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At least 1,567 records · Page 87
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

The effect of submicron grain size on thermal stability and mechanical properties of high-entropy carbide ceramics

(Hf 0.2 Zr 0.2 Ta 0.2 Nb 0.2 Ti 0.2 )C high-entropy ceramics (HEC) with a submicron grain size of 400 to 600 nm were fabricated by spark plasma sintering using a two-step sintering process. Both X-ray and neutron diffractions confirmed the formation of single-phase with rock salt structure in the as-fabricated (Hf 0.2 Zr 0.2 Ta 0.2 Nb 0.2 Ti 0.2 )C samples. The effect of submicron grain size on the thermal stability and mechanical properties of HEC was investigated. The grain growth kinetics in the fine-grained HEC was small at 1300 and 1600°C, suggesting high thermal stability that was possibly related to the compositional complexity and sluggish diffusion in HEC. Compared to the coarse-grain HEC with a grain size of 16.5 µm, the bending strength and fracture toughness of fine-grained HEC were 25% and 20% higher respectively. The improvement of mechanical properties in fine-grained HEC may be attributed to micromechanistic mechanisms such as crack deflection.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Self-propagating high-temperature synthesis of Lu{sub 2}O{sub 3} powders for optical ceramics

A technique has been developed for the self-propagating high-temperature synthesis of lutetium oxide (Lu{sub 2}O{sub 3}) powders using citric acid, glycine, and lutetium acetate as fuels. We have carried out thermodynamic analysis of synthesis conditions and examined the effect of the nature of the fuel on the properties of the resultant powders. Using vacuum sintering at a temperature of 1780°C and powders prepared with glycine as a fuel and containing 25 mol % yttrium oxide and 5 mol % lanthanum oxide as sintering aids, we have obtained transparent lutetium oxide-based ceramics.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of the Surface Modification of Synthetic Diamond with Nickel or Tungsten on the Properties of Copper–Diamond Composites

Tungsten- and nickel-containing coatings have been produced on the surface of synthetic diamond crystals by rotary chemical vapor deposition (RCVD) using tungsten hexacarbonyl, W(CO){sub 6}, and nickelocene, Ni(C{sub 5}H{sub 5}){sub 2}, as gaseous precursors. The thickness, composition, and morphology of the coatings have been shown to depend on the RCVD process duration and reactant concentrations in the vapor phase. The synthetic diamond microcrystals with tungsten- and nickel-containing coatings have been used to produce copper–diamond heat-conducting composites. Powder mixtures containing 50 vol % diamond with a particle size of 50, 100, or 200 μm have been consolidated by spark plasma sintering or hot pressing. It has been shown that the highest relative density (97%) and thermal conductivity (340 W/(m K)) are offered by the composites produced by spark plasma sintering using tungsten carbide-coated 50-μm diamond crystals.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Effect of Sequential Heat Impacts on the Formation of a Stable State of the xLPM–(1 – x)PT Multiferroic Composites

The effect of thermal cycling and sintering temperature on the chemical and thermodynamic stability of the bulk multiferroic xLa{sub 0.7}Pb{sub 0.3}MnO{sub 3}–(1 – x)PbTiO{sub 3} quasi-ceramic and ceramic composites has been experimentally investigated. It is shown that the limiting temperature of the long-term sample firing should not exceed 1070 K. It has been found that sintering at this temperature and/or short-term exposure of the samples at higher temperatures (up to 1220 K) significantly increase the sample compactness, stabilize the thermal expansion, and enhance the quality of the composites. It has been established that the component grain integrity is violated by shrinkage of the samples and a sharp change in their volume during the phase transition of a ferroelectric component.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

The Effect of Porosity and Grain Size on the Phase Composition and Mechanical Properties of Zirconium-Dioxide-Based Ceramic

ZrO{sub 2}(Y) ceramic with embedded particles of a pore-forming agent—ultrahigh molecular weight polyethylene—has been studied. It has been shown that the porosity of samples after sintering changed from 2 to 42 vol % and the grain size changed from 0.5 to 1.55 μm depending on sintering regime. The strength of materials with minimum porosity was 3000 ± 200 MPa, while the strength of materials with maximum porosity was 100 ± 20 MPa, regardless of grain size. It has been shown that the tetragonal to monoclinic martensitic phase transformation related to mechanical stresses takes place in the material without any effect on the macrostrength of the material. Internal microscopic stresses decreasing with an increase in porosity and ceramic grain size are the main factor causing this transformation in a porous material.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Development of low-cost technology for the next generation of high efficiency solar cells composed of earth abundant elements

The development of renewable, affordable, and environmentally conscious means of generating energy on a global scale represents a grand challenge of our time. Due to the “permanence” of radiation from the sun, solar energy promises to remain a viable and sustainable power source far into the future. Established single-junction photovoltaic technologies achieve high power conversion efficiencies (pce) near 20% but require complicated manufacturing processes that prohibit the marriage of large-scale throughput (e.g. on the GW scale), profitability, and quality control. Our approach to this problem begins with the synthesis of nanocrystals of semiconductor materials comprising earth abundant elements and characterized by material and optoelectronic properties ideal for photovoltaic applications, namely Cu2ZnSn(S,Se)4 (CZTSSe). Once synthesized, such nanocrystals are formulated into an ink, coated onto substrates, and processed into completed solar cells in such a way that enables scale-up to high throughput, roll-to-roll manufacturing processes. This project aimed to address the major limitation to CZTSSe solar cell pce’s – the low open-circuit voltage (Voc) reported throughout literature for devices comprised of this material. Throughout the project significant advancements have been made in fundamental understanding of the CZTSSe material and device limitations associated with this material system. Additionally, notable improvements have been made to our nanocrystal based processing technique to alleviate performance limitations due to the identified device limitations. Notably, (1) significant improvements have been made in reducing intra- and inter-nanoparticle heterogeneity, (2) improvements in device performance have been realized with novel cation substitution in Ge-alloyed CZTGeSSe absorbers, (3) systematic analysis of absorber sintering has been conducted to optimize the selenization process for large grain CZTSSe absorbers, (4) novel electrical characterization analysis techniques have been developed to identify significant limitations to traditional electrical characterization of CZTSSe devices, and (5) the developed electrical analysis techniques have been used to identify the role that band gap and electrostatic potential fluctuations have in limiting device performance for this material system. The device modeling and characterization of CZTSSe undertaken with this project have significant implications for the CZTSSe research community, as the identified limitations due to potential fluctuations are expected to be a performance limitation to high-efficiency CZTSSe devices fabricated from all current processing techniques. Additionally, improvements realized through enhanced absorber processing conditions to minimize nanoparticle and large-grain absorber heterogeneity are suggested to be beneficial processing improvements which should be applied to CZTSSe devices fabricated from all processing techniques. Ultimately, our research has indicated that improved performance for CZTSSe will be achieved through novel absorber processing which minimizes defect formation, elemental losses, secondary phase formation, and compositional uniformity in CZTSSe absorbers; we believe this novel absorber processing can be achieved through nanocrystal based processing of CZTSSe which is an active area of research at the conclusion of this award. While significant fundamental understanding of CZTSSe and the performance limitations associated with this material system, as well as notable improvements in the processing of nanocrystal based CZTSSe absorbers, have been achieved under this project, the limitation of two years of research funding towards our goals prevents further significant advancements directly identified through pce. improvements relative to those reported herein. As the characterization and modeling subtask of this project has been the main driving force for understanding device limitations, the conclusions of this analysis have just recently been applied to the processing of nanocrystal based CZTSSe absorbers -- with notable success. We expect the notable fundamental understanding of device limitations and absorber sintering achieved under this project will lead to significant improvements in device performance for CZTSSe devices in the near future for devices fabricated from a variety of processing techniques

14 SOLAR ENERGY↗
DOE OSTI2015

Powder Metallurgy Fabrication of Molybdenum Accelerator Target Disks

Powder metallurgy approaches for the fabrication of accelerator target disks are being examined to support the development of Mo-99 production by NorthStar Medical Technologies, LLC. An advantage of powder metallurgy is that very little material is wasted and, at present, dense, quality parts are routinely produced from molybdenum powder. The proposed targets, however, are thin wafers, 29 mm in diameter with a thickness of 0.5 mm, with very stringent dimensional tolerances. Although tooling can be machined to very high tolerance levels, the operations of powder feed, pressing and sintering involve complicated mechanisms, each of which affects green density and shrinkage, and therefore the dimensions and shape of the final product. Combinations of powder morphology, lubricants and pressing technique have been explored to produce target disks with minimal variations in thickness and little or no distortion. In addition, sintering conditions that produce densities for optimum target dissolvability are being determined.

43 PARTICLE ACCELERATORS↗
DOE OSTI2016

Shear Alignment of Diblock Copolymers for Patterning Nanowire Meshes

Metallic nanowire meshes are useful as cheap, flexible alternatives to indium tin oxide – an expensive, brittle material used in transparent conductive electrodes. We have fabricated nanowire meshes over areas up to 2.5 cm 2 by: 1) mechanically aligning parallel rows of diblock copolymer (diBCP) microdomains; 2) selectively infiltrating those domains with metallic ions; 3) etching away the diBCP template; 4) sintering to reduce ions to metal nanowires; and, 5) repeating steps 1 – 4 on the same sample at a 90° offset. We aligned parallel rows of polystyrene-b-poly(2-vinylpyridine) [PS(48.5 kDa)-b-P2VP(14.5 kDa)] microdomains by heating above its glass transition temperature (T g ≈ 100°C), applying mechanical shear pressure (33 kPa) and normal force (13.7 N), and cooling below T g . DiBCP samples were submerged in aqueous solutions of metallic ions (15 – 40 mM ions; 0.1 – 0.5 M HCl) for 30 – 90 minutes, which coordinate to nitrogen in P2VP. Subsequent ozone-etching and sintering steps yielded parallel nanowires. We aimed to optimize alignment parameters (e.g. shear and normal pressures, alignment duration, and PDMS thickness) to improve the quality, reproducibility, and scalability of meshes. We also investigated metals other than Pt and Au that may be patterned using this technique (Cu, Ag).

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Process R&D for Particle Size Control of Molybdenum Oxide

The primary goal of this study was to produce MoO 3 powder with a particle size range of 50 to 200 μm for use in targets for production of the medical isotope 99 Mo. Molybdenum metal powder is commercially produced by thermal reduction of oxides in a hydrogen atmosphere. The most common source material is MoO 3 , which is derived by the thermal decomposition of ammonium heptamolybdate (AHM). However, the particle size of the currently produced MoO 3 is too small, resulting in Mo powder that is too fine to properly sinter and press into the desired target. In this study, effects of heating rate, heating temperature, gas type, gas flow rate, and isothermal heating were investigated for the decomposition of AHM. The main conclusions were as follows: lower heating rate (2-10°C/min) minimizes breakdown of aggregates, recrystallized samples with millimeter-sized aggregates are resistant to various heat treatments, extended isothermal heating at >600°C leads to significant sintering, and inert gas and high gas flow rate (up to 2000 ml/min) did not significantly affect particle size distribution or composition. In addition, attempts to recover AHM from an aqueous solution by several methods (spray drying, precipitation, and low temperature crystallization) failed to achieve the desired particle size range of 50 to 200 μm. Further studies are planned.

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 OSTI2017

Performance and Reliability of Bonded Interfaces for High-temperature Packaging: Annual Progress Report

As maximum device temperatures approach 200 °Celsius, continuous operation, sintered silver materials promise to maintain bonds at these high temperatures without excessive degradation rates. A detailed characterization of the thermal performance and reliability of sintered silver materials and processes has been initiated for the next year. Future steps in crack modeling include efforts to simulate crack propagation directly using the extended finite element method (X-FEM), a numerical technique that uses the partition of unity method for modeling discontinuities such as cracks in a system.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2019

A Review on Binder Jet Additive Manufacturing of 316L Stainless Steel

Binder jet additive manufacturing enables the production of complex components for numerous applications. Binder jetting is the only powder bed additive manufacturing process that is not fusion-based, thus manufactured parts have no residual stresses as opposed to laser-based additive manufacturing processes. Binder jet technology can be adopted for the production of various small and large metallic parts for specific applications, including in the biomedical and energy sectors, at a lower cost and shorter lead time. One of the most well-known types of stainless steels for various industries is 316L, which has been extensively manufactured using binder jet technology. Binder jet manufactured 316L parts have obtained near full density and, in some cases, similar mechanical properties compared to conventionally manufactured parts. This article introduces methods, principles, and applications of binder jetting of SS 316L. Details of binder jetting processes, including powder characteristics (shape and size), binder properties (binder chemistry and droplet formation mechanism), printing process parameters (such as layer thickness, binder saturation, drying time), and post-processing sintering mechanism and densification processes, are carefully reviewed. Furthermore, critical factors in the selection of feedstock, printing parameters, sintering temperature, time, atmosphere, and heating rate of 316L binder jet manufactured parts are highlighted and summarized. Finally, the above-mentioned processing parameters are correlated with final density and mechanical properties of 316L components to establish a guideline on feedstock selection and process parameters optimization to achieve desired density, structure and properties for various applications.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Microstructural Transitions during Powder Metallurgical Processing of Solute Stabilized Nanostructured Tungsten Alloys

Exploiting grain boundary engineering in the design of alloys for extreme environments provides a promising pathway for enhancing performance relative to coarse-grained counterparts. Due to its attractive properties as a plasma facing material for fusion devices, tungsten presents an opportunity to exploit this approach in addressing the significant materials challenges imposed by the fusion environment. Here, we employ a ternary alloy design approach for stabilizing W against recrystallization and grain growth while simultaneously enhancing its manufacturability through powder metallurgical processing. Mechanical alloying and grain refinement in W-10 at.% Ti-(10,20) at.% Cr alloys are accomplished through high-energy ball milling with transitions in the microstructure mapped as a function of milling time. We demonstrate the multi-modal nature of the resulting nanocrystalline grain structure and its stability up to 1300 °C with the coarser grain size population correlated to transitions in crystallographic texture that result from the preferred slip systems in BCC W. Field-assisted sintering is employed to consolidate the alloy powders into bulk samples, which, due to the deliberately designed compositional features, are shown to retain ultrafine grain structures despite the presence of minor carbides formed during sintering due to carbon impurities in the ball-milled powders.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Practical colloidal processing of multication ceramics

The use of colloidal processing principles in the formation of ceramic materials is well appreciated for developing homogeneous material properties in sintered products, enabling novel forming techniques for porous ceramics or 3D printing, and controlling microstructure to enable optimized material properties. The solution processing of electronic ceramic materials often involves multiple cationic elements or dopants to affect microstructure and properties. Material stability must be considered through the steps of colloidal processing to optimize desired component properties. This review provides strategies for preventing material degradation in particle synthesis, milling processes, and dispersion, with case studies of consolidation using spark plasma sintering of these systems. The prevention of multication corrosion in colloidal dispersions can be achieved by utilizing conditions similar to the synthesis environment or by the development of surface passivation layers. The choice of dispersing surfactants can be related to these surface states, which are of special importance for nanoparticle systems. A survey of dispersant chemistries related to some common synthesis conditions is provided for perovskite systems as an example. Furthermore, these principles can be applied to many colloidal systems related to electronic and optical applications.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Development of Aluminum Feedstock for Additive Manufacturing

The rapid evolution of materials science and manufacturing technologies in recent years has offered new pathways to manipulate materials for bespoke manufacturing. Here we aim to develop feedstocks for applications such as radiator panels, fuel tanks, and structural components for outfitting. As a strong, light weight and thermally conductive material aluminum is ideal for these applications. An often-overlooked source of aluminum waste is food packaging used on the International Space Station. Reusing this waste stream will reduce the cost and logistics of regular sparing. In Space Manufacturing (ISM) will utilize this technology is such areas as sparing and outfitting. However, processing aluminum can present challenges, especially in the context of additive manufacturing and sintering, due to its high reactivity and tendency to form a tenacious oxide layer. Identifying appropriate binders and sintering profiles can overcome these challenges. Herein we present our work on obtaining aluminum powder derived from food packaging, binder selection for aluminum feedstock, and a demonstration of bound metal deposition printing.

aluminum↗
DOE OSTI2018

Performance and Reliability of Bonded Interfaces for High-Temperature Packaging

The presentation focuses on mechanical characterization, reliability evaluation and thermomechanical modeling of sintered silver bonded interface material. Two types of sintered silver material are being investigated in this study - first one based on nanosilver particles and the other one comprising of a mixture of nanosilver particles and micron-sized silver flakes. Shear stress results obtained as a function of displacement rates and ambient temperature are reported. Also, scanning acoustic microscopy images of samples for accelerated testing and thermomechanical modeling results are presented.

25 ENERGY STORAGE↗
DOE OSTI2019

Power Electronics Materials and Bonded Interfaces - Reliability and LIfetime

The emergence of wide-bandgap (WBG) devices in power electronics packages has brought significant attention to the reliability and thermal performance of the bonded interfaces. These interfaces, such as die-attach and substrate-attach, need to withstand the severe stress induced on them by the high-temperature (> 200 degrees C) operation of the WBG devices. Sintered silver and transient liquid phase alloys are key bonded interfaces that can enable the high-temperature operation of WBG devices, however it is essential to evaluate their reliability and study the possible failure mechanisms before they can be used in power electronics packages. Sintered silver is already being adopted in commercial packages as a die-attach, but large-area substrate-attach offers additional reliability challenges. In this project, we investigate the reliability of these interface materials under accelerated thermal cycling and correlate these results with finite element simulations to develop lifetime prediction models. The failure mechanisms of these bonded interfaces are also studied.

33 ADVANCED PROPULSION SYSTEMS↗