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At least 1,315 records · Page 73

Formation and properties of biocoatings based on wollastonite and calcium phosphates

Wollastonite-calcium phosphate coatings were produced on titanium substrates by micro-arc oxidation method. There presented the study of influence of oxidation voltage, process duration and pulse duration on properties of the coatings such as thickness, surface morphology and surface roughness. The morphology and phase composition of the coatings were studied by scanning electron microscopy and X-ray diffraction methods. It was found that biocoatings with large amount of wollastonite particles were deposited under minimum oxidation voltage of 130–150 V. The structural elements with a spherical or plate-like shape were formed on the coating surface depending on micro-arc oxidation parameters.

36 MATERIALS SCIENCE↗

High-Temperature Oxidation of Stellite 12 Hardfacings: Effect of Mo on Characteristics of Oxide Scale

This study aims to understand the oxide scale formation on the surfaces of commercial and Mo (10 wt.%)-modified Stellite 12 hardfacings deposited on 4140 steel. For this purpose, samples of the hardfacings were isothermally oxidized in air at various temperatures in between 500 and 900 °C for 30 h. As a result of changes in the microstructure upon Mo addition, about 50% higher mass gain at all oxidation temperatures was observed. The characteristics of the developed oxide scales were examined by utilizing Raman spectroscopy, scanning electron microscopy and x-ray diffraction analysis. The oxide scale formed over Stellite 12 consisted of CoO-, Co{sub 3}O{sub 4-} and Cr{sub 2}O{sub 3}-type oxides, while additionally CoMoO{sub 4}-type complex oxide was detected on Mo-modified hardfacing, more likely at the alloy–scale interface. On the basis of findings of isothermal oxidation tests, the formation mechanisms of this complex oxide imposing better wear resistance as reported in our previous studies were explained during high-temperature wear testing, i.e., dynamic oxidation conditions.

36 MATERIALS SCIENCE↗

Effect of Welding Parameters on the Corrosion Behavior of Dissimilar Alloy Welds of T6 AA6061 Al-Galvanized Mild Steel

Partial replacement of steel by Aluminium (Al) alloys is a promising approach adopted by automotive sector to improve fuel efficiency without compromising on the strength. However, this results in the generation of dissimilar welds of Al alloys and steel. Understanding the corrosion behavior of Al alloys–steel welds as a function of welding parameters is critical in the successful application of such alloys. The present study reports the intergranular corrosion behavior of T6 heat-treated AA6061 Al alloy-galvanized mild steel lap joints, welded by metal inert gas welding–brazing technique as a function of different welding parameters, viz. weld speed (4-6 m/min) and wire feed rate (0.8-0.9 m/min), following ASTM G 67-04. Weld characterization was performed by field emission scanning electron microscopy (FESEM), x-ray diffraction and nano-hardness measurement. Results indicate heavy dissolution and metal loss at the interface. A high volume fraction of Al-Fe intermetallics was precipitated at the weld interfaces, resulting in high hardness and higher localized corrosion. The thickness of Al-Fe intermetallic layer increased with increasing wire feed rate and lower weld speed which enhanced the severity of galvanic and intergranular corrosion.

36 MATERIALS SCIENCE↗

Texture Evolution and Its Effect on Fatigue Crack Propagation in Two 2000 Series Alloys

The texture evolution and fatigue crack propagation (FCP) of 2000 series alloys were investigated, respectively, by using scanning electron microscopy and x-ray diffraction. Results showed that the intensity change in different textures (such as Goss, Copper, S and Brass) abides by a linear evolution law, and a new model for texture evolution is proposed to predict the texture intensity during different heat treatments. With increasing annealing temperature, the FCP rate increased, but the damage tolerance decreased. The intensity of P texture was the key to affecting FCP rate and damage tolerance of the alloys. A new model based on the average grain diameter and P texture volume fraction was proposed to predict FCP rate and damage tolerance, and the predicted FCP rates agree very well with the experimental FCP rates of the alloys after different T83 treatments.

36 MATERIALS SCIENCE↗

Texture formation in iron particles using mechanical milling with graphite as a milling aid

Crystallographically anisotropic platelet iron particles were successfully prepared using a conventional ball mill with addition of graphite (Gp) particles. The morphological and structural changes resulting from the milling were investigated using scanning electron microscopy and X-ray diffraction. The spherical iron particles were plastically deformed into platelet shapes during the milling. Simultaneously, it is suggested that the size of the Gp particles decreased and adhered as nanoparticles on the surface of the iron particles. The adhered Gp particles affected the plastic deformation behavior of the iron particles: the (001) planes of α-iron were oriented parallel to the particle face, and no preferred in-plane orientation was observed. This study not only details the preparation of soft magnetic metal particles that crystallographically oriented to enhance their magnetic properties but also provides new insight into the activities of the well-established and extensively studied mechanical milling method.

36 MATERIALS SCIENCE↗

Comparative Study of the Effect of Magnetic Nanoparticle CoFe{sub 2}O{sub 4} on Fluctuation-Induced Conductivity of Y-123 and Y-358 Superconductors

In this study, a comparative investigation of the electrical conductivity fluctuations in nano-CoFe{sub 2}O{sub 4} added to Y{sub 3}Ba{sub 5}Cu{sub 8}O{sub 18±x} (Y-358) and YBa{sub 2}Cu{sub 3}O{sub 7−d} (Y-123) products is performed. All products were made using the solid-state reaction process. X-ray powder diffraction (XRD) analyses confirmed the formation of different phases. Scanning electron microscope (SEM) analysis shows the reduction of grain size with increasing the quantity of nano-CoFe{sub 2}O{sub 4} particles for both the Y-123 and Y-358 samples. The decrease of grain size is more accentuated in the case of the Y-358 samples compared with the Y-123 ones. The data of conductivity fluctuations are examined in terms of the derivative of the electrical resistivity with respect to temperature and the logarithmic derivative of the conductivity with regard to temperature. The results illustrate the existence of a transition with two stages; intragrain and intergrain. It is demonstrated that the addition of CoFe{sub 2}O{sub 4} nanoparticles affects the electrical conductivity fluctuations, the values of the critical exponents, and the fluctuation dimensionality in YBCO systems.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Interface characteristics of Ti6Al4V-TiAl metal-intermetallic laminate (MIL) composites prepared by a novel hot-pack rolling

Highlights: • The Ti6Al4V/high Nb-TiAl metal-intermetallic (MIL) composite was fabricated. • The formation of γ and α{sub 2} phase at interface is diffusion controlled. • The formation of O phase at interface is due to the segregation of Nb atoms. • The Vickers hardness from Ti6Al4V to TiAl alloy shows a trend of a decrease then an increase and finally a decrease. - Abstract: Ti6Al4V (wt%)/Ti-44Al-8Nb-0.2W-0.2B-0.03Y (at.%) (high Nb-TiAl) metal–intermetallic laminate (MIL) composite with a defect-free interface was successfully prepared by hot-pack rolling and the interface microstructure was characterized by XRD, SEM, EBSD, and TEM techniques. The results showed that the interface was about 260 μm thick and consisted of four different microstructure regions. The thickness of each region was about 60–80 μm and the microstructure of the four regions consisted of acicular O, α{sub 2}, and β/B2 phases; acicular α{sub 2} phase; acicular α{sub 2} and β/B2 phases; and acicular γ, α{sub 2}, and β/B2 phases respectively. The resulting microstructure of the interface region was attributed to the interdiffusion of Ti atoms from the starting Ti6Al4V alloy layer to the high Nb-TiAl alloy layer and Al and Nb atoms from the high Nb-TiAl alloy layer to the Ti6Al4V alloy layer. The formation of acicular α{sub 2} and γ phases was diffusion-controlled and the Nb segregation at the interface caused the formation of O phase which had specific relationships with α{sub 2} and β/B2 phases. The detailed interface microstructural evolution of the Ti6Al4V/high Nb-TiAl MIL composite and the Vickers hardness of the composite are also discussed in this paper.

36 MATERIALS SCIENCE↗

Microwave exfoliated graphene oxide/TiO{sub 2} nanowire hybrid for high performance lithium ion battery

Lithium ion battery (LIB) is a key solution to the demand of ever-improving, high energy density, clean-alternative energy systems. In LIB, graphite is the most commonly used anode material; however, lithium-ion intercalation in graphite is limited, hindering the battery charge rate and capacity. To date, one of the approaches in LIB performance improvement is by using porous carbon (PC) to replace graphite as anode material. PC's pore structure facilitates ion transport and has been proven to be an excellent anode material candidate in high power density LIBs. In addition, to overcome the limited lithium-ion intercalation obstacle, nanostructured anode assembly has been extensively studied to increase the lithium-ion diffusion rate. Among these approaches, high specific surface area metal oxide nanowires connecting nanostructured carbon materials accumulation have shown promising results for enhanced lithium-ion intercalation. Herein, we demonstrate a hydrothermal approach of growing TiO{sub 2} nanowires (TON) on microwave exfoliated graphene oxide (MEGO) to further improve LIB performance over PC. This MEGO-TON hybrid not only uses the high surface area of MEGO but also increases the specific surface area for electrode–electrolyte interaction. Therefore, this new nanowire/MEGO hybrid anode material enhances both the specific capacity and charge–discharge rate. Scanning electron microscopy and X-ray diffraction were used for materials characterization. Battery analyzer was used for measuring the electrical performance of the battery. The testing results have shown that MEGO-TON hybrid provides up to 80% increment of specific capacity compared to PC anode.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Extraction of Microcrystalline Cellulose from Cotton Sliver and Its Comparison with Commercial Microcrystalline Cellulose

The work was aimed at the extraction of microcrystalline cellulose (EMC) from raw cotton sliver (RCS) by acid hydrolysis using sulphuric acid. The EMC was characterized and compared with commercial grade microcrystalline cellulose (CMC). Basic chemical pretreatments, bleaching and scouring were given to the RCS before extraction to remove natural colourants and hydrophobic impurities like oils, waxes, minerals, fats etc. The properties of EMC and CMC are considerably different from the RCS. Average particle size obtained was around 5–10 µm for EMC and CMC respectively. The EMC suspension was more stable than CMC suspension. The RCS, EMC and CMC were characterized by using X-ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy, scanning electronic microscopy and contact angle. EMC prepared from RCS has properties at par with CMC. Cotton being rich in cellulose content can be potentially used as the source for microcellulose extraction, particularly in the production of hydrophilic microcomposites.

36 MATERIALS SCIENCE↗

Influence of multi-walled carbon nanotubes (MWCNTs) volume percentage on the magnetic and microwave absorbing properties of BaMg{sub 0.5}Co{sub 0.5}TiFe{sub 10}O{sub 19}/MWCNTs nanocomposites

Graphical abstract: Reflection losses of (a) doped barium hexaferrite, BaMg{sub 0.5}Co{sub 0.5}TiFe{sub 10}O{sub 19}, sample and their nanocomposites with (b) 4 vol. (c) 8 vol. and (d) 12 vol.% of MWCNTs are presented. - Highlights: • BaMg{sub 0.5}Co{sub 0.5}TiFe{sub 10}O{sub 19}/MWCNTs nanocomposites were synthesized. • The structural, magnetic and microwave absorption properties were investigated. • The microwave absorption is strongly influenced by volume percentage of MWCNTs. • The nanocomposite with 8 vol.% of MWCNTs can be proposed as a wideband absorber. - Abstract: In this study BaMg{sub 0.5}Co{sub 0.5}TiFe{sub 10}O{sub 19}/MWCNTs nanocomposites with different amount of MWCNTs (0, 4, 8 and 12 vol.%) were synthesized. Here, the X-ray diffraction (XRD), Fourier transform spectroscopy (FTIR) and scanning electron microscopy (SEM) were used to demonstrate the structural and morphological characteristics of the prepared samples. XRD along with FTIR examinations exhibited that the nanocomposites were successfully synthesized. Vibrating sample magnetometer (VSM) showed the relatively strong dependence of saturation magnetization and coercivity on the volume percentage of MWCNTs. The microwave evaluation also confirmed that the complex permittivity of nanocomposites could be enhanced by adding MWCNTs. Finally, the nanocomposite with 8% vol. of MWCNTs exhibited the best microwave absorption performance among the samples.

36 MATERIALS SCIENCE↗

The Formation of Oxide Layers on a Titanium Surface by Irradiation with Femtosecond Laser Pulses

By subjecting technical grade titanium to irradiation with femtosecond laser pulses with high energy density, we create a microporous nanocrystalline oxide layer with a thickness of ∼50 μm on its surface. The structure and phase composition of the modified surface layers are studied using X-ray diffraction and high-resolution scanning and transmission electron microscopies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Real-Time Interactive 4D-STEM Phase-Contrast Imaging From Electron Event Representation Data: Less computation with the right representation

The arrival of direct electron detectors (DED) with high frame-rates in the field of scanning transmission electron microscopy has enabled many experimental techniques that require collection of a full diffraction pattern at each scan position, a field which is subsumed under the name four dimensional-scanning transmission electron microscopy (4D-STEM). DED frame rates approaching 100 kHz require data transmission rates and data storage capabilities that exceed commonly available computing infrastructure. Current commercial DEDs allow the user to make compromises in pixel bit depth, detector binning or windowing to reduce the per-frame file size and allow higher frame rates. This change in detector specifications requires decisions to be made before data acquisition that may reduce or lose information that could have been advantageous during data analysis. The 4D Camera, a DED with 87 kHz frame-rate developed at Lawrence Berkeley National Laboratory, reduces the raw data to a linear-index encoded electron event representation (EER). Here we show with experimental data from the 4D Camera that linear-index encoded EER and its direct use in 4D-STEM phase contrast imaging methods enables real-time, interactive phase-contrast from large-area 4D-STEM datasets. Furthermore, we detail the computational complexity advantages of the EER and the necessary computational steps to achieve real-time interactive ptychography and center-of-mass differential phase contrast using commonly available hardware accelerators.

4D-STEM↗

Engineered Barrier System R&D and International Collaborations – LANL (FY20): Spent Fuel and Waste Disposition

The United States Department of Energy’s Spent Fuel and Waste Disposition (SFWD) program is investigating the design and safety function of generic nuclear geologic repositories in a variety of geologic settings (salt, argillite, and crystalline rock). Different configurations and loadings of spent nuclear fuel and waste within disposal canisters are also being investigated, some of which have the potential to generate repository temperatures higher than previously considered (i.e., temperatures >100ºC) by foreign and domestic concepts. This report expands on engineered barrier material stability in a high temperature crystalline rock repository through high temperature hydrothermal experiments. Experiments were designed to develop engineered barrier system (EBS) concepts in a hightemperature crystalline environment in 1) bentonite-Grimsel Granodiorite interactions, 2) bentonite-cement reactions, and 3) interaction between waste canister materials and bentonite. Experiment results are applied to understanding long-term repository performance in terms of radionuclide isolation. One hydrothermal experiment was completed in the rocking autoclaves at LANL in FY-20: IEBS-6 (Grimsel Granodiorite + Wyoming bentonite + cured ordinary Portland cement + Grimsel Granodiorite synthetic groundwater, 250ºC/150 bar, 8 weeks). Several other experiments were planned but were delayed due to the COVID-19 pause in laboratory work. In addition, some characterization of the reaction products of experiments conducted in FY-20 was prevented by COVID-19. Mineral phase chemistry was not measured via electron microprobe analyses for IEBS-6. Quantitative X-ray diffraction results from IEBS-6 and HBT-1 were not completed. The missing analyses and discussion of the results will be included in next year’s report. New characterization that was completed includes scanning electron microscopy of reaction products from IEBS-6, quantitative X-ray diffraction results are presented from IEBS-1 through IBES-5, preliminary scanning electron microscope images and chemical analyses for IEBS-6, X-ray diffraction of the clay fraction from all experiments, measurement/imaging of mineral growth on the surface of steel coupons. Major observations pertaining to bentonite stability in a Grimsel Granodiorite environment include the stability of Na-montmorillonite at 250°C, the formation of trace CSH phases, and the formation of bentonite colloids on experiment cooling. The addition of a cured chip of Portland cement to the bentonite-Grimsel system results in slightly higher pH values and the formation of diverse secondary mineral phases that were not observed in the previous experiments (e.g., analcime, garronite, CSH phases). The new characterization efforts related to the interaction of stainless-steel coupons and bentonite clay focused on thickness and mineralogy of phases that formed at the steel surface. In Wyoming bentonite + Grimsel Granodiorite systems, newly formed minerals at the bentonitesteel coupon interface included alteration of the outermost steel edge to Fe,Cr-oxide phases, followed by Fe-rich phyllosilicates (Fe-saponite, chlorite) and interbedded Fe,Cr,Ni-sulfide phases (pentlandite). Hydrothermal experiments were completed to assess uranium-carbonate complexation at conditions relevant to high-temperature disposal. Autoclave solubility experiments were conducted at 150 to 250ºC with a range of carbonate and uranium concentrations. The experiment results were characterized via situ UV-Visible spectroscopy and synchrotron-based in situ XAS techniques. Results show a significant decrease in the stability of uranyl-carbonate complexes at temperatures above 100ºC along with the precipitation of uranium oxides. Further, at T > 200ºC, results show that uranyl-hydroxyl complexes control solubility of uranium instead of the previously predicted uranyl-carbonate species. These results are significant for understanding the mobility of uranium in the EBS, which will likely contain carbonate-rich fluids. International research efforts focused on three main areas: 1) participation in international conferences, 2) building collaborations with foreign repository programs, and 3) the initiation of an experimental program to complement the full-scale HotBENT test at the Grimsel test site. This experiment included Wyoming bentonite + low carbon steel + Grimsel Granodiorite synthetic groundwater and was run at the planned maximum temperature of the HotBENT test (200°C). Complete characterization of reaction products was hindered by disruptions to laboratory work but will be reported in the next FY. The experimental results obtained in FY-20 continue to document the wide-ranging effects of bulk composition and pressure-temperature conditions in the mineralogical and geochemical evolution of a high-temperature repository environment. Concepts developed will be used to inform models of long-term material stability in a generic crystalline rock-hosted repository.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Corrosion Behavior of AZ31 Magnesium Alloy Produced by Continuous Variable Cross Section Direct Extrusion

In order to study the corrosion behavior of magnesium alloys of high performance in the simulated seawater by continuous variable cross section direct extrusion (CVCDE), an electrochemical method and weight loss method were used to study the difference between AZ31 magnesium alloys produced by CVCDE with different numbers of interim dies to examine the electrochemical corrosion behavior and corrosion rate at 3.5 wt.% NaCl solution in this paper. Scanning electron microscopy and x-ray diffraction were used to analyze the morphology of corrosion surfaces and the composition of the corrosion products of samples soaked for different times. The results show that after CVCDE with different numbers of interim dies, the size of the microstructure is refined gradually, and the grain orientation is also different; with the increase in the number of interim dies, the thermodynamic corrosion tendencies are different, and the corrosion resistance of samples extruded by conventional extrusion is relatively good; the charge transfer and material transfer process are the two main factors affecting the corrosion rate, which determines the direction of the electrochemical reaction; the corrosion form of the sample extruded by CVCDE is the local corrosion which is the filiform corrosion and pitting corrosion, and the corrosion product is mainly water-insoluble Mg(OH){sub 2}.

36 MATERIALS SCIENCE↗

Fabrication of RGO-Fe3O4 Hybrid Functionalized with Ag3PO4 as photocatalyst for degradation of Rhodamime B under Visible Light Irradiation

Highlights: • The RFA-Cs, RGO-Fe{sub 3}O{sub 4} and Ag{sub 3}PO{sub 4} were successfully fabricated by a facile and effective electrostatic self-assembly method. • The RFA-Cs exhibited excellent efficiency on degradation of RhB in short time 2 min nearly 100% without sacrificial reagent. • The RFA-Cs is useful to reduce the recombination rate. • The RFA-Cs has provided a better photocatalytic efficiency without leaving behind any hazardous. - Abstract: RGO-Fe{sub 3}O{sub 4}-Ag{sub 3}PO{sub 4} composite (RFA-Cs) photocatalyst was prepared by a facile and effective electrostatic self-assembly method for photodegradation of Rhodamine B (RhB) under visible light irradiation. The prepared composites were fully characterized by scanning electron microscopy (SEM), X-ray diffraction meter (XRD), UV–vis diffuse reflectance spectroscopy (UV–vis), Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), photoluminescence spectroscopy (PL) and electrochemical impedance spectroscopy (EIS). The RFA-Cs exhibit extremely high photocatalytic activity and better re-usability. The photocatalytic conversion of RhB reaches as high as 100% after 2 min of light irradiation. A possible photocatalytic degradation and charge separation mechanism were suggested based on the PL spectra and the active species trapping experiments.

36 MATERIALS SCIENCE↗

Joining of C{sub f}/SiBCN Composite with a Ni-Cr-Pd(Si,B) Filler Alloy

Joining of C{sub f}/SiBCN composite was conducted by a newly designed Ni-Cr-Pd(Si,B) system filler alloy. The dynamic wettability on the C{sub f}/SiBCN composite was measured by the sessile drop method. The joint microstructure and the fracture surface were analyzed by scanning electron microscope and x-ray diffraction spectrometer. The results showed that the Ni-Cr-Pd(Si,B) filler alloy exhibited a low contact angle of 11.6° on the composite after holding at 1170 °C for 30 min. Element Cr played an active role in the interfacial reaction, and a Cr{sub 7}C{sub 3} reaction layer with a thickness of 8 µm was formed at the surface of the C{sub f}/SiBCN composite. Under the brazing condition of 1170 °C for 10 min, the joint strength at the room temperature reached 66.8 MPa. When the test temperature increased to 600 and 800 °C, the joint strength was even elevated to 90.3 and 81.2 MPa, respectively. The joint strength at high temperature was higher than that at room temperature, and this should be attributed to the improvement of the joint plasticity and the release of the residual thermal stresses within the brazed joint.

36 MATERIALS SCIENCE↗

Rapid Separation of Copper Phase and Iron-Rich Phase From Copper Slag at Low Temperature in a Super-Gravity Field

A novel approach for quickly separating a metal copper phase and iron-rich phase from copper slag at low temperature is proposed based on a super-gravity method. The morphology and mineral evolution of the copper slag with increasing temperature were studied using in situ high-temperature confocal laser scanning microscopy and ex situ scanning electron microscopy and X-ray diffraction methods. Fe{sub 3}O{sub 4} particles dispersed among the copper slag were transformed into FeO by adding an appropriate amount of carbon as a reducing agent, forming the slag melt with SiO{sub 2} at low temperature and assisting separation of the copper phase from the slag. Consequently, in a super-gravity field, the metallic copper and copper matte were concentrated as the copper phase along the super-gravity direction, whereas the iron-rich slag migrated in the opposite direction and was quickly separated from the copper phase. Increasing the gravity coefficient (G) significantly enhanced the separation efficiency. After super-gravity separation at G = 1000 and 1473 K (1200 °C) for 3 minutes, the mass fraction of Cu in the separated copper phase reached 86.11 wt pct, while that in the separated iron-rich phase was reduced to 0.105 wt pct. The recovery ratio of Cu in the copper phase was as high as up to 97.47 pct.

36 MATERIALS SCIENCE↗

Enhanced long-term strength and durability of shotcrete with high-strength C{sub 12}A{sub 7} mineral-based accelerator

This study evaluated the performance of shotcrete using high strength C{sub 12}A{sub 7} mineral-based accelerator that has been developed to improve the durability and long-term strength. Rebound, compressive strength and flexural strength were tested in the field. Test result showed that existing C{sub 12}A{sub 7} mineral-based accelerator exhibits better early strength than the high-strength C{sub 12}A{sub 7} mineral-based accelerator until the early age, but high-strength C{sub 12}A{sub 7} mineral-based accelerator shows about 29% higher at the long-term age of 28 days. Microstructural analysis such as scanning electron microscope (SEM), X-ray diffraction (XRD) and nitrogen adsorption method was evaluated to analyze long-term strength development mechanism of high strength C{sub 12}A{sub 7} mineral-based accelerator. As analysis result, it had more dense structure due to the reaction product by adding material that used to enhanced strength. It had better resistance performance in chloride ion penetration, freezing–thawing and carbonation than shotcrete that used existing C{sub 12}A{sub 7} mineral-based accelerator.

36 MATERIALS SCIENCE↗