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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

The Influence of Corundum Content and Sintering Temperature on the Mechanical Properties of CaO–ZrO{sub 2}–Al{sub 2}O{sub 3} Ceramic Composites

We have studied the mechanical properties (Vickers microhardness H{sub V} and fracture toughness K{sub C}) of nanostructured CaO–ZrO{sub 2}–Al{sub 2}O{sub 3} ceramic composites as dependent on the content of corundum (0 ≤ C{sub Al{sub 2O{sub 3}}} ≤ 25%) and the temperature of sintering (1250°C ≤ T{sub 1} ≤ 1500°C). Optimum value of the corundum content (C{sub Al{sub 2O{sub 3}}} = 5%) and optimum regime (T{sub 1} = 1300°C, 5 min; T{sub 2} = 1200°C, 4 h) of two-stage sintering are established, which favor attaining the best mechanical characteristics of ceramic composites (H{sub V} = 12.25 GPa, K{sub C} = 8.47 MPa m{sup 1/2}).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of Cobalt and Molybdenum Additives on the Structure and Shape Memory Parameters of Reaction-Sintered Porous Nickel Titanium Alloys

We have studied the structure and properties of porous nickel titanium (TiNi) alloys obtained upon reaction sintering of Ti and Ni powders with Co and Mo additives. It is established that Co and Mo doping additives retain the compaction of Ni powder achieved at the initial stage of sintering. The maximum deformation of porous samples loaded in the austenite state was observed upon adding Co, while the addition of Mo resulted in minimum deformation. The addition of Co leads to single-stage martensitic transformation in TiNi phase, while the addition of Mo leads to the two-stage transformation that is more homogeneous over the volume. Both Co and Mo additives lead to increase in the maximum accumulated strain due to the formation of favorably oriented stress-induced martensite and reoriented quench-induced martensite.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

A High-Performance Sintered Iron Electrode for Rechargeable Alkaline Batteries to Enable Large-Scale Energy Storage

Iron-based alkaline rechargeable batteries such as iron-air and nickel-iron batteries are particularly attractive for large-scale energy storage because these batteries can be relatively inexpensive, environment- friendly, and also safe. Therefore, our study has focused on achieving the essential electrical performance and cycling properties needed for the widespread use of iron-based alkaline batteries in stationary and distributed energy storage applications.We have demonstrated for the first time, an advanced sintered iron electrode capable of 3500 cycles of repeated charge and discharge at the 1-hour rate and 100% depth of discharge in each cycle, and an average Coulombic efficiency of over 97%. Such a robust and efficient rechargeable iron electrode is also capable of continuous discharge at rates as high as 3C with no noticeable loss in utilization. We have shown that the porosity, pore size and thickness of the sintered electrode can be selected rationally to optimize specific capacity, rate capability and robustness. As a result, these advances in the electrical performance and durability of the iron electrode enables iron-based alkaline batteries to be a viable technology solution for meeting the dire need for large-scale electrical energy storage.

25 ENERGY STORAGE↗
DOE OSTI2024

High-throughput, Ultra-fast Laser Sintering of Ceramics and AI Based Prediction on Processing-Microstructure-Property Relationships

We report high-throughput, ultra-fast laser sintering of alumina sample array and characterization of sample units’ microstructure and hardness, as a fast exploration of laser processing parameters, microstructure, and property. These experimental data were used to train machine-learning (ML) models. Accurate ML predictions were demonstrated for the processing-microstructure-property relationship, specifically in (1) prediction of the microstructure of alumina under arbitrary laser power and (2) prediction of the expected microstructure from the desired hardness. An independent neural network was developed and showed that ML-predicted microstructure had less than 10% error from real ones, in terms of projected hardness. To monitor the microstructure during laser sintering, we demonstrated an ML model that can instantaneously predict ceramic’s microstructure at the laser spot, based on the laser spot brightness. The ML model can generate more than 10 predictions per second, and the error in average grain size was less than 5% from the experimental observations.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Coupling of Spark Plasma Sintering with Advanced Modeling to Enable Process Scale-Up: Presentation to DOE-NE [Slides]

The research goal of this project is to develop at Idaho National Laboratory (INL) a first-of-its-kind Multiphysics Object-Oriented Simulation Environment (MOOSE)-based, multiscale, multiphysics spark plasma sintering (SPS) modeling and simulation code application, termed “Freya.” Freya will simulate the thermo-mechanical-electrical aspects of the SPS fabrication process and will be paired with lower length scale sub-models, such as phase-field, to predict the resulting microstructure. SPS is an advanced manufacturing process that can be used to solve a variety of material manufacturing challenges; however, this process is an extremely challenging problem for modeling and simulation. The SPS process is inherently multiphysics and multi-scale, with the macroscale electro-thermo-mechanical behavior linked intricately to the microstructure evolution of the part being sintered. Accurate modeling and simulation tools, specifically geared towards the SPS process, are needed to predict the influence of the multiple variables involved in the manufacturing process. Modeling and simulation accuracy is achieved and demonstrated through comparison to multiple validation experiments. The validation efforts for Freya include both separate effects and complete multiphysics SPS process experiments. One of the key benefits this Laboratory Directed Research & Development (LDRD) project offers stems from the emphasis placed on experimental validation of the Freya models, both on the individual length scales and of the final coupled multiscale multiphysics simulations. Experimental validation of Freya’s multiscale coupling capability provides the technical credibility necessary for potential future industry and research partners to accept the simulation predictions.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Machine-learning-based, online estimation of ceramic’s microstructure upon the laser spot brightness during laser sintering

The ceramic microstructure strongly influences its properties. During manufacturing, the online monitoring of microstructure is critical to ensure the desired material properties. So far, the microstructure on the relevant scale is usually characterized offline using scanning electron microscopy (SEM), which is time and cost-consuming. In this work, we demonstrate a cost-effective, machine learning (ML)-based approach to simulate the SEM micrographs in real-time from the laser spot brightness. We experimentally observed a strong correlation between the laser spot brightness and the corresponding microstructure at the exact locations. The brightness values obtained from thermal emission images and the corresponding SEM micrographs were used in the training datasets. The ML algorithm was a style-based conditional generative adversarial network (CGAN). After training, the ML model could generate high-fidelity microstructure images within 0.1 seconds based on in-situ captured brightness at the laser sintering spot. We used the average grain sizes as the metric to evaluate the accuracy of the ML-predicted micrographs. Here, the ML-predicted microstructures were in good agreement, with less than 5% in difference from the real SEM images. In conclusion, we demonstrate the cost-effective, online microstructure estimation during laser sintering with a simple setup (a camera, a regular computer, and the ML model).

08 HYDROGEN↗
DOE OSTI2022

In Situ Microstructure Characterization of Potassium Di-Phosphate (KDP) Densification during Cold Sintering

In order for ceramic additive manufacturing (AM) to achieve its full potential, it is increasingly important to develop a more rigorous understanding of fundamental phenomena that govern the kinetics and thermodynamics of ceramic AM processes. In the case of additive build processes, such as direct ink write and ceramic extrusion, methods for densifying the resulting green-body product need to be considered to complement the efficiencies of ceramics AM, itself. One densification route, at least for monolithic components, built layer-by-layer, is offered by the recently developed cold sintering process, whereby high-density final product is achieved through addition of a small amount of liquid solvent and application of modest uniaxial compressive stress at relatively low temperature. In situ small-angle X-ray scattering methods and X-ray diffraction have been applied to characterize and quantify the pore morphology evolution during cold sintering for a model system: potassium di-phosphate, KH 2 PO 4 (KDP). It is shown that both temperature and applied stress affect the densification rate, but stress has a stronger effect on the evolving morphology. A regime with an approximate linear densification rate can be identified, yielding an effective densification activation energy of ≈90 kJ/mol.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Unconventional Materials Processing Using Spark Plasma Sintering

Spark plasma sintering (SPS) has gained recognition in the last 20 years for its rapid densification of hard-to-sinter conventional and advanced materials, including metals, ceramics, polymers, and composites. Herein, we describe the unconventional usages of the SPS technique developed in the field. The potential of various new modifications in the SPS technique, from pressureless to the integration of a novel gas quenching system to extrusion, has led to SPS’ evolution into a completely new manufacturing tool. The SPS technique’s modifications have broadened its usability from merely a densification tool to the fabrication of complex-shaped components, advanced functional materials, functionally gradient materials, interconnected materials, and porous filter materials for real-life applications. The broader application achieved by modification of the SPS technique can provide an alternative to conventional powder metallurgy methods as a scalable manufacturing process. The future challenges and opportunities in this emerging research field have also been identified and presented.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Investigating Sintering Mechanisms for Additive Manufacturing of Conductive Traces

Additive Manufacturing (AM) processes enable the fabrication of miniaturized and flexible devices on complex geometries. This paper explores a hybrid additive manufacturing technology that integrates micro-extrusion and PICO-jetting methods. Conductive slurries and colloidal inks were optimized for their rheological properties to aid their precise deposition. A variety of conductive materials which include carbon, silver, nano-particle silver and nickel were deposited on both rigid (glass) and flexible (Kapton) substrates. The deposited traces were cured using two sintering mechanisms which include furnace heating and in situ laser irradiation. The effect of curing mechanism on the conductance of deposited traces was evaluated. The results indicated that traces could be cured successfully with the laser curing mechanism. Nickel and silver laser cured traces had lower resistivity than the furnace sintered traces. An increase in the laser power resulted in lower resistivity of the traces. The lowest resistivity was achieved at 40W laser power with a single laser pass. Scanning electron microscopy and energy dispersive spectroscopy were used to characterize the trace morphology and elemental compositions. Higher power laser curing resulted in better bonding of the particles. Laser cured samples had minimal oxidation to the cross-section region of the traces as compared to furnace cured samples. Furthermore, this research lays the foundation for the fabrication of electronic components for a high level of freeform 3D electronics using a hybrid additive manufacturing technology.

42 ENGINEERING↗
NASA NTRS1961

Sintering of Hafnium Carbide With A Fugitive Metal Binder

The sintering behavior of a mixture of hafnium carbide and 10 weight percent cobalt powders is presented. Compacts were heated in a vacuum at elevates temperatures for densification and removal of the cobalt. Densities of 99 percent of theoretical for the hafnium carbide were achieved with a maximum sintering temperature of 2200' C. Retained cobalt, grain size, microhardness, and weight loss were determined.

SINTERING↗
NASA NTRSDate not supplied

Microwave Sintering for Lunar Base Construction

Presentation to the Materials Science and Technology Conference 2023 on microwave sintering for the construction of a lunar base. Content includes an overview of NASA's goals, lunar materials, lunar construction, development and testing of the microwave sintered materials, and a summary of the work to date.

Microwave sintering↗
NASA NTRS2019

Manufacturing of Thermoset Polyimide Composites by Laser Sintering

Selective Laser Sintering (SLS) is an additive manufacturing technique that builds 3D models layer by layer using a laser to selectively melt cross sections in powdered polymeric materials, following sequential slices of the computer-aided design (CAD) model. SLS generally uses thermoplastic polymeric powders such as polyamides. The resultant 3D-printed objects are often weaker in their strength compared to traditionally processed materials, due to their higher porosity. This paper described the process development of using melt-processable imide oligomers terminated with reactive 4-phenylethynylphthalic anhydride (4-PEPA) to conduct laser sintering (LS). The first successful 3D-printing of high temperature RTM370 thermoset polyimide carbon fiber composites were further post-cured to promote additional crosslinking for achieving higher temperature (T g = 370°C) capability. Another novel imide oligomer, RTM385-SLS, formulated with a complex melt viscosity [ƞ*] of ~104-105 poise is also suitable for LS. RTM385-SLS resin powder was mixed with 20-25% of hexagonal boron nitride (h-BN) and subjected to LS to print out “Green” specimens which could be further post-cured to afford a thermally conductive but electrically insulating composites with high T g of 385 °C. The cured composite specimens were then subjected to mechanical testing, thermal conductivity and porosity measurements as well as SEM characterization.

additive Manufacturing↗
DOE OSTI2020

Ultra‐Uniform Nanocrystalline Materials via Two‐Step Sintering

Abstract Nanocrystalline materials with superior properties are of great interest. Much is discussed about obtaining nanograins, but little is known about maintaining grain‐size uniformity that is critical for reliability. An especially intriguing question is whether it is possible to achieve a size distribution narrower than what Hillert theoretically predicted for normal grain growth, a possibility suggested—for growth with a higher growth exponent—by the generalized mean‐field theory of Lifshitz, Slyozov, Wagner (LSW), and Hillert but never realized in practice. Following a rationally designed two‐step sintering route, it has been made possible in bulk materials by taking advantage of the large growth exponent in the intermediate sintering stage to form a uniform microstructure despite residual porosity, and freezing the grain growth thereafter while continuing densification to reach full density. The bulk dense Al 2 O 3 ceramic thus obtained has an average grain size of 34 nm and a size distribution much narrower than Hillert's prediction. Bulk Al 2 O 3 with a grain‐size distribution narrower than the particle‐size distribution of starting powders is also demonstrated, as are highly uniform bulk engineering metals (refractory Mo and W‐Re alloy) and complex functional ceramics (BaTiO 3 ‐based alloys with superior dielectric strength and energy capacity).

Dong, Yanhao↗
DOE OSTI2024

Laser‐Sintered Silver Metallization for Silicon Heterojunction Photovoltaic Cells

Herein, a novel metallization technique is reported for crystalline silicon heterojunction (SHJ) solar cells in which silver (Ag) fingers are printed on the SHJ substrates by dispensing Ag nanoparticle‐based inks through a needle and then sintered with a continuous‐wave carbon dioxide (CO 2 ) laser. The impact of the Ag ink viscosity on the line quality and the line resistance is investigated on three Ag inks with different viscosities. Increasing ink viscosity yields higher Ag contact heights, larger aspect ratios, and lower line resistance values. The Ag line height increases from less than a micrometer to ≈18.62 ± 3.48 μm with the increasing viscosity. Photoluminescence imaging shows that the low‐resistance Ag metal contacts obtained do not result in any passivation damage of the SHJ substrate. This is because the wavelength of light emitted from the CO 2 laser (i.e., 10.6 μm) leads to optical absorption in the Ag, but this light is effectively transparent to the transparent conductive oxide film, amorphous silicon films, and crystalline silicon substrate. Bulk resistivity values as low as 6.5 μΩ cm are obtained for the laser‐sintered Ag contact and printed using the Ag ink with the highest viscosity in this work.

Mousumi, Jannatul Ferdous↗
DOE OSTI2019

Effects of Sintering Temperature on Structural, Morphological and Magnetic Properties of Strontium Ferrite Nanoparticles

In the present investigation, structural, morphological and magnetic properties of SrFe{sub 2}O{sub 4} ferrite nanoparticles prepared by a sol–gel method were studied. The techniques used in this investigation were thermogravimetric analysis/differential thermal analysis (TGA/DTA), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrometry (FT-IR), vibrating sample magnetometry (VSM) and Curie temperature analysis. The average crystallite sizes of the SrFe{sub 2}O{sub 4} were calculated using the Scherrer formula and found in the range of 11–22 nm, and this can be attributed to the grain growth of the particles. The lattice parameter of SrFe{sub 2}O{sub 4} nanoparticles decreased from 6.64 to 6.51 nm as the sintering temperature was raised from 600 to 900 °C. FT-IR analysis confirmed that bands in the range 430–590 cm{sup − 1} are due to the stretching vibration of oxygen atom and metal ions (M–O) that is Fe–O confirming the formation of spinel ferrite. Surface morphology of the samples has been studied using FESEM. The elemental composition along with their relative ratios was given by EDX and was found to be in agreement with their initial calculated values. The saturation magnetization, magnetic coercivity and remanence increase with an increasing sintering temperature from 600 to 900 °C. The present study reports the Curie temperature with an amount of 551 °C of the synthesized strontium nanoferrites using the Faraday technique.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Structural, Infrared, Magnetic, and Electrical Properties of Ni{sub 0.6}Cd{sub 0.2}Cu{sub 0.2}Fe{sub 2}O{sub 4} Ferrites Synthesized Using Sol-Gel Method Under Different Sintering Temperatures

Ni{sub 0.6}Cd{sub 0.2}Cu{sub 0.2}Fe{sub 2}O{sub 4} ferrites were synthesized using sol-gel method under different sintering temperatures. XRD patterns with the Rietveld refinement indicate that samples crystallize in the cubic spinel structure. The increase of sintering temperature leads successively to the increase of lattice constant, average crystallite size, intensities of absorption bands, magnetization, and electrical conductivity of the prepared ferrites. Dielectric constants decrease with frequency and their behaviors have been investigated using the interfacial polarization theory predicted by Maxwell. The modulus analysis shows the presence of electrical relaxation phenomenon and non-Debye nature for the samples. An appropriate electrical equivalent circuit was used to analyze the Nyquist plots, and the results show that the conduction mechanism of the synthesized ferrites is mainly due to the grain boundary contribution.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Mechanical and Tribological Behavior of ZrB{sub 2}-TiB{sub 2} System Prepared by Mechanical Activation Spark Plasma Sintering Technique

ZrB{sub 2}-TiB{sub 2} system among varying amount of TiB{sub 2} loading (5, 10, 15, 20 and 30 wt.%) was prepared by mechanical activation spark plasma sintering at 2100 °C for 15-min dwell time under 50 MPa uniaxial pressure in argon atmosphere. The effect of the TiB{sub 2} loading on properties like physical, mechanical and tribological of the prepared samples was studied and evaluated with monolithic ZrB{sub 2} ceramic. Finally, almost fully dense samples (> 96% of theoretical density) were fabricated. Microstructural observation and XRD phase analysis of sintered compact revealed that TiB{sub 2} completely went into the ZrB{sub 2} structure by formation of solid solution with ZrB{sub 2} phase. ZrB{sub 2}-TiB{sub 2} (30 wt.%) showed the highest Vickers micro-hardness (H{sub V}) of 20.64 GPa at 10 N load. On addition of TiB{sub 2}, the fracture toughness of the ZrB{sub 2}-TiB{sub 2} improved up to 4.69 ± 0.43 MPa m{sup 1/2} over monolithic ZrB{sub 2} at 10 N load. At 10 N load, the scratch resistance coefficient, wear rate and wear resistance coefficient of ZrB{sub 2}-TiB{sub 2} (30 wt.%) reached a lowest value of 0.32, 0.35 mm{sup 3}/N m and 0.008, respectively, at 10 N load than other ZrB{sub 2} compositions.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of MWCNT Content on the Structure and Properties of Spark Plasma-Sintered Iron-MWCNT Composites Synthesized by High-Energy Ball Milling

The effect of multiwall carbon nanotube (MWCNT) content on the physical and mechanical properties of Fe-MWCNT composites has been studied. High-energy ball milling (HEBM) is employed to produce the composite powder; following this, spark plasma sintering (SPS) process has been adopted for powder consolidation. The composite powder and the sintered products were subjected to structural characterization by XRD. Microstructural studies were carried out by optical, field-emission scanning and high-resolution transmission electron microscopy. While Fourier transform infrared spectroscopic study of composites was done to understand the bonding characteristics, Raman spectroscopy was employed to assess the structural damage of MWCNT after HEBM. The effects of processing on the behavior of C-C, C-O and Fe-O bonds are studied by x-ray photoelectron spectroscopy. Microhardness and compressive strength of composites are also determined. Finally, magnetic and electrical properties of the composites were characterized. It was observed that optimized ball milling conditions help to preserve the structural identity of MWCNT. Consolidation by SPS insured good interfacial bonding. The microhardness and compression strength are significantly improved in MWCNT-reinforced iron matrix composite. MWCNT has appreciably improved the electrical conductivity of the composites. Tethering of MWCNT by iron oxide has led to appreciable improvement in saturation magnetization till 3 wt.% MWCNT.

36 MATERIALS SCIENCE↗