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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 865 records · Page 48
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Structure and phase transitions in niobium and tantalum derived nanoscale transition metal perovskites, Ba(Ti,MV)O3, M=Nb,Ta

The prospect of creating ferroelectric or high permittivity nanomaterials provides motivation for investigating complex transition metal oxides of the form Ba(Ti, MV)O3, where M = Nb or Ta. Solid state processing typically produces mixtures of crystalline phases, rarely beyond minimally doped Nb/Ta. Using a modified sol-gel method, we prepared single phase nanocrystals of Ba(Ti, M)O3. Compositional and elemental analysis puts the empirical formulas close to BaTi0.5Nb0.5O3−δ and BaTi0.5Ta0.5O3−δ. For both materials, a reversible temperature dependent phase transition (non-centrosymmetric to symmetric) is observed in the Raman spectrum in the region 533–583 K (260–310 °C); for Ba(Ti, Nb)O3, the onset is at 543 K (270 °C); and for Ba(Ti, Ta)O3, the onset is at 533 K (260 °C), which are comparable with 390–393 K (117–120 °C) for bulk BaTiO3. The crystal structure was resolved by examination of the powder x-ray diffraction and atomic pair distribution function (PDF) analysis of synchrotron total scattering data. It was postulated whether the structure adopted at the nanoscale was single or double perovskite. Double perovskites (A2B′B″O6) are characterized by the type and extent of cation ordering, which gives rise to higher symmetry crystal structures. PDF analysis was used to examine all likely candidate structures and to look for evidence of higher symmetry. The feasible phase space that evolves includes the ordered double perovskite structure Ba2(Ti, MV)O6 (M = Nb, Ta) Fm-3m, a disordered cubic structure, as a suitable high temperature analog, Ba(Ti, MV)O3Pm-3m, and an orthorhombic Ba(Ti, MV)O3Amm2, a room temperature structure that presents an unusually high level of lattice displacement, possibly due to octahedral tilting, and indication of a highly polarized crystal.

Chemistry↗
DOE OSTI2017

Magnetic and magnetocaloric properties of HoCr O 3 tuned by selective rare-earth doping

Rare-earth chromites ( R Cr O 3 ) are an important subclass of functional materials with interesting magnetic, electrical, and catalytic properties that make them promising for various applications. In this paper, we report comparisons on the structural and magnetic properties of HoCr O 3 with those of H o 0.67 T m 0.33 Cr O 3 and H o 0.67 G d 0.33 Cr O 3 powder samples, which were doped by T m 3 + (or G d 3 + ) ions at the A -site with ionic radius smaller (or larger) than that of H o 3 + ion. The structural properties of the samples were characterized by x-ray diffraction, Raman spectroscopy, and scanning electron microscopy carried out at ambient. The band gaps of the three samples were determined by analyzing their ultraviolet Vis spectra. Magnetic studies carried out from 5 K to 300 K show that the Néel temperature ( T N Cr , where C r 3 + ions order) increases with an increase in the average A -site ( R -site) ionic radius, tolerance factor, and Cr1-O1-Cr1 bond angle but decreases with an increase in the orthorhombic strain factor. In addition, the application of external hydrostatic pressure was found to enhance T N Cr of HoCr O 3 , similar to the effect observed by doping HoCr O 3 with G d 3 + ions. These changes in T N Cr with A -site doping and hydrostatic pressure are related to changes in C r 3 + - C r 3 + exchange coupling resulting from changes in the Cr1-O1-Cr1 bond angle and Cr1-O1 bond lengths, respectively. Temperature dependent paramagnetic susceptibility data of the samples was fitted to the modified Curie-Weiss law that included the Dzyloshinskii-Moriya interaction. Isothermal magnetization data showed that the magnetic behavior of the samples changes from canted antiferromagnetic at low temperatures to paramagnetic at higher temperatures. The large magnetocaloric entropy change was observed in HoCr O 3 , which was enhanced by Gd doping but lowered by Tm doping, showing its tunability by A -site doping. Correlation between magnetoelectric properties and magnetization is discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2023

ac susceptibility studies of intra- and intergrain properties of high-$J_c$ Bi-2212 wires

Bi 2 Sr 2 CaCu 2 O x (Bi-2212) is the only high-$T_c$ superconductor (HTS) available as a multifilamentary round wire with multiple architectures and it is a very promising conductor for the realization of high-field applications. Despite their relatively simple wire fabrication by the powder-in-tube technique, Bi-2212 wires require a tightly controlled overpressure heat treatment (HT) with a multi-parameter time-temperature schedule to achieve high critical current density, $J_c$. Further, the variation of these HT parameters, changes in the wire design, wire diameter and powder quality can lead to variations in both the microstructure and the superconducting performance. Particularly noticeable are variations in $J_c$ performance and degree of filament bridging. In this work, we focus on the use of different magnetic characterization techniques to estimate the bridging level and assess the balance of INTER-grain and intra-grain superconducting properties including the irreversibility field ($H_{\text{irr}}$) and the pinning energy ($U_0$) in differently processed wires. Regardless of the actual bridging level, we find that the supercurrent flows at the filament bundle level, not just at the individual filament level. Moreover, using AC susceptibility we identify two distinct supercurrent contributions, one related to the intra-grain and one to the INTER-grain properties, whose irreversibility fields are different but without large sample-to-sample variation. Moreover, an additional component of intra-grain pinning mechanism becomes effective at low temperatures with positive effects also on the INTER-grain performance. The work clearly shows that detailed magnetic characterizations can become valuable tools to investigate the performance of differently processed Bi-2212 wires, correlating their microstructure and overall transport $J_c$, to obtain a deeper understanding of the causes of performance variation and paths to achieve further improvement.

2212↗
DOE OSTI2017

Thermal safety characterization on PETN, PBX-9407, LX-10-2, LX-17-1 and detonator in the LLNL's P-ODTX system

Incidents caused by fire and other thermal events can heat energetic materials that may lead to thermal explosion and result in structural damage and casualty. Thus, it is important to understand the response of energetic materials to thermal insults. The One-Dimensional-Time to Explosion (ODTX) system at the Lawrence Livermore National Laboratory (LLNL) has been used for decades to characterize thermal safety of energetic materials. In this study, an integration of a pressure monitoring element has been added into the ODTX system (P-ODTX) to perform thermal explosion (cook-off) experiments (thermal runaway) on PETN powder, PBX-9407, LX-10-2, LX-17-1, and detonator samples (cup tests). The P-ODTX testing generates useful data (thermal explosion temperature, thermal explosion time, and gas pressures) to assist with the thermal safety assessment of relevant energetic materials and components. This report summarizes the results of P-ODTX experiments that were performed from May 2015 to July 2017. Recent upgrades to the data acquisition system allows for rapid pressure monitoring in microsecond intervals during thermal explosion. These pressure data are also included in the report.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Optical properties of BaFCl:Eu 2+ scintillating composites for X-ray imaging screens

The development of composite scintillating materials is necessary for the optimization of advanced pixelated X-ray imaging technology. Polycrystalline BaFCl:Eu 2+ was synthesized via a flux growth technique and its emission properties were characterized through photo-luminescence (PL) spectroscopy and time-correlated single photon counting (TCSPC). PL emission wavelengths were observed at 365 nm, 383 nm, and 430 nm under UV excitation. Composite pastes, consisting of BaFCl:Eu 2+ powder and NOA1665 UV-curable resin, were fabricated and subsequently analyzed through absorption and radio-luminescence (RL) spectroscopy. An interchange of transmissivity and light production, resulting from differences in the amount of solvent and resin in the composite, was observed in fabricated composites.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Models to Incorporate Reaction Mechanisms into DG-OSPREY: Fixed-Bed Simulations for Organic Iodides Capture Using Ag 0 Z

As one of the most potent radioisotopes released during spent nuclear fuel reprocessing, 129 I is strictly regulated and must be removed before discharge. Organic iodides (primarily alkyl iodides with different chain lengths, i.e., CH 3 I, C 4 H 9 I, and C 12 H 25 I) comprise ~2% of the total iodine in the reprocessing off-gases and are primarily present in vessel off-gas (VOG). Reduced silver mordenite (Ag 0 Z) is predominantly considered for the removal of radioiodine; however, its capture performance and underlying interaction processes with long-chain organic iodides are not fully understood. Two major tasks were accomplished in this study. First, to improve upon the previous experimental studies where Ag 0 Z was used to capture CH 3 I, C 4 H 9 I, and C 12 H 25 I at different concentrations, we comprehensively investigated the corresponding capture mechanisms by characterizing fully loaded Ag 0 Z samples. Second, computational codes were implemented to perform fixed-bed simulations that account for transport and reaction mechanisms. Scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX), powder X-ray diffraction (PXRD), UV-visible diffuse reflectance spectroscopy (UV-vis DRS), and thermogravimetric analysis (TGA) were conducted on Ag 0 Z samples that are saturated with I 2 , CH 3 I, C 4 H 9 I, and C 12 H 25 I), respectively. Results indicate that AgI is the predominant adsorption product regardless of the adsorbed iodine species, yet alkyl iodides with different carbon chain lengths may have different compositions of α- and γ-AgI. Synchrotron pair distribution function (PDF) measurements and TGA coupled with a Fourier transformed infrared detector (TGA FTIR) have been performed, and experimental data are currently analyzed. Results are expected to provide further insights into the adsorption mechanisms. The fixed-bed capture performance for CH 3 I was successfully simulated by solving mathematical equations that describe the underlying transport processes and adsorption reactions. The computational framework, Catalytic After Treatment System (CATS), that was originated in our research group, was used to solve the governing equations. Kinetic parameters, including the pore diffusivity and reaction rate constant were obtained by optimization techniques using data from thin-bed experiments performed at Oak Ridge National Laboratory. The performance of a deep bed predicted using the optimized parameters showed promising agreement with the experimental data.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

High‐Pressure Characterization of High‐Performance Insensitive Energetic Materials: Dihydroxylammonium 5,5’‐Bis(3‐Nitro‐1,2,4‐Triazolate‐1 N ‐Oxide) (MAD‐X1)

Abstract The high‐pressure behavior of dihydroxylammonium 5,5’‐bis(3‐nitro‐1,2,4‐triazolate‐ 1 N ‐oxide) (MAD‐X1) was studied at room temperature to 25 GPa by Raman spectroscopy and powder X‐ray diffraction. No evidence of polymorphism was observed over this pressure range, indicating that the ambient structure of MAD‐X1 remains stable up to conditions similar to the detonation pressure of the material. Additionally, such findings suggest that this high performance material can serve as an insensitive RDX replacement in energetic formulations without the concern of uncontrolled polymorphism that might otherwise affect the performance and safety of the munition.

Bennion, Jonathan C.↗
DOE OSTI2021

Nonlinear ultrasonic technique for the characterization of microstructure in additive materials

This study employs nonlinear ultrasonic techniques to track microstructural changes in additively manufactured metals. The second harmonic generation technique based on the transmission of Rayleigh surface waves is used to measure the acoustic nonlinearity parameter, β. Stainless steel specimens are made through three procedures: traditional wrought manufacturing, laser-powder bed fusion, and laser engineered net shaping. The β parameter is measured through successive steps of an annealing heat treatment intended to decrease dislocation density. Dislocation density is known to be sensitive to manufacturing variables. In agreement with fundamental material models for the dislocation-acoustic nonlinearity relationship in the second harmonic generation, β drops in each specimen throughout the heat treatment before recrystallization. Geometrically necessary dislocations (GNDs) are measured from electron back-scatter diffraction as a quantitative indicator of dislocations; average GND density and β are found to have a statistical correlation coefficient of 0.852 showing the sensitivity of β to dislocations in additively manufactured metals. Moreover, β shows an excellent correlation with hardness, which is a measure of the macroscopic effect of dislocations.

42 ENGINEERING↗
DOE OSTI2018

Size and Morphology Controlled Synthesis of Boehmite Nanoplates and Crystal Growth Mechanisms

The aluminum oxyhydroxide boehmite is an important crystalline phase in nature and industry. We report development of a flexible additive-free hydrothermal synthesis method to prepare high quality boehmite nanoplates with sizes ranging from under 20 nm to 5 um via using hydrated alumina gels and amorphous powders as precursors. The size and morphology of the boehmite nanoplates was systematically varied between hexagonal and rhombic by adjusting precursor concentrations, pH, and the synthesis temperature, due to face-specific effects. The transformation mechanism is consistent with dissolution and reprecipitation, and involves transitory initial appearance of metastable gibbsite that is later consumed upon nucleation of boehmite. Detailed X-ray pair distribution characterization of the solids over time showed similarities in short-range order that suggest linkages in local chemistry and bonding topology between the precursors and product boehmite, yet also that precursor-specific differences in long-range order appear to manifest subtle changes in resulting boehmite characteristics, suggesting that the rate and extent of water release or differences in the resulting solubilized aluminate speciation leads to slightly different polymerization and condensation pathways. The findings suggest that during dissolution of the precursor that precursor-specific dehydration or solution speciation could be important aspects of the transformation impacting the molecular level details of boehmite nucleation and growth.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Processing and Characterization of Sol-Gel Cerium Oxide Microspheres

Of interest to space exploration and power generation, Radioisotope Thermoelectric Generators (RTGs) can provide long-term power to remote electronic systems without the need for refueling or replacement. Plutonium-238 (Pu-238) remains one of the more promising materials for thermoelectric power generation due to its high power density, long half-life, and low gamma emissions. Traditional methods for processing Pu-238 include ball milling irregular precipitated powders before pressing and sintering into a dense pellet. The resulting submicron particulates of Pu-238 quickly accumulate and contaminate glove boxes. An alternative and dust-free method for Pu-238 processing is internal gelation via sol-gel techniques. Sol-gel methodology creates monodisperse and uniform microspheres that can be packed and pressed into a pellet. For this study cerium oxide microspheres were produced as a surrogate to Pu-238. The similar electronic orbitals between cerium and plutonium make cerium an ideal choice for non-radioactive work. Before the microspheres can be sintered and pressed they must be washed to remove the processing oil and any unreacted substituents. An investigation was performed on the washing step to find an appropriate wash solution that reduced waste and flammable risk. Cerium oxide microspheres were processed, washed, and characterized to determine the effectiveness of the new wash solution.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Optimization of Processing, Microstructure, and Hardness of an Al–Ce–Ni–Mn–Zr Alloy With Laser Additive Manufacturing

Here, this study examines the processing behavior, microstructure, surface roughness, and hardness properties of an aluminum alloy containing 8.2 Ce, 4.5 Ni, 0.5 Mn, and 0.7 Zr (wt%) fabricated using laser powder bed fusion. Sixty samples were produced across a range of laser powers, scan speeds, and hatch spacings to evaluate their effect on porosity, hardness, and microstructural features. Porosity was measured using X-ray computed tomography, while microstructure and surface roughness were characterized by scanning electron (SEM) and laser confocal microscopy. High dense and cracking-free Al–Ni–Ce alloy was successfully manufactured. Porosity showed a U-shaped dependence on energy input, increasing under both insufficient and excessive melting conditions. Hardness increased with cooling rate due to finer cellular structures and solute redistribution. A general statistical model was developed to capture the relationships between processing parameters and material response. Results identify a narrow processing window defined by laser powers between 350 and 370 W, scan speeds from 1400 to 1800 mm/s, and hatch distances between 0.14 and 0.18 mm. Within this window, porosity is minimized (below 0.01%) and hardness is maximized (up to 160 HV), demonstrating that careful control of these parameters enables dense, high strength aluminum components suitable for demanding structural applications.

Aluminum alloys↗
DOE OSTI2021

Application of HRGS for forensic characterization of uranium oxides, pure uranium metals and uranium alloys

A nondestructive iterative method for uranium-bearing material characterization with HRGS developed earlier in (J. appl. Rad. Isotopes, 166 (2020) 109433) is applied to determine matrix densities and uranium isotope masses of a variety of uranium materials, namely uranium ore, UO 2 and U 3 O 8 powders, fuel elements in the form of UO2 microspheres, uranium metal and uranium alloys. It is shown that U 3 O 8 powders with uranium mass fraction of about 84% can be distinguished from the powders of UO 2 with uranium mass fraction of about 87%; uranium products in the form of liquid or loose powder with matrix density of 0.5-2.0 g/cm 3 can be distinguished from uranium products in the form of compacted fuel elements with matrix density of 6.0-10.0 g/cm 3 and from pure metal uranium and uranium alloys with matrix density of 14.0- 19.0 g/cm 3 . In fuel microspheres based on UO2 the uranium mass fraction 88.02% measured by HRGS is consistent, within the measurement uncertainties, with the results of isotope dilution mass spectrometry 87.76±0.64 % and also is confirmed by X-ray diffraction technique. The uranium mass fraction of the uranium ore estimated as 0.08% by HRGS is consistent, within the measurement uncertainties, with the value 0.09±0.01% determined with WDXRF. Densities of two different uranium metal samples, estimated as 18.42 g/cm 3 and 19.33 g/cm 3 by HRGS are consistent with values 18.24±0.55 g/cm 3 and 18.86±0.59 g/cm 3 , respectively, obtained by the gas pycnometry technique.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

Complete Status Report Documenting the Processing, Microstructure and High-Temperature Mechanical Properties of the Nanostructured Ferritic Alloy OFRAC

This report provides a summary of the new nanostructured ferritic alloy, OFRAC (Oak Ridge Fast Reactor Advanced Fuel Cladding), that was developed for the advanced sodium fast reactor fuel cladding and core internals. The composition of OFRAC, which is Fe-12Cr-1Mo-03.Ti-0.3Nb + 0.3Y2O3 (wt. %), was chosen to achieve high temperature strength as well as high temperature creep performance and swelling resistance requirements that past structural materials such as austenitic stainless steels and ferritic/martensitic steels, i.e. HT-9, are not suitable as SFR cladding materials. The mechanical alloying procedures were described for producing OFRAC and the detailed characterization studies revealed uniformly distributed, high concentration of Y-Ti-O enriched oxide particles, or nanoclusters. The Nb addition that was intended to sequester interstitial C and N that are commonly introduced as contamination during ball milling of powder was found to be very effective in forming coarse size Nb carbonitrides along with excess Ti that removes these interstitial elements from the bcc-Fe matrix of OFRAC. The tensile tests on the OFRAC in the extruded condition showed excellent balance in strength and ductility from room temperature to 800°C. Both the microstructure and tensile properties were not significantly degraded after annealing the extruded OFRAC samples for 8 h at 1050°C and 1150°C. The latter temperature is ~76% of the melting point of OFRAC. These results demonstrated the stability of the microstructure and tensile properties to extremely high temperatures. The thermal creep resistance at elevated temperatures and stresses was investigated using strain rate jump testing. The results showed that OFRAC possessed high stress exponents at high stresses and temperatures of 550°C, 600°C, 700ºC and 800°C. This thermal dependence of minimum creep rate indicates that OFRAC will show quite low creep rates at higher temperatures and stresses compared to HT-9 and stainless steels. These significant improvements indicate that the NFA OFRAC alloy is a compelling and viable choice for sodium fast reactor fuel cladding.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Characterization of Grain Boundaries and Associated Minor Phases in Disk Alloy ME3 Exposed at 815 °C

The objective of this work was to address the effect of 815 °C exposures on the chemistry of interior grain boundaries and associated minor phases from the fatigued volume of tested notched low cycle fatigue (NLCF) specimens of an advanced powder metallurgy superalloy ME3, which is used in turbine disk applications. Prior to NLCF testing at 704 °C in air, selected ME3 specimens were pre-exposed at 815 °C for exposures times up to 2,020 h to capture projected service conditions for the turbine disk rim. Structure, compositions and size distributions of minor phases, including MC carbides, M23C6 carbides, M3B2 borides and sigma, were identified. Minor phase and grain boundary chemistry for various conditions were evaluated with atom probe tomography and high resolution x-ray energy-dispersive spectroscopy.

Sudbrack, Chantal K.↗
DOE OSTI2017

Additive manufacturing and mechanical characterization of high density fully stabilized zirconia

Mechanical properties of additively manufactured 8 mol% yttria-stabilized zirconia (8YSZ) parts were extensively studied for the first time. A novel freeform extrusion fabrication process, called Ceramic On-Demand Extrusion (CODE), was employed to deposit an aqueous viscous suspension (~50 vol% solids loading) of fully stabilized zirconia powder in a layer-by-layer fashion. Each layer was exposed to infrared radiation after deposition to attain partial solidification due to drying. Before exposure, the layer was surrounded by oil to preclude non-uniform evaporation, which could cause warpage and crack formation. After the fabrication process was completed, the parts were humid-dried in an environmental chamber and densified by sintering under atmospheric pressure. Here standard test methods were employed to examine the properties of sintered parts including density, Vickers hardness, fracture toughness, Young's modulus, and flexural strength. Microstructural evaluation was also performed to observe the microstructural morphology and measure grain size. The results indicate that the properties of 8YSZ parts produced by the CODE process match those obtained by conventional fabrication techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Viewing internal bubbling and microexplosions in combusting metal particles via x-ray phase contrast imaging

The combustion performance of metal particles for explosives, propellants, pyrotechnics, and bio-agent defeat can be optimized by controlling the chemistry, size, and coatings of the particles. Many pure and composite metal fuels used in these applications have been observed to microexplode during combustion. This causes particles to fragment, revealing fresh surfaces, which may enhance burn rates and efficiencies. Despite these potential benefits, few have attempted to control the bubbling and the microexplosion of metal powders as they combust in molten states. Here, we choose Al:Zr composite powders as a representative system to study bubbling and microexplosions and to identify active mechanisms. Using synchrotron x-rays and phase contrast imaging, we observe molten metal particles of various sizes as they burn in air at temperatures ranging from 2700 to 3500 K. We characterize bubble nucleation and growth in the interior of the particles during the combustion process, and we identify heterogeneous nucleation, slow growth and coalescence of bubbles, as well as rapid bubble growth leading to microexplosions. Bubble growth rates and Laplace pressures are calculated, and we find that during slow expansion growth rates are similar to classical predictions of bubble growth in superheated liquids. For rapid expansions we find that a critical growth rate of ~0.5m s –1 , independent of the initial particle size, is necessary to enable microexplosions. We calculate the rate of gas generation that is needed to enable this growth and we conclude that nitrogen is the gas most likely driving rapid bubble growth and fragmentation. Furthermore these results provide the first in situ observations of the mechanisms that control bubbling and microexplosions during the combustion of metal particles.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Ambient pressure synthesis and characterization of layered honeycomb Li 2 PdO 3

Single-phase polycrystalline Li 2 PdO 3 has been synthesized at 640°C in oxygen for the first time under ambient pressure. X-ray and neutron diffraction analyses show that the sample possesses a monoclinic layered structure belonging to the C2/m space group. Rietveld refinements of neutron powder diffraction data indicate ~10% Li–Pd site exchange and DIFFaX modelling manifest ~2% stacking faults present within LiPd 2 layers. A band gap of ~2.23 eV was calculated for the golden Li 2 PdO 3 using absorbance measurements. Thermogravimetric analysis of the sample shows that Li 2 PdO 3 is stable up to 730°C under oxygen. Here a Curie tail is observed at low temperature magnetic measurements (T < 50K), yielding an effective moment of 0.038 μ B , possibly due to spin ½ impurities.

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

Atomic structure and grain shape evolution of nanodiamond during annealing in oxidizing atmosphere from neutron diffraction and MD simulations

In this work, real space pair-distribution function (PDF) analysis in conjunction with molecular dynamics (MD) simulations was applied to characterize crystal structure, shape and surface structure of diamond nanoparticles annealed in air up to 880 °C. MD simulated models of individual nanodiamond particles of various shapes and sizes were used to calculate theoretical radial distribution functions G(r) for powders with different grain size distributions. The calculated curves, showing distinct differences for the explored parameter space, were compared to the experimental G(r) functions obtained from neutron scattering for annealed detonated nanodiamond samples in a search for a model best describing the actual powders. It was found that as-synthesized nanodiamond grains are terminated by equally abundant (100), (110) and (111) crystallographic faces and their structure does not change upon annealing in air up to 280 °C. The shape and size of grains annealed above 480 °C changes due to surface etching. The etching rate differs between crystals faces and depends on temperature, resulting in the observed differences in grain shape. Below 680 °C the share of the (110) facets gradually increases and at 680 °C the grains become rhombic dodecahedra terminated solely by (110) surfaces. Further increase of the annealing temperature promotes formation of (111) surfaces and at 880 °C the preferred grain shape becomes an octahedron terminated by a variant of (111) surfaces possessing three dangling sp3 bonds per atom. At lower temperatures all grains become smaller and the size distribution moves towards the lower values. Furthermore, as the annealing temperature increases, the smallest grains disappear entirely and the average grain size grows back.

36 MATERIALS SCIENCE↗