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All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Effect of boron on the structural and magnetic properties of Co{sub 2}FeSi{sub 1-x}B{sub x} Heusler alloys

The partial substitution of Si with B on the structural and magnetic properties of Co{sub 2}FeSi{sub 1-x}Bx (x = 0-0.5) alloys was systematically investigated. X-ray and microstructural investigations show the presence of second phase at the grain boundaries which increases with increasing boron content. From thermal analysis studies, it was observed that L2{sub 1}-B2 ordering temperature remain constant whereas the melting point decreases with increase in boron addition and merges with ordering temperature at x = 0.5. The increase in T{sub C} for the alloys x ≥ 0.25 was attributed to the increase in second phase due to boron.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Wide-blocky veins explained by dependency of crystal growth rate on fracture surface type: Insights from phase-field modeling

Vein microstructures contain a wealth of information on coupled chemical and mechanical processes of fracturing, fluid transport, and crystal growth. Numerical simulations have been used for exploring the factors controlling the development of vein microstructures; however, they have not been quantitatively validated against natural veins. Here we combined phase-field modeling with microtextural analysis of previously unexplained wide-blocky calcite veins in natural limestone and of the fresh fracture surface in this limestone. Results show that the wide-blocky vein textures can only be reproduced if ~10%–20% of crystals grow faster than the rest. This fraction corresponds to the amount of transgranularly broken grains that were observed on the experimental fracture surfaces, which are dominantly intergranular. We hypothesize that transgranular fractures allow faster growth of vein minerals due to the lack of clay coatings and other nucleation discontinuities that are common along intergranular cracks. Our simulation results show remarkable similarity to the natural veins and reproduce the nonlinear relationship between vein crystal width and vein aperture. This allows accurate simulations of crystal growth processes and related permeability evolution in fractured rocks.

Geology↗
NASA NTRS1998

Fundamentals of Passive Oxidation In SiC and Si3N4

The very slow oxidation kinetics of silicon carbide and silicon nitride, which derive from their adherent and passivating oxide films, has been explored at length in a broad series of studies utilizing thermogravimetric analysis, electron and optical micrography, energy dispersive spectrometry, x-ray diffractometry, micro-analytical depth profiling, etc. Some interesting microstructural phenomena accompanying the process of oxidation in the two materials will be presented. In Si3N4 the oxide is stratified, with an SiO2 topscale (which is relatively impervious to O2)underlain by a coherent subscale of silicon oxynitride which is even less permeable to O2- Such "defence in depth" endows Si3N4 with what is perhaps the highest oxidation resistance of any material, and results in a unique set of oxidation processes. In SiC the oxidation reactions are much simpler, yet new issues still emerge; for instance, studies involving controlled devitrification of the amorphous silica scale confirmed that the oxidation rate of SiC drops by more than an order of magnitude when the oxide scale fully crystallizes.

Thomas-Ogbuji, Linus U.↗
NASA NTRS1992

Automated Weld Characterization Using the Thermoelectric Method

The effective assessment of the integrity of welds is a complicated NDE problem that continues to be a challenge. To be able to completely characterize a weld, detailed knowledge of its tensile strength, ductility, hardness, microstructure, macrostructure, and chemical composition is needed. NDE techniques which can provide information on any of these features are extremely important. In this paper, we examine a seldom used approach based on the thermoelectric (TE) effect for characterizing welds and their associated heat affected zone (HAZ). The thermoelectric method monitors the thermoelectric power which is sensitive to small changes in the kinetics of the conduction electrons near the Fermi surface that can be caused by changes in the local microstructure. The technique has been applied to metal sorting, quality testing, flaw detection, thickness gauging of layers, and microscopic structural analysis. To demonstrate the effectiveness of the technique for characterizing welds, a series of tungsten-inert-gas welded Inconel-718 samples were scanned with a computer controlled TE probe. The samples were then analyzed using a scanning electron microscope and Rockwell hardness tests to characterize the weld and the associated HAZ. We then correlated the results with the TE measurements to provide quantitative information on the size of the HAZ and the degree of hardness of the material in the weld region. This provides potentially valuable information on the strength and fatigue life of the weld. We begin the paper by providing a brief review of the TE technique and then highlight some of the factors that can effect the measurements. Next, we provide an overview of the experimental procedure and discuss the results. Finally, we summarize our findings and consider areas for future research.

Fulton, J. P.↗
NASA NTRS2003

Superalloy Disk With Dual-Grain Structure Spin Tested

Advanced nickel-base disk alloys for future gas turbine engines will require greater temperature capability than current alloys, but they must also continue to deliver safe, reliable operation. An advanced, nickel-base disk alloy, designated Alloy 10, was selected for evaluation in NASA s Ultra Safe Propulsion Project. Early studies on small test specimens showed that heat treatments that produced a fine grain microstructure promoted high strength and long fatigue life in the bore of a disk, whereas heat treatments that produced a coarse grain microstructure promoted optimal creep and crack growth resistance in the rim of a disk. On the basis of these results, the optimal combination of performance and safety might be achieved by utilizing a heat-treatment technology that could produce a fine grain bore and coarse grain rim in a nickel-base disk. Alloy 10 disks that were given a dual microstructure heat treatment (DMHT) were obtained from NASA s Ultra-Efficient Engine Technology (UEET) Program for preliminary evaluation. Data on small test specimens machined from a DMHT disk were encouraging. However, the benefit of the dual grain structure on the performance and reliability of the entire disk still needed to be demonstrated. For this reason, a high temperature spin test of a DMHT disk was run at 20 000 rpm and 1500 F at the Balancing Company of Dayton, Ohio, under the direction of NASA Glenn Research Center personnel. The results of that test showed that the DMHT disk exhibited significantly lower crack growth than a disk with a fine grain microstructure. In addition, the results of these tests could be accurately predicted using a two-dimensional, axisymmetric finite element analysis of the DMHT disk. Although the first spin test demonstrated a significant performance advantage associated with the DMHT technology, a second spin test on the DMHT disk was run to determine burst margin. The disk burst in the web at a very high speed, over 39 000 rpm, in line with the predicted location and speed. Furthermore, significant growth of the disk was observed before failure, in line with predictions, clearly demonstrating the reliability and safety of the DMHT technology. Although successful spin testing in Ultra Safe's Nickel Disk Program represents a significant milestone for DMHT technology, realistic engine operation will require repeated loading of a DMHT nickel disk. For this reason, a cyclic spin test study of DMHT nickel disk technology has been proposed to start in fiscal year 2003 under NASA's Aviation Safety Program. The goal of this program will be to determine the fatigue failure mechanism in DMHT nickel disks, thereby demonstrating the reliability and safety of DMHT technology under repetitive loading conditions encountered in realistic engine operation.

Gayda, John↗
NASA NTRSDate not supplied

Unraveling Solar Wind Space Weathering of Carbon-Rich Asterods: Low-Flux VS. High-Flux Ion Irradiation of Murchison

Introduction: Space weathering processesalter the microstructural, compositional, and optical properties of airless planetary surfaces.Solar wind space weatheringforms ion-damaged rims within the outermost ~100 nm of regolith grains through atomic-displacements and implantation of energetic H+and He+ions[1]. Transmission electron microscope(TEM)studies of space weathered Itokawa and lunar olivine particles reveal predominantly nanocrystalline solar wind-damaged rims with only minor regions of amorphization[2-5]. This finding differs from laboratoryion irradiation experiments in which samples become amorphous at fluences 2-3 orders of magnitude lower than the independentlyconstrained fluences for still-crystalline natural samples [6-7].Ion flux is generally considered to have a secondaryeffectcompared to fluence in these irradiation experiments. However, solar wind irradiation of natural samples occurs at a flux that is ~4-5 orders of magnitude lower than whatisused inlaboratory simulations (e.g., [6,8-9]). Constraining how the very low ion flux of solar wind influences the microstructural, chemical, and spectral alteration of silicate minerals will improve our understanding of solar wind space weathering and aid in the analysis of returned samples from the Hayabusa2 and OSIRIS-REx missions. Here we report results from low-and high-flux ion irradiation experiments on the Murchison (CM2)meteoritewithcomparable total fluences. Methods: We performed low-flux and high-flux He+(4 keV) and H+(1 keV) irradiation experiments on separate, dry-cut Murchison slabs. Low-flux He+irradiation reached a total fluence of 2.1 x 1016ions/cm2(~400 years of exposure at Bennu) using a flux of 3.6 x 1011ions/cm2/s; low-flux H+irradiation reached a total fluence of 3.9 x 1016ions/cm2(~30 years) using a flux of 6.6 x 1011ions/cm2/s. High-flux He+irradiation reached a total fluence of 2.0 x 1016ions/cm2(~400 years)using a flux of 9.1 x 1012ions/cm2/s; high-flux H+irradiation reached a total fluence of 5.8 x 1016ions/cm2(~50 years)using flux of 8.4 x 1012ions/cm2/s. By irradiating to similar total fluences in both the low-flux and high-flux experiments, we can better isolate and evaluatethe effects of ion flux. Differences between unirradiatedand irradiated surfaces are determined using threeanalytical techniques:(1) in situX-ray photoelectron spectroscopy(XPS) reveals changes in surface chemistry,(2) visible to near-infrared spectroscopy (VNIR; 0.35-2.5 μm) highlights changes in spectraltrends, such as albedo and slope, and (3) TEM and energy-dispersive X-ray spectroscopy (EDS) identifieschanges in nanoscale structure and elemental composition within olivine and matrix electron-transparent thin sections prepared using focused ion beam scanning electron microscopy (FIB-SEM). Results and Discussion: XPS analyses of the low-fluxand high-fluxHe+-and H+-irradiated samples showa minorreduction in surface carbon contentand chemicalreduction ofFe3+to Fe2+. The latter result is consistent with the higher Fe2+/Fe3+ratios observed in phyllosilicate-rich space weathered rims of Ryugu grains [10].VNIR analyses suggest that the low-flux H+-irradiated spectrum has a slightly bluer slope (over 0.65-2.5 μm) compared to the unirradiated VNIR spectrum from [9] while the low-flux He+-irradiated spectral slope is comparable to the unirradiated surface. Both the high-flux He+-and H+-irradiated VNIR spectra exhibitslightlyhigheralbedos at shorter wavelengths relativeto their unirradiated counterparts, with He+irradiation yielding a greater change. Thus far, the low-flux He+-irradiated matrix and olivine FIBsections as well as the low-flux H+-irradiated olivine FIBsection have been examined with TEM. The surfaces of all three samplesshowless vesiculation than high-flux/high-fluenceirradiated matrix and olivine samples from [9]. The depth of phyllosilicate amorphization in thelow-fluxHe+-irradiated matrix FIBsection varieslaterally, with crystalline domains occurring as shallow as ~25 nm in some regions. Thelow-flux He+-irradiated olivine FIBsection has acontinuous,~40-90 nm thick ion-affected layer with polycrystalline and amorphous microstructures. The low-flux H+-irradiated olivine sampleexhibits a distinct, ~10-40 nm ion-affected layer whose uppermost ~20 nmin thicker regions is predominantly amorphous.Continuing to compare results from this work to those from [9] will provide a comprehensive understanding of how ion flux impacts the microstructural, chemical, and optical modification of various mineral phases and, in turn,help identify space weathering features from parent body alteration in Hayabusa2 and OSIRIS-REx returned samples.

D L Laczniak↗
DOE OSTI2015

Monoclinically distorted perovskites, A{sub 2}ZnTiO{sub 6} (A=Pr, Gd): Rietveld refinement, and dielectric studies

Double perovskite related oxide A{sub 2}ZnTiO{sub 6}A=Pr, Gd were synthesized by the solid state reaction method at 1523 K. The structure and microstructure of the compounds were studied by X-ray, SAED and FESEM. Rietveld refinement of the powder X-ray analysis shows that the compounds crystallizes in monoclinic space group P2{sub 1}/n (a{sup +}b{sup −}b{sup −}) with unit cell parameter √2a{sub p}×√2a{sub p}×2a{sub p} (a=5.5026(1) Å, b=5.6305(1) Å, c=7.8149(1) Å, β=90.02(1)° for Pr{sub 2}ZnTiO{sub 6} and a=5.3621(1) Å, b=5.6565(2) Å, c=7.6779(2) Å and β=90.264(2)° for Gd{sub 2}ZnTiO{sub 6}. Electron diffraction study confirms P2{sub 1}/n symmetry of the oxides. The monoclinic distortion is larger in Gd{sub 2}ZnTiO{sub 6} than Pr{sub 2}ZnTiO{sub 6} which is associated with the tolerance factor and the tilting angle of ZnO{sub 6} and TiO{sub 6} octahedra (ϕ=13.64° for Pr{sub 2}ZnTiO{sub 6} and 16.51° for Gd{sub 2}ZnTiO{sub 6}). The compounds are highly ordered. The charge and size difference between B site cations are the driving force for the ordering of the B′O{sub 6} and B″O{sub 6} octahedra. Pr{sub 2}ZnTiO{sub 6} shows a dielectric constant of 27 and dielectric loss of 0.003 while Gd{sub 2}ZnTiO{sub 6} has a dielectric constant of 17 and dielectric loss of 0.005 measured at 1 MHz. - Graphical abstract: Synthesis of new double perovskite dielectric material with very low dielectric loss. - Highlights: • Synthesis of new monoclinically distorted double perovskite (Pr{sub 2}ZnTiO{sub 6}). • Synthesis of monoclinically distorted double perovskite (Gd{sub 2}ZnTiO{sub 6}). • Selected area electron diffraction study of A{sub 2}ZnTiO{sub 6} (A=Pr, Gd). • Study of dielectric properties of A{sub 2}ZnTiO{sub 6} (A=Pr, Gd)

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Report on Properties and Microstructure of 3D Printed Inc-718

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 to assess its potential use as a structural material for the Transformation Challenge Reactor (TCR). The structural components near the outlet of the core will experience significant neutron fluxes and outlet coolant temperatures from the hot standby temperature of 300°C to nearly 550°C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. Strong spatial and chemical heterogeneity was found in as-built (ASB) Inconel 718. Three heat treatments were designed and conducted to simplify the microstructure and determine how each precipitating phase contributed to the overall strength. Baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600°C. Microstructure electron microscopy was performed on ASB Inconel 718 and heat treated to correlate the observed mechanical properties with nanoscale features. Homogenization of the microstructure led to a highly ductile Inconel with lower strength compared with wrought Inconel 718. The tensile properties of additively manufactured 718 using a standard ASTMrecommended heat treatment were consistent with literature and with the ASTM for the properties of this alloy. A higher fraction of the δ phase led to shorter uniform elongation without altering other engineering properties.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2019

Thermo-Oxidative Aging of LDPE/Stearoyl Chloride-Grafted Cellulose Nanocrystals Blown Films

The effect of the incorporation of pristine and stearoyl chloride grafted CNCs on the chemical, mechanical, thermal and microstructural properties, during the thermo-oxidative aging, of LDPE blown films at 60 °C was studied. The success of the pristine CNCs grafting was assessed by Fourier transform infrared (FT-IR) spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Thermal-gravimetric analysis (TGA), Atomic Force Spectroscopy (AFM) and contact angle measurements. The results show that chemical modification decreases both, the CNCs thermal stability and the polar component of surface energy, i.e. increases the nanocrystals hydrophobicity. Also, it was found that neither CNCs crystalline structure nor its dimensions changed with grafting. The changes on the blown film properties during thermo-oxidative aging were monitored using FT-IR, DSC, DRX and tensile testing. It was found that the CNCs catalyzed the production of carboxylic acids as a final degradation by-product, whereas the CNC-g-C{sub 18} inhibits its formation, i.e. in presence of CNCs grafted with stearoyl chloride the catalytic effect attributed to the pristine CNCs was partially inhibited. The DSC, DRX and tensile testing results show the microstructural arrangements due to the annealing and the chains oxidation predominated during the first 30 days of aging and then chain scissions prevail. These findings suggest an analogous reduction in molecular weight at the end thermo-oxidative aging. In addition, the presence of a high concentration of carboxylic acid and the drop in molecular weight after LDPE aging will facilitate the biodegradation of these oxo-degradable films.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Low Activation Joining of SiC/SiC Composites for Fusion Applications: Thermomechanical Modeling of Dual-Phase Microstructures and Dissimilar Material Joints

Finite element (FE) continuum damage mechanics (CDM) models have been developed to simulate and model dual-phase joints and cracked joints for improved analysis of SiC materials in nuclear environments. This report extends the analysis from the last reporting cycle by including preliminary thermomechanical analyses of cracked joints and implementation of dual-phase damage models.

Nguyen, Ba Nghiep↗
DOE OSTI2012

Microstructures and microhardness evolutions of melt-spun Al-8Ni-5Nd-4Si alloy

Al-Ni-Nd-Si alloy with nominal composition of Al-8 wt.%Ni-5 wt.%Nd-4 wt.%Si was rapidly solidified by using melt-spinning technique to examine the influence of the cooling rate/conditions on microstructure and mechanical properties. The resulting conventional cast (ingot) and melt-spun ribbons were characterized by X-ray diffraction, optical microscopy, scanning electron microscopy together with energy dispersive spectroscopy, differential scanning calorimetry, differential thermal analysis and Vickers microhardness tester. The ingot alloys consists of four phases namely {alpha}-Al, intermetallic Al{sub 3}Ni, Al{sub 11}Nd{sub 3} and fcc Si. Melt-spun ribbons are completely composed of {alpha}-Al phase. The optical microscopy and scanning electron microscopy results show that the microstructures of rapidly solidified ribbons are clearly different from their ingot alloy. The change in microhardness is discussed based on the microstructural observations. - Highlights: Black-Right-Pointing-Pointer Rapid solidification allows a reduction in grain size, extended solid solution ranges. Black-Right-Pointing-Pointer We observed the matrix lattice parameter increases with increasing wheel speed. Black-Right-Pointing-Pointer Melt-spun ribbons consist of partly amorphous phases embedded in crystalline phases. Black-Right-Pointing-Pointer The solidification rate is high enough to retain most of alloying elements in the Al matrix. Black-Right-Pointing-Pointer The rapid solidification has effect on the phase constitution.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Insight into the interfacial microstructure and chemistry of hot isostatically pressed AA6061-AA6061 bonds for U-10Mo fuel cladding application

Here, in the present study, hot isostatic pressing (HIP) bonding was carried out using AA6061-AA6061 plates for U-10Mo monolithic fuel cladding application. HIP was performed at 560°C with an applied isostatic pressure of 103 MPa for 90 min. Interfacial microstructure characterizations were performed using scanning electron microscopy (SEM) combined with electron backscatter diffraction (EBSD) to quantify precipitate fractions and study recrystallization, grain growth, and orientation relationships across the interface. EBSD results confirmed that no interfacial grain growth occurred during the HIP process. Transmission electron microscopy (TEM) was also employed to quantify composition and identify phases of various precipitates and an oxide layer that formed at the interface during HIP bonding. Microstructural analyses revealed the formation of a large fraction of Mg 2 Si precipitate and a ~50 nm thick Mg-oxide layer at the interface. Further TEM analysis confirmed that the oxide layer was not continuous, and Mg 2 Al 2 O 5 oxide particles with an average size of 18 nm were present in the oxide layer. Finite element modeling analysis was performed to study the stress distribution at the interface during HIP processing.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

Effects of alpha-zirconium phosphate on thermal degradation and flame retardancy of transparent intumescent fire protective coating

Graphical abstract: - Highlights: • A transparent intumescent fire protective coating was obtained by UV-cured technology. • OZrP could enhance the thermal stability and anti-oxidation of the coating. • OZrP could reduce the combustion properties of the coatings. - Abstract: Organophilic alpha-zirconium phosphate (OZrP) was used to improve the thermal and fire retardant behaviors of the phenyl di(acryloyloxyethyl)phosphate (PDHA)-triglycidyl isocyanurate acrylate (TGICA)-2-phenoxyethyl acrylate (PHEA) (PDHA-TGICA-PHEA) coating. The morphology of nanocomposite coating was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effect of OZrP on the flame retardancy, thermal stability, fireproofing time and char formation of the coatings was investigated by microscale combustion calorimeter (MCC), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), laser Raman spectroscopy (LRS) and scanning electric microscope (SEM). The results showed that by adding OZrP, the peak heat release rate and total heat of combustion were significantly reduced. The highest improvement was achieved with 0.5 wt% OZrP. XPS analysis indicated that the performance of anti-oxidation of the coating was improved with the addition of OZrP, and SEM images showed that a good synergistic effect was obtained through a ceramic-like layer produced by OZrP covered on the surface of char.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Structural and thermal characterization of CaO-MgO-SiO2-P2O5-CaF2 glasses

The paper presents the influence of varying CaO/MgO ratio on the structure and thermal properties of CaO-MgO-SiO2-P2O5-CaF2 glasses. A series of eight glass compositions in the glass forming region of diopside (CaMgSi2O6) - fluorapatite [Ca5(PO4)3F] - wollastonite (CaSiO3) ternary system have been designed and synthesized by varying diopside/wollastonite ratio in glasses. The as prepared melt-quenched glasses have been characterized for their structure by infrared spectroscopy (FTIR) and magic angle spinning (MAS)-nuclear magnetic resonance (NMR) spectroscopy. Silicon is predominantly present as Q2 (Si) species, while phosphorus tends to coordinate in orthophosphate environment in all the investigated glasses. The change in CaO/MgO ratio had an insignificant affect on the structure of glasses. The thermal sintering and crystallization parameters for the studied glasses have been obtained from differential thermal analysis (DTA) while crystalline phase fractions in the sintered glass-ceramics have been analyzed by X-ray diffraction adjoined with Rietveld refinement. Diopside, fluorapatite, wollastonite and pseudowollastonite have crystallized as the main crystalline phases in all the glass-ceramics with their content varying with respect to variation in CaO/MgO ratio in glasses. Scanning electron microscopy (SEM) has been used to shed light on the microstructure of glass-ceramics. The possible implications of structure and sintering behaviour of glasses on their bioactivity have been discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2021

The onset of alloying in Cu-Ni powders under high-shear consolidation

Friction consolidation (FC) is a solid phase processing methodology that densifies a material through high-shear deformation and pressure at elevated temperature. The method has garnered interest in the scientific community because of its ability to produce extremely refined and homogeneous microstructures, off-axis texture development, and improved material properties. This manuscript presents an investigation of Cu and Ni material mixing via evaluation of morphological evolution, grain boundary characterization, and compositional analysis to provide insights on the operational alloying mechanisms occurring under high shear and elevated temperature. Using correlative microscopy techniques, we show alloying progresses via a combination of grain boundary diffusion and interfacial roughening at heterophane boundaries. Evidence supporting Cu infiltration along Ni-Ni grain boundaries along with asymmetric diffusion of Cu into Ni grains is highlighted. The resultant, consolidated microstructure was produced directly from a powder compact in ~30 s and exhibited a submicron, equiaxed grain size.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Effect of KCl, NaCl and CaCl{sub 2} mixture on volume combustion synthesis of TiB{sub 2} nanoparticles

Highlights: {yields} A low melting diluent lowers the ignition temperature in combustion synthesis. {yields} Deagglomerated synthesized products are formed as the result of diluent addition. {yields} Addition of 45% salt mixture resulted in formation of 70 nm TiB{sub 2} nanoparticles. {yields} Thermodynamically unstable Mg{sub 2}TiO{sub 4} and Mg{sub 3}B{sub 2}O{sub 6} by-products were formed. {yields} Small change in particle size was observed with addition of salt mixture. -- Abstract: Preparation of titanium diboride (TiB{sub 2}) nanoparticles was carried out by volume combustion synthesis. TiO{sub 2}, B{sub 2}O{sub 3} and elemental Mg were mixed with 0-60% salt mixture of KCl, NaCl and CaCl{sub 2} with increment of 15% as a low melting temperature diluent. Compressed samples were synthesized in a tubular furnace at a constant heating rate under argon atmosphere. Thermal analysis of the process showed that the addition of the low melting temperature salts mixture led to a significant decrease in ignition and combustion temperatures. Synthesized samples were then leached by nitric and hydrochloric acids to remove impurities. The samples were examined by XRD, SEM and DLS analysis. The results showed the formation of fine deagglomerated particles with the addition of the salts mixture. The results revealed that 45% salts mixture had the smallest average particle size of about 90 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Fabrication of flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} and their electrochemical properties evaluation

Graphical abstract: Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} nano-flakes materials, which have a flower-like structure, were successfully synthesized by a facile solvothermal method without adding any surfactant. The as-prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} possesses a maximum specific capacitance of 2212.5 F g{sup −1} at the current density of 5 mA, suggesting its potential application in electrode material for secondary batteries and electrochemical capacitors. Highlights: ► Flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} materials were fabricated in a simple method. ► High specific capacitance of 2212.5 F g{sup −1} has been achieved. ► For the first time the effects of concentration and temperature on its specific capacitance has been studied. -- Abstract: Flower-like Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} was successfully synthesized by a facile solvothermal method. The microstructure and surface morphology of prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} were physically characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and transmission electron microscope (TEM). The electrochemical properties studies were carried out using cyclic voltammetry (CV), chronopotentiometry technology and AC impedance spectroscopy, respectively. The results indicate that the flower-like structure has a profound impact on electrode performance at high discharge capacitance. A maximum specific capacitance of 2212.5 F g{sup −1} at the current density of 5 mA could be achieved, suggesting its potential application in electrode material for secondary batteries and electrochemical capacitors. Furthermore, the effects of Ni(NO{sub 3}){sub 2}·6H{sub 2}O concentration and temperature on the microstructure and specific capacitance of prepared Ni{sub 3}(NO{sub 3}){sub 2}(OH){sub 4} have also been systematically studied. The results show that flower-like structure can be formed when the concentration is appropriate, while the temperature has just little effect on its electrochemical properties.

36 MATERIALS SCIENCE↗

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