((Cu5Fe)S4) and locally metallic copper. Some regions display dendritic pentlandite ((Fe,Ni)9S8). Magnetic samples are mainly composed of fayalite (Fe2SiO4) and wüstite (FeO), with minor magnetite (Fe3O4). The mineralogical composition indicates that slags were the product of copper smelting. The slag compositions and morphologies are analogous to slags described from the Oberhalbstein (Graubünden, Switzerland) and the Trentino Alps (Italy) which are attributed to metallurgical exploitations of the Late Bronze Age. While the origin of the ore could not be determined, it may be related to ore deposits of chalcopyrite in greenschists and serpentinites in the vicinity, such as Alp Tgavretga (Septimer Pass) and Val Perossa (Val Bregaglia).

58 GEOSCIENCES↗

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↗

Preparation and characterisation of nanoscale α-Al{sub 2}O{sub 3} by precipitation method

Nanometer-scale α-Al{sub 2}O{sub 3} particles have been synthesized by a simple precipitation method from an aqueous solution in the presence of AlCl{sub 3} and NH{sub 3}. The surface morphology and composition of the as-synthesized Al{sub 2}O{sub 3} nanoparticle were characterized by means of scanning electron microscopy (SEM) and X-ray diffraction (XRD). The powder was nanocrystalline in nature having hexagonal structure with unit cell parameters: a=4.76A°, c=12.99A°. The Al{sub 2}O{sub 3} nanocrystallites with an average crystal size of about 86 nm. The powder has been characterized by means of FT-IR, and UV-Vis Study. From these results it is possible to conclude that the precipitation method is a very suitable technique to prepare α-Al{sub 2}O{sub 3} materials. The technique is fast, low cost and produces well defined materials that can be used for dosimetric applications.

36 MATERIALS SCIENCE↗

Fabrication of hierarchical meso/macroporous TiO2 scaffolds by evaporation-induced self-assembly technique for bone tissue engineering applications

Highlights: • Hierarchical meso/macroporous TiO{sub 2} scaffolds were produced. • TiO{sub 2} formation mechanism was investigated. • The scaffolds had a pore size of 150–300 μm and meso pores of 6–12 nm. • The specific surface area obtained from BET theory was 67.89 m{sup 3} g{sup −1}. - Abstract: This paper reports the synthesis of hierarchical meso/macroporous TiO{sub 2} scaffolds by mimicking bone structure. Evaporation-induced self-assembly (EISA) method along with foamy method was utilized to produce TiO{sub 2} scaffolds in situ. Simultaneous thermal analysis (STA), small angle X-ray diffraction (SAXD), wide-angle X-ray diffraction (WAXD), nitrogen adsorption–desorption isotherm analysis, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques were applied to characterize the scaffolds. The results showed that TiO{sub 2} scaffolds can be produced after sintering the specimens at 550 °C for 2 h. The obtained scaffolds had a pore size in the range of 150–300 μm and meso pores in the range of 6–12 nm. The specific surface area was obtained from the Brunauer–Emmett–Teller theory, the total volume and mean diameter of pores were 67.89 m{sup 3} g{sup −1}, 0.1245 cm{sup 3} g{sup −1} and 7.3 nm, respectively.

36 MATERIALS SCIENCE↗

Synthesis and characterization of α-MoO{sub 3} nanobelt composite positive electrode materials for lithium battery application

Graphical abstract: (a) TEM image of MoO{sub 3}/PEO nanobelts composite, (b) CV curves of MoO{sub 3}/PEO nanobelts composite. - Highlights: • α-MoO{sub 3} and PEO surfactant MoO{sub 3} nanobelts were synthesized by solvothermal method. • The capacity retention of 12.5 wt% PEO surfactant MoO{sub 3} nanobelts is 88.78%. • The specific capacity of 12.5 wt% PEO surfactant MoO{sub 3} nanobelts is 352 mAh g{sup −1}. • MoO{sub 3}/PEO nanobelts composite material demonstrates good cycling stability as cathode. - Abstract: α-MoO{sub 3} and PEO surfactant MoO{sub 3} nanobelts were synthesized by a solvothermal method. The morphology and nanostructure of samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Bare α-MoO{sub 3} and 12.5 wt% PEO surfactant MoO{sub 3} nanobelts have an initial specific capacities of 279 and 352 mAh g{sup −1}, respectively, at constant current density 30 mA g{sup −1} with potential range of 1.5–4.0 V vs. Li/Li{sup +}. While MoO{sub 3} is modified by the intercalation of PEO, it is effectively shielded against electrostatic interaction between the MoO{sub 3} interlayer and Li{sup +} ions. We reported positive material, a nanocomposite of MoO{sub 3} coated with polyethylene oxide. It presents good cycling stability due to existence of the conductive and protective polyethylene oxide coating and the nanobelt morphology of MoO{sub 3}. The polyethylene oxide acts as a conducting matrix, a binder and an active material, as well as a volume change buffer agent, which holds the MoO{sub 3} particles in place during the discharge cycles. The cyclic voltammograms of the 12.5 wt% PEO surfactant MoO{sub 3} nanobelt composite displayed better cyclic performance compared with pure MoO{sub 3} nanobelts. The specific capacity of the pure MoO{sub 3} nanobelts and 12.5 wt% PEO surfactant MoO{sub 3} nanobelts exhibit as 199 mAh g{sup −1} and 225 mAh g{sup −1}, respectively, after 9 cycles, suggesting that the stability of surfactant material is worthy.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Giant dielectric response at low frequency of B-site modified Aurivillius oxide potassium bismuth titanate

Highlights: • K{sub 0.5}Bi{sub 4.5}Ti{sub 4-x}(Al{sub 0.5}V{sub 0.5}){sub x}O{sub 12} ceramics were synthesized by the conventional solid-state reaction method. • Giant dielectric response at low frequency were observed in the KBT-AlV ceramics. • A giant dielectric constant (5.4 × 10{sup 4} at 100 Hz) was obtained in the KBT-AlV specimens. - Abstract: K{sub 0.5}Bi{sub 4.5}Ti{sub 4-x}(Al{sub 0.5}V{sub 0.5}){sub x}O{sub 15} (KBT-AlV, x = 0.00, 0.04, 0.06 and 0.08) ceramics were prepared by using the conventional solid-state reaction method. Phase analysis was performed by X-ray diffraction, and micro-structural morphology was assessed by scanning electron microscopy. The Effect of aluminium and vanadium on the structures, morphologies and electric properties of the K{sub 0.5}Bi{sub 4.5}Ti{sub 4}O{sub 12} (KBT) ceramics were investigated. Frequency dependence of the dielectric constant exhibited that the dielectric constant of the KBT ceramic is enhanced gradually by the aluminium and vanadium modification and a giant dielectric constant (5.4 × 10{sup 4} at 100 Hz) can be observed in the KBT-AlV specimens. Moreover, the reasons for the giant dielectric constant of the KBT-AlV ceramics are discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Preparation and characterization of nanocomposite polymer electrolytes poly(vinylidone fluoride)/nanoclay

Polymer electrolytes are defined as semi solid electrolytes used as separator in lithium ion battery. Separator used as medium for transfer ions and to prevent electrical short circuits in battery cells. To obtain the optimal battery performance, separator with high porosity and electrolyte uptake is required. This can reduce the resistance in the transfer of ions between cathode and anode. The main objective of this work is to investigate the impact of different solvent (Dimethyl acetamide (DMAc), N-methyl-2-pyrrolidone (NMP) and dimethyl formamide (DMF)), pore forming agent poly(vinylpyrolidone) (PVP) and nanoclay as filler in addition of membrane using phase inversion method on the morphology, porosity, electrolyte uptake and degree of crystallinity. The membrane was prepared by the phase inversion method by adding PVP and Nanoclay using different solvents. The phase inversion method was prepared by dissolving Nanoclay and PVP in solvent for 1-2 hours, and then add the PVDF with stirring for 4 hours at 60°C. The membranes were characterized by porosity test, electrolyte uptake test, scanning electron microscope (SEM), and X-ray diffraction (XRD). The results showed that DMAc as solvent gives the highest value of porosity and electrolyte uptake. The addition of nanoclay and PVP enlarge the size of the pores and reduce the degree of crystallinity. So, the usage of DMAc as solvent is better than NMP or DMF.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Cryogenic Treatment of CoCrFeMnNi(NbC) High-Entropy Alloys

The effect of cryogenic treatment on the microstructure and mechanical properties of CoCrFeMnNi and CoCrFeMnNi(NbC) high-entropy alloys was investigated during annealing. The heat-treated samples were characterized by optical microscopy, scanning electron microscopy–wavelength-dispersive x-ray spectroscopy, x-ray diffraction technique, differential scanning calorimetry, Vickers hardness testing and tensile testing. The results showed a single-phase FCC crystal structure matrix in both alloys during cryogenic treatment and annealing. Cryogenic treatment altered the recrystallization behavior of CoCrFeMnNi high-entropy alloy, while it did not influence the recrystallization of CoCrFeMnNi(NbC) high-entropy alloy. It was also found that cryogenic treatment changed the precipitation behavior of CoCrFeMnNi(NbC) high-entropy alloy during annealing. In both studied high-entropy alloys, the mechanical testing indicated that the cryogenic treatment can effectively reduce the yield strength of cold-rolled samples after annealing. This was primarily attributed to the effect of cryogenic treatment in enhancing crystalline defects annihilation. Furthermore, the cryogenic treatment increased the ultimate tensile strength of CoCrFeMnNi(NbC). A lager plastic deformation and precipitates were considered as the main reasons for the higher ultimate tensile strength.

36 MATERIALS SCIENCE↗

Improving Corrosion Resistance of 316L Austenitic Stainless Steel Using ZrO{sub 2} Sol-Gel Coating in Nitric Acid Solution

In this study, thin-film coating of zirconium oxide (ZrO{sub 2}) was prepared by sol-gel method and subsequent heat treatment process. The sol was prepared by controlled hydrolysis of zirconium tetrapropoxide using acetic acid and ethanol/acetylacetone mixture as catalyst and chelating agent, respectively, and finally deposited onto the 316L austenitic stainless steel (316L SS) using dip coating method in order to improve its corrosion resistance in nitric acid medium. The composition, structure, and morphology of the coated surface were investigated by x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The obtained results from XRD and FTIR state the formation of tetragonal and monoclinic ZrO{sub 2} phase. Also, the obtained results from surface morphology investigation by SEM and AFM indicate the formation of smooth, homogeneous and uniform coatings on the steel substrate. Then, the corrosion behavior of stainless steel was investigated in a 1 and 10 M nitric acid solutions using electrochemical impedance spectroscopy and linear polarization test. The obtained results from these tests for ZrO{sub 2}-coated specimens indicated a considerable improvement in the corrosion resistance of 316L stainless steel by an increase in corrosion potential and transpassive potential, and a decrease in passive current density and corrosion current density. The decrease in passive current density in both the concentration of solutions was two orders of magnitude from bare to coated specimens.

36 MATERIALS SCIENCE↗

Influence of Sodium Silicate/Sodium Alginate Additives on Discharge Performance of Mg–Air Battery Based on AZ61 Alloy

The application of Mg–air batteries is limited due to passivation and self-corrosion of anode alloys in electrolyte. In effort of solving this problem, the present work studied the influence of sodium silicate (SS)/sodium alginate (SA) on electrochemical behaviors of AZ61 alloy in NaCl solution by circle potentiodynamic polarization and galvanostatic discharge. The corrosion morphology and discharge product were examined by scanning electron microscopy (SEM) and x-ray diffraction (XRD). Results have shown that sodium silicate/sodium alginate inhibitors have an apparent effect on the self-corrosion of AZ61 alloy without affecting its discharge performance. The discharge capacity and the anodic utilization for Mg–air battery in a 0.6 M NaCl + 0.01 M SS +0.04 M SA solution are measured to be 1397 mAhg{sup −1} and 48.2%, respectively. Electrochemical impedance spectroscopy (EIS) and SEM investigation have confirmed that the sodium silicate/sodium alginate inhibitor can obviously decrease the self-corrosion of AZ61 alloy. SEM and XRD diffraction examinations suggest that the inhibiting mechanism is due to the formation of a compact and “cracked mud” layer. AZ61 alloy can be used as the anode for Mg–air battery in a solution of 0.6 M NaCl + 0.01 M SS +0.04 M SA.

36 MATERIALS SCIENCE↗

The synthesis and characterization of Mg-Zn-Ca alloy by powder metallurgy process

Known for its biodegradation and biocompatible properties, magnesium alloys have gained many interests to be researched as implant material. In this study, Mg-3Zn-1Ca, Mg-29Zn-1Ca, and Mg-53Zn-4.3Ca (in wt%) were synthesized by means of powder metallurgy method. The compression strength and corrosion resistance of magnesium alloy were thoroughly examined. The microstructures of the alloy were characterized using optical microscopy, Scanning Electron Microscope, and also X-ray diffraction analysis. The corrosion resistance were evaluated using electrochemical analysis. The result indicated that Mg- Zn- Ca alloy could be synthesized using powder metallurgy method. This study showed that Mg-29Zn-1Ca would make the highest mechanical strength up to 159.81 MPa. Strengthening mechanism can be explained by precipitation hardening and grain refinement mechanism. Phase analysis had shown the formation of α Mg, MgO, and intermetallic phases: Mg2Zn11 and also Ca2Mg6Zn3. However, when the composition of Zn reach 53% weight, the mechanical strength will be decreasing. In addition, all of Mg-Zn-Ca alloy studied here had better corrosion resistance (Ecorr around -1.4 VSCE) than previous study of Mg. This study indicated that Mg- 29Zn- 1Ca alloy can be further analyzed to be a biodegradable implant material.

36 MATERIALS SCIENCE↗