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At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Microstructural evolution of thin polycrystalline metallic films under extreme conditions

Thin films are materials systems that are widely used in applications ranging from electronics and optical devices to industrial and biomedical ones. However, these systems are unstable against various homogenization processes and aging mechanisms (grain growth, coarsening, surface evolution, and diffusion of species) even at low service temperatures. In this work, we examine the role of various aspects of microstructure (grain boundary types and characters, free surfaces, surface diffusion, and thermal grooves) on the thermal aging of such systems. Existing experimental tools will be leveraged to characterize thin films, i.e., in-situ quantitative thermal annealing, and provide direct comparisons to predications emerging from a recently developed meso-scale model via Precession Electron Diffraction (PED). Parametric studies will be conducted to gain insights on the role of each of the aforementioned aspects of microstructure on the dynamics. Herein, we will focus on “hard” gold thin films (with alloying elements like Co, Ni, or Fe) as they are materials of choice in a wide range of applications at Sandia. Initially, pure gold systems are examined and future studies will focus on microstructure evolution in the presence of alloying elements and second-phase particles.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructures, mechanical behavior and strengthening mechanism of TiSiCN nanocomposite films

Recently, the arguments have existed in the strengthening mechanism and microstructural model of the nanocomposite film due to lack of the convincible experimental evidences. In this investigation, the quarternary TiSiCN nanocomposite films with the different C and Si contents are synthesized by the reactive-magnetron-sputtering technique. The TiSiCN film is characterized as the nanocomposite structure with the TiN nanocrystallites surrounded by the (Si 3 N 4 + C + CN x ) interface phase. When the C/Si content ratio is 2:2, the TiSiCN nanocomposite film is remarkably strengthened with the maximal hardness and elastic modulus of 46.1 GPa and 425 GPa, respectively. Meanwhile, the (Si 3 N 4 + C + CN x ) interfaces exhibit as a crystallized form, which can coordinate the growth misorientations and maintain the coherently epitaxial growth between the TiN nanocrystallites and interfaces. Through the high-resolution transmission electron microscopy (HRTEM) observations, this investigation firstly provides the direct experimental evidence for the crystallized feature of the interfaces when the TiSiCN nanocomposite film is strengthened, suggesting that the strengthening effect of the TiSiCN nanocomposite film can be attributed to the coherent-interface strengthening mechanism, which is expressed as the “nc-TiN/c-Si 3 N 4 /c-C/c-CN x ” model.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Role of microstructure and doping on the mechanical strength and toughness of polysilicon thin films

We investigated the role of microstructure and doping on the mechanical strength of microscale tension specimens of columnar grain and laminated polysilicon doped with different concentrations of phosphorus. The average tensile strengths of undoped columnar and laminated polysilicon specimens were 1.3 ± 0.1 and 2.45 ± 0.3 GPa, respectively. Heavy doping reduced the strength of columnar polysilicon specimens to 0.9 ± 0.1 GPa. On grounds of Weibull statistics, the experimental results from specimens with gauge sections of 1000 μm × 100 μm × 1 μm predicted quite well the tensile strength of specimens with gauge sections of 150 μm × 3.75 μm × 1 μm, and vice versa. The large difference in the mechanical strength between columnar and laminated polysilicon specimens was due to sidewall flaws in columnar polysilicon, which were introduced during reactive ion etching (RIE) and were further exacerbated by phosphorus doping. Moreover, the removal of the large defect regions at the sidewalls of columnar polysilicon specimens via ion milling increased their tensile strength by 70%-100%, approaching the strength of laminated polysilicon, which implies that the two types of polysilicon films have comparable tensile strength. Measurements of the effective mode I critical stress intensity factor, KIC,eff, also showed that all types of polysilicon films had comparable resistance to fracture. Therefore, additional processing steps to eliminate the edge flaws in RIE patterned devices could result in significantly stronger microelectromechanical system components fabricated by conventional columnar polysilicon films.

42 ENGINEERING↗
DOE OSTI2015

Nano-indentation of single-layer optical oxide thin films grown by electron-beam deposition

Mechanical characterization of optical oxide thin films is performed using nano-indentation, and the results are explained based on the deposition conditions used. These oxide films are generally deposited to have a porous microstructure that optimizes laser induced damage thresholds, but changes in deposition conditions lead to varying degrees of porosity, density, and possibly the microstructure of the thin film. This can directly explain the differences in the mechanical properties of the film studied here and those reported in literature. Of the four single-layer thin films tested, alumina was observed to demonstrate the highest values of nano-indentation hardness and elastic modulus. This is likely a result of the dense microstructure of the thin film arising from the particular deposition conditions used.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Superconducting properties of Nb-Cu nano-composites and nano-alloys

The evolution of the superconducting transition temperature (T{sub c}) in nano-composite and nano-alloys of Nb-Cu, grown by DC magnetron co-sputtering are investigated. Microstructure of these films depends less strongly on the ratio of Nb:Cu but more on the growth temperature. At higher growth temperature, phase separated granular films of Nb and Cu were formed which showed superconducting transition temperatures (T{sub c}) of ~ 7.2±0.5 K, irrespective of the composition. Our results show that this is primarily influenced by the microstructure of the films determined during growth which rules out the superconducting proximity effect expected in these systems. At room temperature growth, films with nano-scale alloying were obtained at the optimal compositional range of 45-70 atomic% (At%) of Nb. These were also superconducting with a T{sub c} of 3.2 K.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2017

Microstructural evolution of ion-irradiated sol–gel-derived thin films

In this paper, the effects of ion irradiation on the microstructural evolution of sol–gel-derived silica-based thin films were examined by combining the results from Fourier transform infrared, Raman, and X-ray photoelectron spectroscopy, Rutherford backscattering spectrometry, and elastic recoil detection. Variations in the chemical composition, density, and structure of the constituent phases and interfaces were studied, and the results were used to propose a microstructural model for the irradiated films. It was discovered that the microstructure of the films after ion irradiation and decomposition of the starting organic materials consisted of isolated hydrogenated amorphous carbon clusters within an amorphous and carbon-incorporated silica network. A decrease in the bond angle of Si–O–Si bonds in amorphous silica network along with an increase in the concentration of carbon-rich SiO x C y tetrahedra were the major structural changes caused by ion irradiation. Finally, in addition, hydrogen release from free carbon clusters was observed with increasing ion energy and fluence.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Texture evolution in nanocrystalline iron films deposited using biased magnetron sputtering

Fe thin films were deposited on sodium chloride (NaCl) substrates using magnetron sputtering to investigate means of texture control in free standing metal films. The Fe thin films were studied using transmission electron microscopy equipped with automated crystallographic orientation microscopy. Using this technique, the microstructure of each film was characterized in order to elucidate the effects of altering deposition parameters. The natural tendency for Fe films grown on (100) NaCl is to form a randomly oriented nanocrystalline microstructure. By careful selection of substrate and deposition conditions, it is possible to drive the texture of the film toward a single (100) orientation while retaining the nanocrystalline microstructure.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Femtosecond Laser Writing of Waveguide Microstructures in Pb(Zr,Ti)O{sub 3} Films and Their Characterization by the Nonlinear Optical Method

Femtosecond laser writing of ferroelectric one-dimensional microstructures possessing waveguide and nonlinear optical properties in Pb(Zr,Ti)O{sub 3} films is considered, and the passage of light beams via obtained waveguide structures is traced. The optimum speed and power density of the writing laser beam are within 50–500 μm/s and 1–1.5 MW/cm{sup 2}, respectively. A two-stage method of writing is proposed, which provides for improved nonlinear optical properties of obtained waveguide microstructures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

A leaf-molded transparent triboelectric nanogenerator for smart multifunctional applications

Transparent, flexible and highly efficient portable power sources are essential components of the next generation electronics and optoelectronic devices. However, complicated technology, expensive cost, environmental pollution and low-efficient output have limited its development. Herein, based on periodic contact/separation between human skin and the microstructured polydimethylsiloxane (PDMS) film, we demonstrate a transparent flexible triboelectric nanogenerator (TENG) through a relatively simple, low-cost, environmental-friendly and high-efficient method. For the first time, the natural leaves with rich surface textures were introduced to make microstructures on PDMS films as effective friction surface in the TENG. Furthermore, long silver nanowires (200 µm in length at least) through novel synthesis were assembled as high-performance electrode, resulting in the entirely flexible and transparent TENG. Owing to the unique design, the transparent flexible TENG was eventually obtained with an enhanced output (Voc=56 V; Isc=3.1 μA) and remarkable transparency (88%). Owing to compelling features of the TENG, a self-powered user-interactive wearable system was successfully established by integrating a flexible electrochromic device (ECD). The remarkable color-tunable ability via mechanical control of our system, highly inspired by chameleons, is potentially useful in military camouflage, monitoring human activity visually, as well as replacing performance of face change in Sichuan Opera. Therefore, this research is a substantial advancement toward the construction of transparent nanogenerator and its multifunctional applications in energy conversation, wearable electronics, healthcare, culture experience, and even environmental protection.

42 ENGINEERING↗
DOE OSTI2016

Microstructural and electrical properties of PVA/PVP polymer blend films doped with cupric sulphate

A series of polyvinyl alcohol (PVA)/polyvinyl pyrrolidone (PVP) polymer blends added with different concentrations of cupric sulphate (CuSO{sub 4}) were prepared by solution casting method and were subjected to X-ray diffraction (XRD) and Ac conductance measurements. An attempt has been made to study the changes in crystal imperfection parameters in PVA/PVP blend films with the increase in concentration of CuSO{sub 4}. Results show that decrease in micro crystalline parameter values is accompanied with increase in the amorphous content in the film which is the reason for film to have more flexibility, biodegradability and good ionic conductivity. AC conductance measurements in these films show that the conductivity increases as the concentration of CuSO{sub 4} increases. These films were suitable for electro chemical applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Microstructural, nanomechanical, and microtribological properties of Pb thin films prepared by pulsed laser deposition and thermal evaporation techniques

In this work, the authors compare the morphological, structural, nanomechanical, and microtribological properties of Pb films deposited by thermal evaporation (TE) and pulsed laser deposition (PLD) techniques onto Si (111) substrates. Films were investigated by scanning electron microscopy, surface probe microscopy, and x-ray diffraction in θ-2θ geometry to determine their morphology, root-mean-square (RMS) roughness, and microstructure, respectively. TE films showed a percolated morphology with densely packed fibrous grains while PLD films had a granular morphology with a columnar and tightly packed structure in accordance with the zone growth model of Thornton. Moreover, PLD films presented a more polycrystalline structure with respect to TE films, with RMS roughness of 14 and 10 nm, respectively. Hardness and elastic modulus vary from 2.1 to 0.8 GPa and from 14 to 10 GPa for PLD and TE films, respectively. A reciprocal friction test has shown that PLD films have lower friction coefficient and wear rate than TE films. Our study has demonstrated for first time that, at the microscale, Pb films do not show the same simple lubricious properties measured at the macroscale.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Highly transparent Nb-doped indium oxide electrodes for organic solar cells

The authors investigated the characteristics of Nb-doped In{sub 2}O{sub 3} (INbO) films prepared by co-sputtering of Nb{sub 2}O{sub 5} and In{sub 2}O{sub 3} for use in transparent anodes for organic solar cells (OSCs). To optimize the Nb dopant composition in the In{sub 2}O{sub 3} matrix, the effect of the Nb doping power on the resistivity and transparency of the INbO films were examined. The electronic structure and microstructure of the INbO films were also investigated using synchrotron x-ray absorption spectroscopy and x-ray diffraction examinations in detail. At the optimized Nb co-sputtering power of 30 W, the INbO film exhibited a sheet resistance of 15 Ω/sq, and an optical transmittance of 86.04% at 550 nm, which are highly acceptable for the use as transparent electrodes in the fabrication of OSCs. More importantly, the comparable power conversion efficiency (3.34%) of the OSC with an INbO anode with that (3.31%) of an OSC with a commercial ITO anode indicates that INbO films are promising as a transparent electrode for high performance OSCs.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1987

A review of recent advances in solid film lubrication

Thin, adherent sputtered MoS2 and ion plated metallic (Au, Ag, Pb) lubricating films are primarily used in precision contacting triboelement surfaces where wear debris formation is critical and high reliability requirements have to be satisfied. Detailed structural and compositional characterization of solid film lubricants is of prime importance. It is this information from the nano-micro-macro level which is needed to interpret and improve the frictional behavior and assure long endurance lives. The purpose of this paper is to summarize in a concise review the solid lubricant film structure and morphology and their effects on the tribological properties of the lubricant systems. The tribological performance of thin lubricating films has significantly advanced through progressive understanding of the film parameters such as adhesion, cohesion, interface formation, nucleation and microstructural growth, critical film thickness and substrate finish, and temperature. Sputtered MoS2 and ion plated Au, Ag, and Pb films are separately discussed and evaluated in terms of the above film parameters to establish the most desirable film structures and thicknesses in order to achieve effective lubrication.

Spalvins, T.↗
DOE OSTI2017

Growth-Induced In-Plane Uniaxial Anisotropy in V 2 O 3 /Ni Films

We report on a strain-induced and temperature dependent uniaxial anisotropy in V 2 O 3 /Ni hybrid thin films, manifested through the interfacial strain and sample microstructure, and its consequences on the angular dependent magnetization reversal. X-ray diffraction and reciprocal space maps identify the in-plane crystalline axes of the V 2 O 3 ; atomic force and scanning electron microscopy reveal oriented rips in the film microstructure. Quasi-static magnetometry and dynamic ferromagnetic resonance measurements identify a uniaxial magnetic easy axis along the rips. Comparison with films grown on sapphire without rips shows a combined contribution from strain and microstructure in the V 2 O 3 /Ni films. Magnetization reversal characteristics captured by angular-dependent first order reversal curve measurements indicate a strong domain wall pinning along the direction orthogonal to the rips, inducing an angular-dependent change in the reversal mechanism. Lastly, the resultant anisotropy is tunable with temperature and is most pronounced at room temperature, which is beneficial for potential device applications.

36 MATERIALS SCIENCE↗
NASA NTRS1972

A study of the microstructure and optical properties of thin lead-dielectric cermet films

A transmission electron microscopy study involving direct and replicating techniques is directed to a definition of the microstructure of radio frequency-sputtered, thin lead-dielectric cermet films. Once defined, this microstructure is used to obtain theoretical film refractive indices. The Maxwell Garnett theory provides a basis for the theoretical results. Measurements of film transmission and reflectivity are used to obtain rough experimental values for film refractive indices by the Tekucheva method. More exact values are obtained via ellipsometry. The rough Tekucheva values are used to determine the range over which computer calculations interpreting the ellipsometric results must be made. This technique yields accurate values for the film refractive indices.

Owen, R. B.↗
DOE OSTI2014

Impact of composition and crystallization behavior of atomic layer deposited strontium titanate films on the resistive switching of Pt/STO/TiN devices

The resistive switching (RS) properties of strontium titanate (Sr{sub 1+x}Ti{sub 1+y}O{sub 3+(x+2y)}, STO) based metal-oxide-metal structures prepared from industrial compatible processes have been investigated focusing on the effects of composition, microstructure, and device size. Metastable perovskite STO films were prepared on Pt-coated Si substrates utilizing plasma-assisted atomic layer deposition (ALD) from cyclopentadienyl-based metal precursors and oxygen plasma at 350 °C, and a subsequent annealing at 600 °C in nitrogen. Films of 15 nm and 12 nm thickness with three different compositions [Sr]/([Sr] + [Ti]) of 0.57 (Sr-rich STO), 0.50 (stoichiometric STO), and 0.46 (Ti-rich STO) were integrated into Pt/STO/TiN crossbar structures with sizes ranging from 100 μm{sup 2} to 0.01 μm{sup 2}. Nano-structural characterizations revealed a clear effect of the composition of the as-deposited STO films on their crystallization behavior and thus on the final microstructures. Local current maps obtained by local-conductivity atomic force microscopy were in good agreement with local changes of the films' microstructures. Correspondingly, also the initial leakage currents of the Pt/STO/TiN devices were affected by the STO compositions and by the films' microstructures. An electroforming process set the Pt/STO/TiN devices into the ON-state, while the forming voltage decreased with increasing initial leakage current. After a RESET process under opposite voltage has been performed, the Pt/STO/TiN devices showed a stable bipolar RS behavior with non-linear current-voltage characteristics for the high (HRS) and the low (LRS) resistance states. The obtained switching polarity and nearly area independent LRS values agree with a filamentary character of the RS behavior according to the valence change mechanism. The devices of 0.01 μm{sup 2} size with a 12 nm polycrystalline stoichiometric STO film were switched at a current compliance of 50 μA with voltages of about ±1.0 V between resistance states of about 40 kΩ (LRS) and 1 MΩ (HRS). After identification of the influences of the films' microstructures, i.e., grain boundaries and small cracks, the remaining RS properties could be ascribed to the effect of the [Sr]/([Sr] + [Ti]) composition of the ALD STO thin films.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Impact of high-power impulse magnetron sputtering pulse width on the nucleation, crystallization, microstructure, and ferroelectric properties of hafnium oxide thin films

The impact of the high-power impulse magnetron sputtering (HiPIMS) pulse width on the crystallization, microstructure, and ferroelectric properties of undoped HfO 2 films is investigated. HfO 2 films were sputtered from a hafnium metal target in an Ar/O 2 atmosphere, varying the instantaneous power density by changing the HiPIMS pulse width with fixed time-averaged power and pulse frequency. The pulse width is shown to affect the ion-to-neutral ratio in the depositing species with the shortest pulse durations leading to the highest ion fraction. In situ x-ray diffraction measurements during crystallization demonstrate that the HiPIMS pulse width impacts nucleation and phase formation, with an intermediate pulse width of 110 μ s stabilizing the ferroelectric phase over the widest temperature range. Although the pulse width impacts the grain size with the lowest pulse width resulting in the largest grain size, the grain size does not strongly correlate with the phase content or ferroelectric behavior in these films. In conclusion, these results suggest that precise control over the energetics of the depositing species may be beneficial for forming the ferroelectric phase in this material.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Diamond synthesis at atmospheric pressure by microwave capillary plasma chemical vapor deposition

Polycrystalline diamond has been synthesized on silicon substrates at atmospheric pressure, using a microwave capillary plasma chemical vapor deposition technique. The CH{sub 4}/Ar plasma was generated inside of quartz capillary tubes using 2.45 GHz microwave excitation without adding H{sub 2} into the deposition gas chemistry. Electronically excited species of CN, C{sub 2}, Ar, N{sub 2}, CH, H{sub β}, and H{sub α} were observed in the emission spectra. Raman measurements of deposited material indicate the formation of well-crystallized diamond, as evidenced by the sharp T{sub 2g} phonon at 1333 cm{sup −1} peak relative to the Raman features of graphitic carbon. Field emission scanning electron microscopy images reveal that, depending on the growth conditions, the carbon microstructures of grown films exhibit “coral” and “cauliflower-like” morphologies or well-facetted diamond crystals with grain sizes ranging from 100 nm to 10 μm.

36 MATERIALS SCIENCE↗