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At least 1,081 records · Page 60
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Characterization of high-temperature mechanical properties of plasma-cladded coatings with thermo-mechanical coupling

High temperature mechanical properties was detected here to study the failure and strengthening mechanism of the coating-substrate (cobalt-based coatings were fabricated on FV520B substrate) integral structure with thermo-mechanical coupling effects. Microstructure, phase composition, element distribution of the coatings was characterized by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscope (TEM), electron back scattering diffraction (EBSD), X-ray diffraction (XRD), electron probe microanalysis (EPMA) and energy dispersive X-ray analysis (EDS). Results elucidate that fracture occurs in the coating for Co50 coating-substrate structure from 300 °C to 700 °C, but failure position transfer to substrate from coating at elevated temperatures with the addition of niobium and cerium oxide. Throughout, there is no crack originated from the interface. Fracture mechanism: the dislocation pile-up causes great stress concentration in the grain boundary, which results in the nucleation of the crack, and then the crack extends along the hard brittle Fe-Cr phase until the material fails. HRTEM shows the high density dislocation and the severe lattice distortion was formed during tensile deformation. On the macro level, the fracture tends to occur in the coarse dendrites region.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Embedded Ge nanocrystals in SiO{sub 2} synthesized by ion implantation

200 nm thick SiO{sub 2} layers grown on Si substrates were implanted with 150 keV Ge ions at three different fluences. As-implanted samples were characterized with time-of-flight secondary ion mass spectrometry and Rutherford backscattering spectrometry to obtain depth profiles and concentration of Ge ions. As-implanted samples were annealed at 950 °C for 30 min. Crystalline quality of pristine, as-implanted, and annealed samples was investigated using Raman scattering measurements and the results were compared. Crystalline structure of as-implanted and annealed samples of embedded Ge into SiO{sub 2} matrix was studied using x-ray diffraction. No secondary phase or alloy formation of Ge was detected with x-ray diffraction or Raman measurements. Scanning transmission electron microscope measurements were done to get the nanocrystal size and localized information. The results confirmed that fluence dependent Ge nanocrystals of different sizes are formed in the annealed samples. It is also observed that Ge is slowly diffusing deeper into the substrate with annealing.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Fractal analysis of Mo and Nb effects on grain boundary character and hot cracking behavior for Ni-Cr-Fe alloys

Highlights: • Cross section of the weld with lower RHGB fractal dimension exhibited higher DDC susceptibility than the surface section. • Mo and Nb addition induced tortuous GB character to increase fractal dimension and improve cracking resistance. • GROD maps indicated that the local strain increased within the grains close to RGBs till cracking. • At 1050 °C deformation recrystallized grains nucleated adjacent to DDC and blocked the crack propagation. - Abstract: In this paper, two filler metals of alloy 690 were evaluated on their hot cracking resistance based on the fractal analysis of random high-angle grain boundary (RHGB) morphologies. A grain reference orientation deviation (GROD) map based on EBSD technique was conducted to investigate the polycrystalline strain distribution on different RHGB network. It was found that for the 52M weld metal, specimen from the cross section with straight dendritic GBs exhibited lower fractal dimension, showing higher DDC susceptibility than the specimen from the surface section with higher fractal dimension due to equiaxed grains with tortuous GBs. With Mo and more Nb adding to the filler metal 52MSS, smaller grains nucleated and fractal dimension of the RHGB network increased, thus the cracking resistance was greatly improved. The GROD results revealed that local strain commonly concentrated around RHGB at high temperatures, especially near long and straight RHGB. The dense and tortuous RHGB network, resulting in the higher fractal dimension, could bear a more uniform strain distribution and balance the deformation between GB and grains, leading to better performance on cracking resistance. Moreover, dynamic recrystallized grains were observed beside GBs and their amount increases where there was cracking at 1050 °C, especially for the 52MSS. As a result, crack propagation path was blocked and fractal dimension increased as well.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Assessment of diagenesis in archaeological human second metacarpal bones using the intensity of the small angle X-ray scattering D -period peak

Bone consists mainly of carbonated apatite (cAp) nanoplatelets embedded in a matrix of collagen fibrils. Earlier, high-energy small angle X-ray scattering (SAXS) studies of archaeological adult human second metacarpal bones (mc2) found collagen D-period peaks with high-intensity I D in specimens in which microcomputed tomography (microCT) showed little diagenesis and I D ~ 0 for specimens where microCT revealed severe diagenesis (Park et al. 2022 Int. J. Osteoarchaeol. 32, 170–181 (doi:10.1002/oa.3053); Stock et al. 2022 Int. J. Osteoarchaeol. 32, 120–131 (doi:10.1002/oa.3049)). Here, the present paper uses SAXS at beamline 1-ID, Advanced Photon Source, Argonne National Laboratory and other techniques to study a set of 10 mc2 from an early Medieval cemetery at Greding, Germany. We hypothesized that non-invasive measurement of I D would provide an accurate and rapid (approx. 6 min/specimen) assessment of diagenesis in archaeological mc2. Results of Raman spectroscopy, laboratory microCT and backscattered electron, reflected light and polarized transmitted light microscopies confirmed the SAXS determinations, but lattice parameter values from X-ray diffraction were uncorrelated with I D value. Age-at-death estimates placed the 10 mc2 in three age categories (young adult, middle adult, old adult): lattice parameters from X-ray diffraction were uncorrelated with age at death. Cross-sectional bone area fraction from microCT dropped noticeably for the older age cohort.

Raman spectroscopy↗
DOE OSTI2012

Structural and electrical studies of ultrathin layers with Si{sub 0.7}Ge{sub 0.3} nanocrystals confined in a SiGe/SiO{sub 2} superlattice

In this work, SiGe/SiO{sub 2} multi-layer (ML) films with layer thickness in the range of a few nanometers were successfully fabricated by conventional RF-magnetron sputtering at 350 deg. C. The influence of the annealing treatment on SiGe nanocrystals (NCs) formation and crystalline properties were investigated by Raman spectroscopy and grazing incidence x-ray diffraction. At the annealing temperature of 800 deg. C, where well defined SiGe NCs were observed, a thorough structural investigation of the whole ML structure has been undertaken by Rutherford backscattering spectroscopy, grazing incidence small angle x-ray scattering, high resolution transmission electron microscopy, and annular dark field scanning transmission electron microscopy. Our results show that the onset of local modifications to the ML composition takes place at this temperature for annealing times of the order of a few tens of minutes with the formation of defective regions in the upper portion of the ML structure. Only the very first layers over the Si substrate appear immune to this problem. This finding has been exploited for the fabrication of a defect free metal-oxide-semiconductor structure with a well-defined single layer of SiGe NCs. A memory effect attributed to the presence of the SiGe NCs has been demonstrated by high frequency capacitance-voltage measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Influence of crystal mosaicity on axial channeling effects and lattice site determination of impurities

Using the electron emission channeling and Rutherford backscattering/channeling techniques, the influence of the mosaicity of a thin film on the axial channeling of charged particles was investigated. It is found that crystal mosaicity leads to a broadening and a degradation of the experimental channeling effects. This phenomenon, which is shown to be of major importance when assessing the lattice site of impurities in a single crystal, can be modeled quantitatively by using the mosaic tilt and twist components derived from X-ray rocking curve scans. As a case study, we illustrate that our approach allows to accurately determine the lattice site of Er in AlN, despite the significant influence of mosaicity on the channeling measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2012

RBS, XRR and optical reflectivity measurements of Ti-TiO{sub 2} thin films deposited by magnetron sputtering

Highlights: Black-Right-Pointing-Pointer The single-, bi- and tri-layered films of Ti-TiO{sub 2} deposited onto Si(1 1 1) substrates. Black-Right-Pointing-Pointer Three methods RBS, XRR, optical reflectometer were used. Black-Right-Pointing-Pointer The real thickness of each layer was smaller than 50 nm. Black-Right-Pointing-Pointer Ti and TiO{sub 2} film-densities were slightly lower than the corresponding bulk values. -- Abstract: Single-, bi- and tri-layered films of Ti-TiO{sub 2} system were deposited by d.c. pulsed magnetron sputtering from metallic Ti target in an inert Ar or reactive Ar + O{sub 2} atmosphere. The nominal thickness of each layer was 50 nm. The chemical composition and its depth profile were determined by Rutherford backscattering spectroscopy (RBS). Crystallographic structure was analysed by means of X-ray diffraction (XRD) at glancing incidence. X-ray reflectometry (XRR) was used as a complementary method for the film thickness and density evaluation. Modelling of the optical reflectivity spectra of Ti-TiO{sub 2} thin films deposited onto Si(1 1 1) substrates provided an independent estimate of the layer thickness. The combined analysis of RBS, XRR and reflectivity spectra indicated the real thickness of each layer less than 50 nm with TiO{sub 2} film density slightly lower than the corresponding bulk value. Scanning Electron Microscopy (SEM) cross-sectional images revealed the columnar growth of TiO{sub 2} layers. Thickness estimated directly from SEM studies was found to be in a good agreement with the results of RBS, XRR and reflectivity spectra.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Important role of the non-uniform Fe distribution for the ferromagnetism in group-IV-based ferromagnetic semiconductor GeFe

We investigate the growth-temperature dependence of the properties of the group-IV-based ferromagnetic semiconductor Ge{sub 1−x}Fe{sub x} films (x = 6.5% and 10.5%), and reveal the correlation of the magnetic properties with the lattice constant, Curie temperature (T{sub C}), non-uniformity of Fe atoms, stacking-fault defects, and Fe-atom locations. While T{sub C} strongly depends on the growth temperature, we find a universal relationship between T{sub C} and the lattice constant, which does not depend on the Fe content x. By using the spatially resolved transmission-electron diffractions combined with the energy-dispersive X-ray spectroscopy, we find that the density of the stacking-fault defects and the non-uniformity of the Fe concentration are correlated with T{sub C}. Meanwhile, by using the channeling Rutherford backscattering and particle-induced X-ray emission measurements, we clarify that about 15% of the Fe atoms exist on the tetrahedral interstitial sites in the Ge{sub 0.935}Fe{sub 0.065} lattice and that the substitutional Fe concentration is not correlated with T{sub C}. Considering these results, we conclude that the non-uniformity of the Fe concentration plays an important role in determining the ferromagnetic properties of GeFe.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Strain rate sensitivity, microstructure variations, and stress-assisted β → α" phase transformation investigation on the mechanical behavior of dual-phase titanium alloys

In this study, the microstructures of three widely used dual-phase titanium alloys: Ti-6Al-4V, Ti-6Al-2Sn-4Zr-2Mo, and Ti-6Al-2Sn-4Zr-6Mo are characterized using backscatter electron imaging and the deformation behaviors in their individual α and β phases are investigated using in situ high-energy X-ray diffraction during uniaxial tension experiments. This is accompanied by calculation of the strain rate sensitivity (SRS) in these alloys, as a function of applied loading. The results of the calculated SRS and the mechanical response (in terms of lattice strains and hardening behaviors) are rationalized based on the local microstructure, composition, and texture of the alloy. A stress-induced β (BCC) to α" (orthorhombic) phase transformation is observed during the in-situ diffraction experiment, which permitted analysis of the lattice strain evolution during the phase transformation. Results from this study provide insights into the relationship between microstructure, composition, applied loading, and the deformation behavior, including effects on loading with time holds. Specifically, the results show that the microstructure, and not necessarily the chemical composition (Mo content), along with the applied loading have a dominant role in the observed SRS variation in titanium alloys. Further, the evolution of the α" (orthorhombic) phase is observed for the first time during deformation of an industrially relevant titanium alloy, Ti-6246.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Molecular beam epitaxy growth and characterization of GePb alloys

Pb based group-IV alloys such as GePb have been gaining interest as a potential alternative for infrared detectors, quantum materials, and high-speed electronic devices. Challenges remain in their growth due to the extremely low solid solubility of Pb in the Ge–Pb system. This paper reports molecular beam epitaxy growth of GePb alloy thin films on Ge(100) substrates. Effusion cells of Ge and Pb are used to control the flux ratio independently. The optimal substrate temperature is found to be near the thermocouple temperature of 300 °C based on the characterization of the grown films using high-resolution x-ray diffraction. A large change in the Ge:Pb beam equivalent pressure ratio from 10:1 to 1:1 results in only a minimal increase of the Pb composition from 0.74% to 2.84% as estimated from Raman spectroscopy and Rutherford backscattering spectrometry. Furthermore, scanning electron microscopy images show a large volume of Pb islands on the surface that form into either long trapezoidal rods or uniform droplets, with increasing Pb flux and growth time the density of Pb islands increased.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Lattice modification in KTiOPO{sub 4} by hydrogen and helium sequentially implantation in submicrometer depth

We investigated lattice modification and its physical mechanism in H and He co-implanted, z-cut potassium titanyl phosphate (KTiOPO{sub 4}). The samples were implanted with 110 keV H and 190 keV He, both to a fluence of 4 × 10{sup 16 }cm{sup −2}, at room temperature. Rutherford backscattering/channeling, high-resolution x-ray diffraction, and transmission electron microscopy were used to examine the implantation-induced structural changes and strain. Experimental and simulated x-ray diffraction results show that the strain in the implanted KTiOPO{sub 4} crystal is caused by interstitial atoms. The strain and stress are anisotropic and depend on the crystal's orientation. Transmission electron microscopy studies indicate that ion implantation produces many dislocations in the as-implanted samples. Annealing can induce ion aggregation to form nanobubbles, but plastic deformation and ion out-diffusion prevent the KTiOPO{sub 4} surface from blistering.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Crystallographic and magnetic identification of secondary phase in orientated Bi{sub 5}Fe{sub 0.5}Co{sub 0.5}Ti{sub 3}O{sub 15} ceramics

The fabrication of highly-oriented polycrystalline ceramics of Bi{sub 5}Fe{sub 0.5}Co{sub 0.5}Ti{sub 3}O{sub 15}, prepared via molten salt synthesis and uniaxial pressing of high aspect ratio platelets is reported. Electron backscatter images show a secondary phase within the ceramic which is rich in cobalt and iron. The concentration of the secondary phase obtained from scanning electron microscopy is estimated at less than 2% by volume, below the detection limit of x-ray diffraction (XRD). The samples were characterized by x-ray diffraction, polarization-electric field measurements, superconducting quantum interference device as a function of sample orientation and vibrating sample magnetometry as a function of temperature. It is inferred from the data that the observed ferromagnetic response is dominated by the secondary phase. This work highlights the importance of rigorous materials characterisation in the study of multiferroics as small amounts of secondary phase, below the limit of XRD, can lead to false conclusions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Micro- and nano-structural evolutions in white Portland cement/pulverized fuel ash cement pastes due to deionized-water leaching

Thin slices of white Portland cement-low calcium pulverized fuel ash (pfa) blended cement pastes containing 30 or 50% pfa were leached progressively in de-ionized water. The paste with 50% pfa was aged 13 years prior to leaching and those with 30% pfa were aged 1 and 13 years. Pastes were leached for up to 75 days and were characterized using thermal analysis, X-ray diffraction, analytical scanning and transmission electron microscopy, and solid-state nuclear magnetic resonance spectroscopy. Leaching affected the pastes in the following sequence: (i) crystals of Ca(OH){sub 2} large enough to be resolved by backscattered electron imaging were removed completely prior to any effect on C-A-S-H; (ii) the Ca/Si ratio of C-A-S-H reduced from ≈ 1.4 to ≈ 1.0 whilst the aluminosilicate structure was unaffected; (iii) further reduction in the Ca/Si ratio of C-A-S-H was accompanied by lengthening of the aluminosilicate chains; (iv) the Ca/Si ratio of C-A-S-H reduced ultimately to ≈ 0.6.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Defect structure of epitaxial CrxV1-x thin films on MgO(001)

Epitaxial thin films of CrxV1-x over the entire composition range were deposited on MgO(001) by molecular beam epitaxy. The films exhibited the expected 45° in-plane rotation with no evidence of phase segregation or spinodal decomposition. Pure Cr, with the largest lattice mismatch to MgO, exhibited full relaxation and cubic lattice parameters. As the lattice mismatch decreased with alloy composition, residual epitaxial strain was observed. For 0.2 ≤ x ≤ 0.4 the films were coherently strained to the substrate with associated tetragonal distortion; near the lattice-matched composition of x = 0.33, the films exhibited strain-free pseudomorphic matching to MgO. Unusually, films on the Cr-rich side of the lattice-matched composition exhibited more in-plane compression than expected from the bulk lattice parameters; this result was confirmed with both x-ray diffraction and Rutherford backscattering spectrometry channeling measurements. Although thermal expansion mismatch in the heterostructure may play a role, the dominant mechanism for this phenomenon is still unknown. High resolution transmission electron microscopy was utilized to characterize the misfit dislocation network present at the film/MgO interface. Dislocations were found to be present with a non-uniform distribution, which is attributed to the Volmer-Weber growth mode of the films. The CrxV1-x / MgO(001) system can serve as a model system to study both the fundamentals of defect formation in bcc films and the interplay between nanoscale defects such as dislocations and radiation damage.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Enhanced electrical and noise properties of nanocomposite vanadium oxide thin films by reactive pulsed-dc magnetron sputtering

Thin films of VO{sub x} (1.3 {<=} x {<=} 2) were deposited by reactive pulsed-dc magnetron sputtering of a vanadium metal target while RF-biasing the substrate. Rutherford back scattering, glancing angle x-ray, and cross-sectional transmission electron microscopy measurements revealed the formation of nanocolumns with nanotwins within VO{sub x} samples. The resistivity of nanotwinned VO{sub x} films ranged from 4 m{Omega}{center_dot}cm to 0.6 {Omega}{center_dot}cm and corresponding temperature coefficient of resistance between -0.1% and -2.6% per K, respectively. The 1/f electrical noise was analyzed in these VO{sub x} samples using the Hooge-Vandamme relation. These VO{sub x} films are comparable or surpass commercial VO{sub x} films deposited by ion beam sputtering.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Molecular beam epitaxy growth and optoelectronic properties of droplet-free lattice-matched GaInAsSbBi on GaSb with wavelength extension exceeding 5 μ m

GaInAsSbBi alloys are grown lattice-matched on GaSb by molecular beam epitaxy demonstrating smooth surface morphologies, >5 μm wavelength photoluminescence emission, and minority carrier lifetimes >1 μs. At a growth temperature of 400 °C, the Ga flux is systematically increased and the Bi flux systematically decreased to identify GaInAsSbBi growth conditions that yield smooth droplet-free surface morphologies. The minority carrier lifetime is evaluated using time-resolved photoluminescence, where it is observed that GaInAsSbBi samples exhibit minority carrier lifetimes comparable to their Bi-free GaInAsSb counterparts, on the order of 1.5–2 μs. The bandgap and Urbach energy are evaluated from steady-state photoluminescence to gain insight into the impact of the incorporated Bi. Coupled with Rutherford backscattering spectrometry measurements of the Bi mole fraction, bandgap reduction rates of 97 meV/% Bi in InAsSbBi and 150 meV/% Bi in GaInAsSbBi are observed, significantly higher than previous evaluations in InAsSbBi (35–55 meV/% Bi). Detailed comparisons of the Bi mole fraction, bandgap energy, and Urbach energy indicate that the bandgap reduction potential in this alloy system is inhibited by the formation of Bi clusters; however, the inclusion of Ga in the quinary alloy is effective in suppressing Bi's tendency to incorporate in clusters for Ga mole fractions >9%, maximizing the bandgap reduction per unit Bi and overall optoelectronic quality.

Atomic force microscopy↗
NASA NTRS1992

Synthesis and characterization of fine grain diamond films

A fine grain diamond film has been developed by microwave plasma assisted chemical vapor deposition. Various analytical techniques, including Rutherford backscattering, proton recoil analysis, Raman spectroscopy, and X-ray diffraction, were utilized to characterize the diamond films. The grain size of the film was determined from bright and dark field electron micrographs, and found to be 200-1000 A. The films exhibited good optical transmission between 2.5 and 10 microns, with a calculated absorption coefficient of 490/cm. The friction coefficients of this film were found to be 0.035 and 0.030 at dry nitrogen and humid air environments, respectively, and the films had low wear rates.

Wu, Richard L. C.↗