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NASA NTRSDate not supplied

Characterizing Martian X-Ray Amorphous Materials Through Terrestrial Analogs

X-ray amorphous materials (i.e., lacking long-range crystallographic order) have been identified on the martian surface from orbit and in-situ. Initial models of orbital IR spectral data identified volcanic glasses [e.g., 1], but subsequent interpretations suggested that amorphous silicates are dominantly secondary in nature and formed from water-rock interactions [e.g., 2-4]. Thermal IR spectra from the Mini-Thermal Emission Spectrometer on the Spirit rover show evidence for the amorphous secondary product opaline silica [e.g., 5]. X-ray diffraction (XRD) measurements by the CheMin instrument on the Mars Science Laboratory rover have identified 20-70 wt.% amorphous materials in every sample analyzed in Gale crater to date [e.g., 6]. Mass balance calculations using CheMin results and bulk elemental measurements by the Alpha Particle X-ray Spectrometer suggest the amorphous component in Gale crater is variably enriched in Si, Fe, and S [e.g., 7,8]. The compositions are not consistent with pure volcanic glass, indicating water must have been involved in the formation of amorphous materials in Gale crater. We seek to better constrain the conditions under which amorphous materials on Mars formed by studying the composition and short-range atomic order of amorphous materials in terrestrial analog environments via XRD and transmission electron microscopy (TEM).

E B Rampe↗

NASA NTRSDate not supplied

High Resolution Imaging and Analysis of Terrestrial Impact Glass: Amorphous Materials, Phyllosilicates and Everything in Between

Introduction: Impact cratering is one of the most ubiquitous geologic processes shaping the surface of all solid bodies in our solar system. Impacts are also a major source of clay minerals, poorly crystalline clay-like phases and amorphous (i.e., lacking long-range atomic order) materials on Earth and Mars. Phyllosilicates and amorphous materials have consistently formed a major component (~20-70 wt%) of every single drilled rock and soil sample in Gale Crater on Mars, as determined by the CheMin instrument on Curiosity. The origin of the amorphous component is speculative, but could be primary impact or volcanic-produced glass(es) deposited via aeolian or fluvial processes, secondary aqueous alteration products or chemical precipitates; it is likely to be a combination of all three possibilities. Efforts to determine the composition of these materials across the rover’s traverse through Gale Crater are ongoing. Naturally occurring amorphous phases are found in a variety of environments on Earth, and terrestrial analogue studies may help shed light on how they may have formed on Mars. Primary and altered impact glass are likely widespread on Mars and may have contributed to the amorphous component found throughout Gale Crater. In its pristine, unaltered state, impact glass (i.e., melt glass) is considered amorphous. However, truly unaltered glass is rarely preserved in crater fill impactites as it quickly alters in the post-impact environ-ment, commonly forming a mixture of hydrated aluminosilicate phases whose structures are not always discernable at the microscale (i.e., they may be amorphous or contain short-range order). These phases are part of an incredibly complex group of materials; differences in their composition and crystalline structure (or lack thereof) and genetic relationship to the more well-crystalline clay minerals are often only discernable at the nanoscale, beyond the resolution of traditional X-ray diffractometers (XRD) and scanning electron microscopes/microprobes (SEM/EPMA) alone. In this contribution, we summarize recent results from ongoing characterization of clay minerals, poorly crystalline clay-like phases, and amorphous materials preserved in altered terrestrial impact glass from the Chicxulub (~66 Ma) and Ries (~15 Ma) impact structures. This work has been performed using a combination of high-resolution transmission electron microscopy (HR-TEM), SEM, microprobe/EPMA, Raman spectroscopy and XRD.

Impact crater↗

DOE OSTI2024

Method for electrochemical transformation of amorphous material to crystalline material

A method for converting amorphous boron nitride to crystalline boron nitride, the method comprising immersing the amorphous boron nitride into anhydrous molten magnesium chloride maintained within a temperature range of 720° C.-820° C. while the amorphous boron nitride is cathodically polarized at a voltage within a range of −2.2V to −2.8V for a period of time of at least 2 minutes to result in conversion of the amorphous boron nitride to the crystalline form. Also described herein is a method for converting an amorphous carbon material to a crystalline carbon material, the method comprising immersing said amorphous carbon material into anhydrous molten magnesium chloride maintained within a temperature range of 780° C.-820° C. while the amorphous carbon material is cathodically polarized at a voltage within a range of −2.2V to −2.8V for a period of time of at least 2 minutes to result in conversion of the amorphous carbon material to the crystalline form.

Bagri, Prashant↗

DOE OSTI2025

Pressure-driven density match nucleates metastable r8 phases from amorphous Si and Ge

The pressure–temperature phase behavior of covalent disordered solids such as amorphous silicon and germanium is complex. Questions remain on possible glass transitions, on polyamorphism via amorphous–amorphous transitions, on connections with liquid–liquid transitions, on structure-behavior relationships, and on their potential as precursor for novel methods for material discovery. Here we demonstrate experimentally the nucleation of a metastable, four-fold coordinated rhombohedral r8 phase from pure amorphous silicon and germanium upon room temperature compression at pressures below 10 GPa. Accompanying theory reveals a strong pressure-driven distortion of the bond angle transforming the starting tetrahedral low-density amorphous network to a distorted four-fold coordinated medium-density state. This state is of lower density than metallic high-density networks, resembles the crystalline r8 phase and initiates its nucleation. Our finding shows that polyamorphism is not the only possible transformation mode for these amorphous solids and that instead nucleation of interesting functional phases at potentially useful pressures is possible. Such novel access modes to metastable structures are critical for future exploitability and could be useful for other tetrahedral materials including carbon, where the related (bc8) post-diamond phase remains elusive. Our observed density match between an amorphous and a metastable crystalline phase clearly allows for a new phase transition pathway, while corresponding theory demonstrates how carefully validated atomistic simulations can guide prediction, discovery and synthesis of novel material structures.

Materials discovery↗

DOE OSTI2013

On the amorphization behavior and hydrogenation performance of high-energy ball-milled Mg{sub 2}Ni alloys

Amorphous Mg{sub 2}Ni alloy was prepared by high energy ball-milling starting with polycrystalline Mg{sub 2}Ni which was prepared with the help of a metallurgy method by using a SPEX 8000D mill. The microstructural and phase structure characterization of the prepared materials was performed via scanning electron microscopy, transition electron microscope and X-ray diffraction. The thermal stabilities were investigated by differential scanning calorimetry. The apparent activation energies were determined by means of the Kissinger method. The first and second crystallization reactions take place at ∼ 255 °C and ∼ 410 °C, and the corresponding activation energy of crystallization is E{sub a1} = 276.9 and E{sub a2} = 382.4 kJ/mol, respectively. At 3 MPa hydrogen pressure and 250 °C, the hydrogen absorption capacities of crystalline, partially and fully amorphous Mg{sub 2}Ni alloy are 2.0 wt.%, 3.2 wt.% and 3.5 wt.% within 30 min, respectively. - Graphical Abstract: We mainly focus on the amorphization behavior of crystalline Mg{sub 2}Ni alloy in the high energy ball-milling process and the crystallization behavior of the amorphous Mg{sub 2}Ni alloy in a follow-up heating process. The relationship of milling, microstructure and hydrogenation properties is established and explained by models. - Highlights: • Amorphous Mg{sub 2}Ni has been obtained by high energy ball milling the as-cast alloy. • The amorphization behavior of polycrystalline Mg{sub 2}Ni is presented. • The crystallization behavior of the amorphous Mg{sub 2}Ni alloy is illustrated. • Establish the relationship of milling, microstructure and hydrogenation properties.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Enhanced stability and local structure in biologically relevant amorphous materials containing pyrophosphate

There is increasing evidence that amorphous inorganic materials play a key role in biomineralisation in many organisms, however the inherent instability of synthetic analogues in the absence of the complex in vivo matrix limits their study and clinical exploitation. To address this, we report here an approach that enhances long-term stability to >1 year of biologically relevant amorphous metal phosphates, in the absence of any complex stabilizers, by utilizing pyrophosphates (P{sub 2}O{sub 7}{sup 4-}); species themselves ubiquitous in vivo. Ambient temperature precipitation reactions were employed to synthesise amorphous Ca{sub 2}P{sub 2}O{sub 7}.nH{sub 2}O and Sr{sub 2}P{sub 2}O{sub 7}.nH{sub 2}O (3.8 < n < 4.2) and their stability and structure were investigated. Pair distribution functions (PDF) derived from synchrotron X-ray data indicated a lack of structural order beyond 8 {angstrom} in both phases, with this local order found to resemble crystalline analogues. Further studies, including {sup 1}H and {sup 31}P solid state NMR, suggest the unusually high stability of these purely inorganic amorphous phases is partly due to disorder in the P-O-P bond angles within the P{sub 2}O{sub 7} units, which impede crystallization, and to water molecules, which are involved in H-bonds of various strengths within the structures and hamper the formation of an ordered network. In situ high temperature powder X-ray diffraction data indicated that the amorphous nature of both phases surprisingly persisted to 450 C. Further NMR and TGA studies found that above ambient temperature some water molecules reacted with P{sub 2}O{sub 7} anions, leading to the hydrolysis of some P-O-P linkages and the formation of HPO{sub 4}{sup 2-} anions within the amorphous matrix. The latter anions then recombined into P{sub 2}O{sub 7} ions at higher temperatures prior to crystallization. Together, these findings provide important new materials with unexplored potential for enzyme-assisted resorption and establish factors crucial to isolate further stable amorphous inorganic materials.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Structure, bonding and electronic characteristics of amorphous Se

Ovonic threshold switching (OTS) selector can effectively improve the storage density and suppress the leakage current of advanced phase-change memory. As a prototypical OTS material, amorphous GeSe is widely investigated. But the attentions paid to amorphous Se (i.e., the functional constituent in amorphous GeSe) is very limited up to now. Here, in this work, we have explored the structure, bonding and electronic characteristics of amorphous Se using ab initio molecular dynamics simulations. The results reveal that the Se atoms in amorphous Se tend to form the 2-coordinated configurations, and they connect with each other to form the long chains. The fraction of vibrational density of state located in high frequency range is relatively large, and the formation energy of Se-Se bond is as large as 4.44 eV, hinting that the Se-Se bonds in chains possess a high stability. In addition, the mid-gap state related to the OTS behavior is also found in the amorphous Se despite of the small proportion. Our findings enrich the knowledge of the amorphous Se, which contributes to the applications of Se-based OTS selectors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Correlation of atomic packing with the boson peak in amorphous alloys

Boson peaks (BP) have been observed from phonon specific heats in 10 studied amorphous alloys. Two Einstein-type vibration modes were proposed in this work and all data can be fitted well. By measuring and analyzing local atomic structures of studied amorphous alloys and 56 reported amorphous alloys, it is found that (a) the BP originates from local harmonic vibration modes associated with the lengths of short-range order (SRO) and medium-range order (MRO) in amorphous alloys, and (b) the atomic packing in amorphous alloys follows a universal scaling law, i.e., the ratios of SRO and MRO lengths to solvent atomic diameter are 3 and 7, respectively, which exact match with length ratios of BP vibration frequencies to Debye frequency for the studied amorphous alloys. This finding provides a new perspective for atomic packing in amorphous materials, and has significant implications for quantitative description of the local atomic orders and understanding the structure-property relationship.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2019

Radiation Tolerance and Mechanical Properties of Nanostructured Amorphous-Ceramic/Metal Composites

The objective of this work was to use a radically non-traditional approach to design amorphous-ceramic/metal composites for service in extreme irradiation environments. The project was built on a strong integration among four research teams for materials synthesis and characterization, ion irradiation, mechanical evaluation, and atomic scale modeling. Rather than try to prevent microstructure changes in polycrystalline aggregates, the research team worked to evolve composite systems where one of the constituents is intentionally synthesized in a non-crystalline or “amorphous” state. Because amorphous materials possess no translational symmetry, such alloys do not contain conventional crystal defects such as vacancies, interstitials, or dislocations. These materials offer the possibility of eliminating the root cause responsible for radiation damage in polycrystalline solids - namely the production of point defects and clusters thereof in collision cascades - and could serve as the basis for developing a new class of structural materials with unprecedented resistance to radiation. The amorphous alloys were used to develop advanced amorphous-ceramic/metal composites with greatly improved radiation tolerance and stability above 500oC, and improved mechanical performance by combining the good properties of amorphous materials (high strength and elastic limit) with those of crystalline materials (high toughness, strain hardening). The ceramic component of the composite consisted of a high crystallization temperature and radiation tolerant amorphous alloy composed of Si-O-C, silicon oxycarbide, while the metal layer was Fe and Fe(Cr), chosen to serve as model materials for steel. A prime hypothesis that drove this work is that the composite interface, together with the composite constituents, would provide significantly enhanced radiation tolerance, similar to or superior to those observed in metallic nanolayered structures, in a more engineering relevant material system. As our experimental data and modeling show, we have successfully developed a new class of ceramic/metal composites that can be adapted for engineering applications, thus significantly impacting improved materials performance for advanced nuclear reactors.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Controlling Dissolution and Transformation of Zeolitic Imidazolate Frameworks by using Electron‐Beam‐Induced Amorphization

Abstract Amorphous zeolitic imidazolate frameworks (ZIFs) offer promising applications as novel functional materials. Herein, amorphization of ZIF‐L through scanning‐electron‐beam exposure is demonstrated, based on amorphization of individual ZIF‐L crystals. The amorphized ZIF product has drastically increased stability against dissolution in water. An electron dose that allows for complete preservation of amorphous particles after immersion in water is established, resulting in new shapes of amorphous ZIF‐L with spatial control at the sub‐micrometer length scale. Changed water stability as a consequence of scanning‐electron‐beam exposure is demonstrated for three additional metal–organic frameworks (ZIF‐8, Zn(BeIm)OAc, MIL‐101), highlighting the potential use of an electron beam for top‐down MOF patterning. Lastly, recrystallization of ZIF‐L in the presence of linker is studied and shows distinct differences for crystalline and amorphized material.

Conrad, Sabrina↗

DOE OSTI2022

Amorphization and Crystallization of Hexanitroazobenzene (HNAB) Using Conventional DSC and Flash DSC

Abstract The present work presents results from an investigation of the glass transition and crystallization behaviors of HNAB tested over more than five orders of magnitude of cooling rate from 0.005 °C/s to 600 °C/s (0.3 to 36000 °C/min) by a combination of conventional and Flash differential scanning calorimetry (DSC). The work quantifies the influence of the thermal amorphization route on the properties of this high explosive. Cooling rates faster than 100 °C/s (6000 °C/min) result in amorphous HNAB as expected from prior work, but we also find that amorphization of the HNAB occurs at cooling rates slower than 0.008 °C/s (0.5 °C/min). The behavior of the amorphous HNAB made by slow cooling is compared with that of amorphous HNAB made by fast cooling, as well as with that made by solvent casting in terms of glass transition temperature, apparent activation energy of glass transition, and dynamic fragility parameter m . Besides, the non‐isothermal crystallization response as a function of cooling rate is also reported. The thermal stability and decomposition energy of amorphous HNAB are compared with those of the crystalline counterpart, being similar heats of decomposition of 3295 and 3392 J/g, respectively; suggesting that the amorphous HNAB will have similar thermal stability and chemical energy to the crystalline form.

Koh, Yung P.↗

DOE OSTI2018

Properties of Poly(Vinyl Alcohol)/Chitosan Nanocomposite Films Reinforced with Oil Palm Empty Fruit Bunch Amorphous Lignocellulose Nanofibers

The objective of this study was to investigate the properties of poly(vinyl alcohol)/chitosan nanocomposite films reinforced with different concentration of amorphous LCNFs. The properties analyzed were morphological, physical, chemical, thermal, biological, and mechanical characteristics. Oil palm empty fruit bunch LCNFs obtained from multi-mechanical stages were more dominated by amorphous region than crystalline part. Varied film thickness, swelling degree, and transparency of PVA/chitosan nanocomposite films reinforced with amorphous part were produced. Aggregated LCNFs, which reinforced PVA/chitosan polymer blends, resulted in irregular, rough, and uneven external surfaces as well as protrusions. Based on XRD analysis, there were two or three imperative peaks that indicated the presence of crystalline states. The increase in LCNFs concentration above 0.5% to PVA/chitosan polymer blends led to the decrease in crystallinity index of the films. A noticeable alteration of FTIR spectra, which included wavenumber and intensity, was obviously observed along with the inclusion of amorphous LCNFs. That indicated that a good miscibility between amorphous LCNFs and PVA/chitosan polymer blend generated chemical interaction of those polymers during physical blending. Reinforcement of PVA/chitosan polymer blends with amorphous LCNFs influenced the changes of T{sub g} (glass transition temperature), T{sub m} (melting point temperature), and T{sub max} (maximum degradation temperature). Three thermal phases of PVA/chitosan/LCNFs nanocomposite films were also observed, including absorbed moisture evaporation, PVA and chitosan polymer backbone structural degradation and LCNFs pyrolysis, and by-products degradation of these polymers. The addition of LCNFs 0.5% had the highest tensile strength and the addition of LCNFs above 0.5% decreased the strength. The incorporation of OPEFB LCNFs did not show anti-microbial and anti-fungal properties of the films. The addition of amorphous LCNFs 0.5% into PVA/chitosan polymer blends resulted in regular and smooth external surfaces, enhanced tensile strength, increased crystallinity index, and enhanced thermal stability of the films.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2021

Critical cooling rates for amorphous-to-ordered complexion transitions in Cu-rich nanocrystalline alloys

Amorphous complexions in nanocrystalline metals have the potential to improve mechanical properties and radiation tolerance, as well as resistance to grain growth. In this study, the stability of amorphous complexions in binary and ternary Cu-based alloys is investigated by observing the effect of cooling rate from high temperature on the occurrence of amorphous-to-ordered complexion transitions. Bulk Cu-Zr and Cu-Zr-Hf alloy samples were annealed to induce boundary premelting and then quenched through a procedure that induces a gradient of local cooling rate through the sample height. Amorphous complexion thickness distributions were found to be invariant to local cooling rate in the Cu-Zr-Hf alloy, demonstrating enhanced stability of the amorphous complexion structure compared to the Cu-Zr alloy, which had thinner amorphous complexions in the regions that were slowly cooled. The experimental results are used to construct time-temperature-transformation diagrams for the amorphous-to-ordered complexion transition in both the binary and ternary alloys, enabling a deeper understanding of the influence of cooling rate and grain boundary chemistry on complexion transitions. In conclusion, the critical cooling rate necessary to avoid complexion transitions in the ternary alloy is found to be at least three orders of magnitude slower than that for the binary alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Neutron irradiation and high temperature effects on amorphous Fe-based nano-coatings on steel – A macroscopic assessment

Here, this study revealed that loss of ductility in an amorphous Fe-alloy coating on a steel substrate composite structure was essentially prevented from occurring, following radiation with modest neutron doses of ~2 x 10 18 n/cm 2 . At the higher neutron dose of ~2 x 10 19 , macroscopic stress-strain analysis showed that the amorphous Fe-alloy nanostructured coating, while still amorphous, experienced radiation-induced embrittlement, no longer offering protection against ductility loss in the coating-substrate composite structure. Neutron irradiation in a corrosive environment revealed exemplary oxidation/corrosion resistance of the amorphous Fe-alloy coating, which is attributed to the formation of the Fe 2 B phase in the coating. To establish the impact of elevated temperatures on the amorphous-to-crystalline transition in the amorphous Fe-alloy, electron microscopy was carried out which confirmed the radiation-induced suppression of crystallization in the amorphous Fe-alloy nanostructured coating.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Physico-chemical studies of amorphous carbon nanotubes synthesized at low temperature

Highlights: ► Amorphous carbon nanotubes are successfully produced via a simple method at low temperature. ► Nanotubes in straight morphologies with open ends. ► Acid treatment increases the extent of amorphous for nanotubes. ► Amorphous nanotubes exhibit phenomena of π plasmon absorbance and possess higher bandgap. -- Abstract: This work provides better understanding on the nature of amorphous carbon nanotubes, which are synthesized via a simple chemical route. Amorphous carbon nanotubes (α-CNTs) are successfully synthesized by heating a mixture of ferrocene and ammonium chloride at temperature as low as 200 °C and are treated with hydrochloric acid. Transmission and field emission scanning electron microscopy techniques are performed to examine the morphology and dimension of the samples. X-ray diffraction tests confirm the amorphous structure of the nanotubes. The Fourier transform infrared spectroscopy and Raman studies indicate that the treated α-CNTs consist of many defective walls and are more amorphous compared with the untreated α-CNTs. Ultraviolet–visible absorption studies reveal that the untreated and treated α-CNTs exhibit plasmon absorbance with high bandgaps of 4 eV and 4.35 eV, respectively.

36 MATERIALS SCIENCE↗

DOE OSTI2021

A High Energy X-ray Diffraction Study of Amorphous Indomethacin

Amorphous pharmaceuticals often possess a wide range of molecular conformations and bonding arrangements. The x-ray pair distribution function (PDF) method is a powerful technique for the characterization of variations in both intra-molecular and inter-molecular packing arrangements. Here, the x-ray PDF of amorphous Indomethacin is shown to be particularly sensitive to the preferred orientations of the chlorobenzyl ring found in isomers in the crystalline state. In some cases, the chlorobenzyl ring has no preferred torsional angle in the amorphous form, while in others evidence of distinct isomer orientations are observed. Amorphous samples with no preferred torsion angles of the chlorobenzyl ring are found to favor enhanced inter-molecular hydrogen bonding, and this is reflected in the intensity of the first sharp diffraction peak. These significant variations in structure rule out amorphous Indomethacin as a possible standard for x-ray PDF measurements. At high humidity, time resolved PDF's for >40 h reveal water molecules forming hydrogen bonds with Indomethacin molecules. Finally, a simple linear hydrogen bond model indicates that water molecules in the wet amorphous form have similar hydrogen bond strengths to those found between Indomethacin dimers or chains in the dry amorphous form.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Amorphous-Phase-Mediated Crystallization of Ni Nanocrystals Revealed by High-Resolution Liquid-Phase Electron Microscopy

Nonclassical features of crystallization in solution have been recently identified both experimentally and theoretically. In particular, an amorphous-phase-mediated pathway is found in various crystallization systems as an important route, different from the classical nucleation and growth model. In this paper, we utilize high-resolution in situ transmission electron microscopy with graphene liquid cells to study amorphous-phase-mediated formation of Ni nanocrystals. An amorphous phase is precipitated in the initial stage of the reaction. Within the amorphous particles, crystalline domains nucleate and eventually form nanocrystals. In addition, unique crystallization behaviors, such as formation of multiple domains and dislocation relaxation, are observed in amorphous-phase-mediated crystallization. Theoretical calculations confirm that surface interactions can induce amorphous precipitation of metal precursors, which is analogous to the surface-induced amorphous-to-crystalline transformation occurring in biomineralization. In conclusion, our results imply that an unexplored nonclassical growth mechanism is important for the formation of nanocrystals.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Orientation-dependent mutual crystalline and amorphous order in a single phase solid

Amorphous materials distinguish themselves from crystalline materials by lacking long-range order while retaining structural order at the local scale (2–5 Å). However, the complexity in topological and chemical order prevents current characterization tools from fully unveiling the structure in disordered materials. Consequently, the nature of medium-range order in amorphous materials has remained elusive. The Zachariasen and crystal competing models have been proposed to describe disordered phases and have both been verified through synthesis and characterization. The main difference between them is thought to be whether the amorphous phase shows medium-range order. Here we demonstrate a form of organized inorganic matter that is amorphous in two dimensions, while exhibiting long-range order and a high degree of crystallinity in the third. The structure consists of periodically stacked 2-dimensional amorphous Nb-W-O monolayers without long-range in-plane order. The unique periodic and therefore crystalline stacking along one principal axis enables direct imaging and revealed that the amorphous Nb-W-O monolayers formed in agreement with the Zachariasen model for 2 dimensions. Our findings show that the gap between crystalline and amorphous materials does not only depend on medium-range order but can also apply to principal dimensions within the same solid.

Nanowires↗