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At least 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

The annealing temperature dependences of microstructures and magnetic properties in electro-chemical deposited CoNiFe thin films

CoNiFe thin films with various compositions had been successfully fabricated using electro-chemical deposition method. The crystal structure of Co{sub 65}Ni{sub 15}Fe{sub 20}, Co{sub 62}Ni{sub 15}Fe{sub 23}, and Co{sub 55}Ni{sub 15}Fe{sub 30} thin films was fcc, bcc-fcc mix, and bcc, respectively. The difference crystal structure results the difference in magnetic properties. The saturation magnetic flux density (Bs) of Co{sub 65}Ni{sub 15}Fe{sub 20}, Co{sub 62}Ni{sub 15}Fe{sub 23}, and Co{sub 55}Ni{sub 15}Fe{sub 30} thin films was 1.89 T, 1.93 T, and 2.05 T, respectively. An optimal annealing temperature was determined for controlling the microstructure and magnetic properties of CoNiFe thin films. Depending on annealing temperature, the ratio of bcc and fcc structure varied without changing the film composition. By annealing at temperature of T ≥ 350°C, the intensity ratio of X-ray diffraction peaks for bcc(110) to fcc(111) increased. The increase of phase ratio of bcc(110) to fcc(111) caused the increase of Bs, from 1.89 T to 1.95 T. Coercivity (Hc) also increased after annealing, from 2.6 Oe to 18.6 Oe for fcc phase thin films, from 2.0 Oe to 12.0 Oe for fcc-bcc mix phase thin films, and 7.8 Oe to 8 Oe for bcc phase thin films. The changing crystal structures during annealing process indicated that the thermal treatment at high temperature cause the changing crystallinity and atomic displacement. The TEM bright-field images with corresponding selected-area electron diffraction (SAED) patterns showed that there are strongly effects of thermal annealing on the size of fcc and bcc phase crystalline grain as described by size of individual spot and discontinuous rings. The size of crystalline grains increased by thermal annealing. The evolution of bcc and fcc structures of CoNiFe during annealing is though to be responsible for the change of magnetic properties.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Surface and magnetic characteristics of Ni-Mn-Ga/Si (100) thin film

Polycrystalline Ni-Mn-Ga thin films have been deposited on Si (100) substrate with different film thickness. The influence of film thickness on the phase structure and magnetic domain of the films has been examined by scanning electron microscope, atomic force microscopy and magnetic force microscopy. Analysis of structural parameters indicates that the film at lower thickness exhibits the coexistence of both austenite and martensite phase, whereas at higher thickness L1{sub 2} cubic non magnetic phase is noticed. The grains size and the surface roughness increase along with the film thickness and attain the maximum of 45 nm and 34.96 nm, respectively. At lower film thickness, the magnetic stripe domain is found like maze pattern with dark and bright images, while at higher thickness the absence of stripe domains is observed. The magnetic results reveal that the films strongly depend on their phase structure and microstructure which influence by the film thickness.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Low temperature aluminum nitride thin films for sensory applications

A low-temperature sputter deposition process for the synthesis of aluminum nitride (AlN) thin films that is attractive for applications with a limited temperature budget is presented. Influence of the reactive gas concentration, plasma treatment of the nucleation surface and film thickness on the microstructural, piezoelectric and dielectric properties of AlN is investigated. An improved crystal quality with respect to the increased film thickness was observed; where full width at half maximum (FWHM) of the AlN films decreased from 2.88 ± 0.16° down to 1.25 ± 0.07° and the effective longitudinal piezoelectric coefficient (d{sub 33,f}) increased from 2.30 ± 0.32 pm/V up to 5.57 ± 0.34 pm/V for film thicknesses in the range of 30 nm to 2 μm. Dielectric loss angle (tan δ) decreased from 0.626% ± 0.005% to 0.025% ± 0.011% for the same thickness range. The average relative permittivity (ε{sub r}) was calculated as 10.4 ± 0.05. An almost constant transversal piezoelectric coefficient (|e{sub 31,f}|) of 1.39 ± 0.01 C/m{sup 2} was measured for samples in the range of 0.5 μm to 2 μm. Transmission electron microscopy (TEM) investigations performed on thin (100 nm) and thick (1.6 μm) films revealed an (002) oriented AlN nucleation and growth starting directly from the AlN-Pt interface independent of the film thickness and exhibit comparable quality with the state-of-the-art AlN thin films sputtered at much higher substrate temperatures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Effect of defects, magnetocrystalline anisotropy, and shape anisotropy on magnetic structure of iron thin films by magnetic force microscopy

Microstructures of magnetic materials, including defects and crystallographic orientations, are known to strongly influence magnetic domain structures. Measurement techniques such as magnetic force microscopy (MFM) thus allow study of correlations between microstructural and magnetic properties. The present work probes effects of anisotropy and artificial defects on the evolution of domain structure with applied field. Single crystal iron thin films on MgO substrates were milled by Focused Ion Beam (FIB) to create different magnetically isolated squares and rectangles in [110] crystallographic orientations, having their easy axis 45° from the sample edge. To investigate domain wall response on encountering non-magnetic defects, a 150 nm diameter hole was created in the center of some samples. By simultaneously varying crystal orientation and shape, both magnetocrystalline anisotropy and shape anisotropy, as well as their interaction, could be studied. Shape anisotropy was found to be important primarily for the longer edge of rectangular samples, which exaggerated the FIB edge effects and provided nucleation sites for spike domains in non-easy axis oriented samples. Center holes acted as pinning sites for domain walls until large applied magnetic fields. The present studies are aimed at deepening the understanding of the propagation of different types of domain walls in the presence of defects and different crystal orientations.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Electrode and Microstructure Dependence of Oxygen Diffusion in Ferroelectric Hafnium Zirconium Oxide Thin Films

Hafnia-based ferroelectrics hold promise to reduce energy demand for computing by enabling compute-in-memory and as non-volatile memories. The ferroelectric phase in this material system is, in part, stabilized by oxygen vacancies. While oxygen vacancies may be a necessity for phase stability, they limit device endurance through diffusion and accumulation into conducting channels. Herein, it is shown that oxygen diffusion is spatially variable within individual grains of ferroelectric hafnium zirconium oxide (HZO). Using 18 O tracers and finite difference modeling, it is shown that grain boundaries and regions near electrode interfaces allow for relatively rapid oxygen diffusion, with values as much as 10 4 larger than the grain cores. Further, the selection of electrode material affects the diffusion coefficients across all microstructural regions. HZO films in contact with TiN electrodes result in more oxygen-deficient HZO films and higher oxygen diffusion coefficients. Tungsten electrodes result in fewer vacancies and lower diffusion coefficients. Diffusion activation energy differences between the HZO with the two electrodes is reconciled by differing populations of charged and uncharged oxygen vacancies. This insight into the local vacancy populations and diffusion pathways provides a platform for designing hafnia-based films, deposition processes, and integration strategies to reduce vacancy gradients and improve performance.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Ti Capping Layer Effects in Microstructure and Magnetic Properties of Sputter-Deposited FePt Thin Film

Ti/FePt/Fe nano-thin films were fabricated by a DC facing-target magnetron sputtering method onto glass substrates at room temperature and were subsequently annealed in situ in vacuum. The impacts of the Ti capping layer on microstructural and magnetic properties of the FePt films were investigated in detail. X-ray diffraction (XRD) patterns demonstrate that the film is deposited onto glass substrates and the addition of a Ti layer forms ternary TiFePt, and binary PtTi and FeTi alloys. The results reveal refined granularity, decreased roughness, and enhanced coercivity and degree of squareness after the introduction of a Ti capping layer.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Neutron irradiation effects on the corrosion of Zircaloy-4 in a pressurized water reactor environment - 2016-0085

Long-time Advanced Test Reactor (ATR) corrosion weight-gain data from non-fueled α-processed Zircaloy-4 cladding coupons are presented herein. The data were generated in pressurized loops that simulated pressurized water reactor (PWR) chemistry, temperature, and neutron flux conditions. High neutron flux and high-fluence post-transition corrosion rates were accelerated over out-of-flux post-transition corrosion rates by more than 40 times at 270 deg. C and more than 30 times at 310 deg. C We conclude in large part that the acceleration was caused by irradiation-induced changes to the base metal. The effect that irradiation has on the base metal and its effect on corrosion has been shown in the past to be carried over into post-irradiation tests in autoclave environments, but its impact was shown in this study to be accentuated in the in-reactor environment, in which sustained corrosion accelerations were much greater than observed in the postirradiation tests (in non-irradiation environments). This suggests some aspect of the radiation environment potentially acts synergistically with the corrosion film formed from the irradiation-damaged base metal to further accelerate in-reactor corrosion rates. We also present results from detailed microstructural examinations of thick (more than 25 μm) oxide films formed on α-processed Zircaloy-4 grown in a 360 deg. C autoclave and in the reactor. The examinations consisted of optical microscopy, field emission gun scanning electron microscopy, focused ion beam microscopy, analytical electron microscopy, and X-ray diffraction, with a focus on the evolution of the microstructure of the intermetallic precipitates in the oxide films during exposure to autoclave water or to the corroding environment under neutron irradiation. The film microstructure suggests that the water environment was closer to the oxide-metal interface in the films grown in the reactor than in the autoclave-grown corrosion films examined, but it was not obvious from the microstructural examinations how the radiation environment facilitated that effect. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2020

Microstructural characterization of phase-separated co-deposited Cu–Ta immiscible alloy thin films

Elevated temperature co-sputtering of immiscible elements ends in a variety of self-organized morphologies due to phase separation. Cu–Ta is used as a model system to understand the evolution of phase-separated microstructural morphologies by co-sputtering thin films with nominal 50–50 at.% composition at four temperatures: 25, 400, 600, and 800 °C. Scanning/transmission electron microscopy of the film cross sections showed the microstructure morphology varied from nanocrystalline Cu–Ta at 25 °C to a wavy ribbon-like structure at 400 °C, to Cu-rich agglomerates surrounded by Ta-rich veins at 600 and 800 °C. In the agglomerate-vein morphology, microstructural features were present on two length scales, from a few nanometers to a few tens of nanometers, thus making the structures hierarchical. On the nanoscale, the Cu-rich agglomerates contained Ta precipitates, whereas the Ta-rich veins had embedded Cu nanocrystals. The various microstructures can be attributed to the highly disparate constituent element interdiffusion at the deposition temperatures with the Cu having orders of magnitude higher mobility than Ta at the deposition temperatures. This research of processing–microstructure relationship will be useful in guiding the design of hierarchical multiphase microstructures in binary or multicomponent thin films with tailored mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Impact of processing conditions on the film formation of lead-free halide double perovskite Cs 2 AgBiBr 6

Lead-free halide double perovskites with enhanced stability have gained attention as a promising environmentally friendly alternative to lead-based halide perovskites. Amongst different halide double perovskites, Cs 2 AgBiBr 6 has shown attractive optoelectronic properties and stability, making it a promising candidate for stable high-efficiency optoelectronic devices. Motivated by a data mining effort, we present here in this study the effects of different processing strategies on the microstructure and thin-film formation dynamics of Cs 2 AgBiBr 6 . We apply some of the most successfully used solvent engineering approaches from the halide perovskite research to halide double perovskites, namely antisolvent- and additive-assisted synthesis. Using in situ spectroscopy and diffraction, the film formation of Cs 2 AgBiBr 6 is investigated during spin coating, and the subsequent post-deposition thermal annealing. Dropping antisolvents during spin coating induces immediate supersaturation and crystallization of the wet film, whereas the time of dropping the antisolvent has implications on the film formation dynamics and the final microstructure. For additive (HBr)-assisted synthesis, we show how the addition of HBr affects colloid formation in solution and thus influences the crystallization pathway during thin-film processing. Finally, HBr additive simplifies synthesis in that it doesn't require solution and substrate preheating to obtain pinhole-free films even with higher thickness.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Microstructural Evolution and ORR Activity of Nanocolumnar Platinum Thin Films with Different Mass Loadings Grown by High Pressure Sputtering

Nanocolumnar platinum thin films (Pt-TFs) with different Pt mass loadings were grown by high pressure sputtering (HIPS) and investigated as oxygen reduction reaction (ORR) electrocatalysts for polymer electrolyte membrane fuel cell applications. Mass loading was controlled by changing the sputter deposition time. A cauliflower-like columnar microstructure was achieved by depositing the Pt-TFs onto a microporous layer (MPL)-like surface composed of carbon particles in order to mimic catalyst-coated gas diffusion electrodes. Microstructural evolution of HIPS Pt-TFs and their ORR activity were investigated. Electrochemical characterization of the nanocolumnar Pt-TFs was performed by cyclic voltammetry and rotating disk electrode measurements on Pt-TF/MPL-like-layer/glassy-carbon samples in an aqueous perchloric acid electrolyte. The electrochemically active surface area increased from 18 to 39 m 2 g –1 as the Pt mass loading was decreased. Specific activity of the films was similar (~600 μA cm –2 ) for all Pt mass loadings, due to the similar nanoparticle sizes of ~5 nm as observed by transmission electron microscopy and X-ray diffraction. Furthermore, mass activity of the films increased from 0.11 to 0.26 A mg –1 as the Pt mass loading was decreased, which is an indication of the effective Pt utilization and better access through the catalyst layer at lower Pt mass loadings.

08 HYDROGEN↗
DOE OSTI2014

Investigations of stochastic resonance in two-terminal device with vanadium dioxide film

The results of stochastic resonance investigation in a nonlinear system, consisting of a microstructure with a polycrystalline vanadium dioxide (VO{sub 2}) film grown on sapphire and resistor in series are reported. Nonlinearity of the system was provided due to insulator-metal phase transition in VO{sub 2}. In the stochastic resonance regime at 100 Hz signal frequency, the transition coefficient of signal-to-noise ratio reached 87 in contrast to 250 for microstructures with VO{sub 2} films grown on silica in our previous investigations. The measured characteristics of microstructures with VO{sub 2} films grown on silica and sapphire substrates were found to be qualitatively similar. For both substrates, a stochastic resonance was observed at threshold switching voltage from insulating to metallic state of VO{sub 2}. For sapphire substrate the output signal-to-noise ratio rose at higher signal frequencies. The stochastic resonance phenomenon in VO{sub 2} films is explained in terms of the monostable damped oscillator model.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Influence of the substrate temperature on the microstructure and electron-induced secondary electron emission properties of MgO/Au composite film

Highlights: • MgO/Au film was prepared by magnetron sputtering of individual Mg and Au targets. • A higher substrate temperature (T{sub s}) is conducive to the growth of MgO grains. • The surface roughness firstly rises and then decreases with T{sub s} increasing. • The increase of T{sub s} greatly enhances the SEE coefficient of the composite film. - Abstract: The influence of the substrate temperature (T{sub s}) on the microstructure and electron-induced secondary electron emission (SEE) properties of MgO/Au composite film prepared by reactive magnetron sputtering was investigated in order to improve the SEE performance of this composite film. During the deposition of MgO/Au film, a relatively high T{sub s} is conducive to the growth of MgO grains and causes the formation of some large aggregated gold particles on which MgO grains cover in the composite film. In terms of the SEE properties of MgO/Au film, the increase of T{sub s} brings about a significant improvement of SEE coefficient (δ), while it also leads to a slightly accelerated SEE degradation under the continuous electron bombardment due to a faster surface charging. The MgO/Au film prepared at T{sub s} of 773 K has a δ value of 4.9 at a primary electron energy of 200 eV and the maximum δ value of 11.5.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Microstructure and magnetic properties of ultrathin FePt granular films

FePt granular films with grain size smaller than 10 nm are promising candidates for storage media used in the next generation heat-assisted magnetic recording technology. However, FePt films show degraded magnetic properties when the grain size is reduced to this scale, which cannot be explained solely by the finite size theory. In this study, we explored the structural cause of property degradation by employing advanced electron microscopy and atomistic modeling. Structural features unique to the nanostructured FePt granular films at significantly reduced grain sizes of 2~8 nm were studied by high-resolution scanning transmission electron microscopy with geometric aberrations corrected up to the third order. Two critical structural parameters, the threshold grain size corresponding to the upper size limit of the FePt grains with zero chemical ordering and the sub-nanometer thin interfacial impurity at grain boundaries, were identified. A new atomistic model was developed to correlate these structural characteristics with key magnetic properties such as Curie temperature, saturation magnetization, magnetocrystalline anisotropy, and their grain-to-grain variation. The model shows good agreement with the experimental magnetic data and explains the gap in magnetic properties between the bulk and nanostructured FePt.

36 MATERIALS SCIENCE↗