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At least 19 records

Ultra-low thermal conductivities of hot-pressed attapulgite and its potential as thermal insulation material

In the past, there have been very few reports on thermal properties of attapulgite which is a widely used clay mineral. In this work, we report on extremely low thermal conductivities in attapulgite samples synthesized by hot-pressing. Attapulgite powder was hot-pressed at different temperatures into bulk samples, and a systematic study was conducted on the microstructures and thermal properties. Differential scanning calorimetry analysis shows that hot-pressing induces a rapid dehydration of the attapulgite powders. X-ray diffraction data and scanning/transmission electron microscopy reveal that the hot-pressed attapulgite features high porosity and complex microstructures, including an amorphous phase. As a result, the hot-pressed attapulgite exhibits thermal conductivity less than 2.5Wm -1 K -1 up to 600 °C. For one sample with porosity of 45.7%, the thermal conductivity is as low as 0.34Wm -1 K -1 at 50 °C. Finally, this suggests the potential of hotpressed attapulgite as a candidate for thermal barrier materials.

36 MATERIALS SCIENCE↗

Consolidation of composite cathodes with NCM and sulfide solid-state electrolytes by hot pressing for all-solid-state Li metal batteries

In this study, hot pressing was evaluated as a method of cell fabrication to increase the energy density of next-generation all-solid-state batteries with NCM active material and sulfide solid-state electrolyte. Hot pressing involves consolidating glassy sulfide electrolyte by the application of pressure at a temperature above the electrolyte’s glass transition temperature. Typically, cell stacks are formed at room temperature and retain 15–30% porosity that limits cell energy density. On the other hand, the porosity of hot-pressed cell stacks is reduced to less than 10%. The electrochemical function of hot-pressed cathode composites was assessed as a function of active material and solid-state electrolyte compositions. Specifically, LiNi 0.85 Co 0.10 Mn 0.05 O 2 and LiNi 0.6 Co 0.2 Mn 0.2 O 2 were studied in combination with either glassy Li 7 P 3 S 11 , glassy Li 3 PS 4 , or β-Li 3 PS 4 solid-state electrolytes. Cathode composites composed of LiNi 0.6 Co 0.2 Mn 0.2 O 2 and Li 3 PS 4 maintained the best function after hot pressing at 200 °C and 370 MPa for 10 min. It was found that LiNi 0.6 Co 0.2 Mn 0.2 O 2 ’s resistance to microcracking and the inherent stability of Li 3 PS 4 ’s fully de-networked local structure are critical to maintain good electrochemical function after hot pressing. Furthermore, the results of this study show that hot pressing reduces porosity in the cathode composite and confirms the feasibility of cathode support of consolidated, reinforced glass separators.

25 ENERGY STORAGE↗

Low-resistivity bulk silicon prepared by hot-pressing boron- and phosphorus-hyperdoped silicon nanocrystals

Technologically important low-resistivity bulk Si has been usually produced by the traditional Czochralski growth method. We now explore a novel method to obtain low-resistivity bulk Si by hot-pressing B- and P-hyperdoped Si nanocrystals (NCs). In this work bulk Si with the resistivity as low as ∼ 0.8 (40) mΩ•cm has been produced by hot pressing P (B)-hyperdoped Si NCs. The dopant type is found to make a difference for the sintering of Si NCs during the hot pressing. Bulk Si hot-pressed from P-hyperdoped Si NCs is more compact than that hot-pressed from B-hyperdoped Si NCs when the hot-pressing temperature is the same. This leads to the fact that P is more effectively activated to produce free carriers than B in the hot-pressed bulk Si. Compared with the dopant concentration, the hot-pressing temperature more significantly affects the structural and electrical properties of hot-pressed bulk Si. With the increase of the hot-pressing temperature the density of hot-pressed bulk Si increases. The highest carrier concentration (lowest resistivity) of bulk Si hot-pressed from B- or P-hyperdoped Si NCs is obtained at the highest hot-pressing temperature of 1050 °C. The mobility of carriers in the hot-pressed bulk Si is low (≤ ∼ 30 cm{sup -2}V{sup -1}s{sup -1}) mainly due to the scattering of carriers induced by structural defects such as pores.

36 MATERIALS SCIENCE↗

Fractographical characterization of hot pressed and pressureless sintered AlN-doped ZrB{sub 2}–SiC composites

In this paper, ZrB{sub 2}–SiC composites doped with 0–5 wt.% AlN were prepared by a low pressure hot pressing as well as a pressureless sintering methods at 1900 °C for 2 h. The influence of aluminum nitride addition on the sinterability and microstructure development of such ceramic composites was studied by a fractographical approach. The results revealed that only 1 wt.% AlN can aid the densification process of the hot pressed ceramic composite via the liquid phase sintering mechanism due to the formation of nano-scale metakaolinite spinel layers. In the pressureless sintering method, adding more AlN can increase the formation of gaseous products which raised the amount of porosities in the final microstructure. The formation of nano-graphite phase in the hot pressing process, the formation of Al{sub 2}OC in the pressureless sintering process, and the formation of BN in the both processes were disclosed by X-ray diffraction, SEM and TEM analyses. - Highlights: • The effect of AlN addition on densification of ZrB{sub 2}–SiC composites was studied. • AlN promotes the densification in hot pressed samples by liquid phase formation. • A fully dense composite was obtained by adding 1 wt.% AlN in hot pressing process. • In pressureless sintering, more AlN content intensifies the formation of porosities.

36 MATERIALS SCIENCE↗

Hot Press Market Study

A study has been conducted to identify vendors for a hot press suitable for meeting program deliverables chiefly to achieve a higher TRL for the material and process. This study identities the high level specifications for the hot press which must be able to produce samples to support both the fabrication method development and fabricate full size components for testing to demonstrate success. Three vendors capable of meeting hot press specifications were contacted and estimates were obtained. A comparison of the equipment was performed and a recommendation is made for equipment acquisition.

36 MATERIALS SCIENCE↗

Microstructure and Properties of Mn-Cu-Based Damping Alloys Prepared by Ball Milling and Hot-Press Sintering

A Mn-Cu-based damping alloy with a nominal composition of 70Mn-24Cu-3Zn-3Al (at.%) was prepared by ball milling of pure elemental powders and subsequent hot-press sintering of powder mixture at 750 and 825 °C for 2 h. For comparison, this alloy was also prepared by induction melting technology and then homogenized at 850 °C for 24 h. Further, they were aged at 430 °C for 2 h. The microstructure, damping capacity and microhardness of the hot-press-sintered and induction-melted alloys have been investigated. The results show that the microstructure of the powder mixture upon ball milling mainly comprises convoluted composite particles containing α-Mn and γ-Cu phases, and isolated α-Mn ones around. The high compactness of the alloys is obtained after hot-press sintering (94.8 and 98.6% at 750 and 825 °C, respectively). At a holding temperature of 750 °C, the microstructure of the alloy is primarily composed of γ-MnCu, γ-CuMn and α-Mn grains. With increasing the target temperature to 825 °C, the single γ-MnCu solid solution has been formed in the alloy by diffusion of Mn etc. into γ-Cu lattices. The hot-press-sintered alloys (especially at 825 °C) possess relatively high damping capacity although which is still lower than that of induction-melted one. In contrast, the microhardness of the hot-press-sintered alloys (especially at 750 °C) is obviously higher than that of the induction-melted one.

36 MATERIALS SCIENCE↗

Additive-free hot-pressed silicon carbide ceramics-A material with exceptional mechanical properties

Densification of silicon carbide without any sintering aids by hot-pressing and rapid hot pressing was investigated. Full density (>99% t.d.) has been reached at 1850 °C, a temperature of at least 150-200 °C lower compared to the up to now known solid state sintered silicon carbide powders. Silicon carbide was freeze granulated and heat treated prior the densification. Furthermore, evolution of microstructure, mechanical properties and creep behavior were evaluated and compared to reference ceramics from as received silicon carbide powder as well as those of commercial one. Novel method results in dense ceramics with Vickers hardness and indentation fracture toughness of 29.0 GPa and 5.25 MPam 1/2 , respectively. Moreover, the creep rate of 3.8 x 10 –9 s –1 at 1450 °C and the load of 100 MPa is comparable to the commercial α-SiC solid state sintered at 2150 °C.

36 MATERIALS SCIENCE↗

Quantitative analysis of inclusion distributions in hot pressed silicon carbide

ABSTRACT Depth of penetration measurements in hot pressed SiC have exhibited significant variability that may be influenced by microstructural defects. To obtain a better understanding regarding the role of microstructural defects under highly dynamic conditions; fragments of hot pressed SiC plates subjected to impact tests were examined. Two types of inclusion defects were identified, carbonaceous and an aluminum-iron-oxide phase. A disproportionate number of large inclusions were found on the rubble, indicating that the inclusion defects were a part of the fragmentation process. Distribution functions were plotted to compare the inclusion populations. Fragments from the superior performing sample had an inclusion population consisting of more numerous but smaller inclusions. One possible explanation for this result is that the superior sample withstood a greater stress before failure, causing a greater number of smaller inclusions to participate in fragmentation than in the weaker sample.

36 MATERIALS SCIENCE↗

The impact of hot-press conditions on the durability of polymer electrolyte membrane fuel cells

The proton exchange membrane integrity can be compromised during hot-press fabrication of membrane electrode assemblies (MEAs) causing premature cell failures during operation. In this work, infrared (IR) thermography was used as a diagnostic tool to spatially visualize hydrogen (H 2 ) crossover and identify process-induced-membrane irregularities (PIMs). These irregularities were identified as seed locations for MEA failures. Fine tuning of hot-press conditions was used to mitigate premature cell failures informed by accelerated stress testing (AST). The impact of PIMs on the initial performance, high-frequency resistances, open-circuit voltage, and H 2 crossover are reported. Nafion XL and 212 membranes, hot-pressed with a force of 16 kg/cm 2 and temperature of 120°C, were found to be consistently irregularity-free. Irregularity-free MEAs using Nafion 211, 212, and XL membranes demonstrated AST lifetime improvements of 58, 64 and 400%, respectively, compared to those fabricated with non-optimized conditions. In conclusion, this work highlights the importance of fabrication parameters on premature cell failures.

08 HYDROGEN↗

Hot Pressing of Reinforced Li-NMC All-Solid State Batteries with Sulfide Glass Electrolyte

The performance of solid-state batteries (SSBs) with sulfide solid-state electrolytes (SSEs) is limited because they are 10 - 30% porous. Porosity limits energy density of the composite cathode and provides a conduit for Li-metal deposits through the separator if operating specifications (e.g. current density, operating temperature, and pressure) are not strictly controlled. This project focused on demonstrating that hot press cell processing and appropriately formulated sulfide glass SSEs can help eliminate porosity to enable SSBs with energy density of ≥ 350 Wh/kg. The objective of the project was to research, develop, and test SSBs capable of achieving program performance metrics by implementing appropriately formulated sulfide glass SSEs and hot press cell processing in a dry room environment. In the composite cathode, hot pressing helps eliminate porosity to increase energy density by enabling thick composite cathodes with high active material loading. In the separator, hot pressing helps eliminate porosity that may otherwise provide a conduit for Li metal deposits to short the cell.

25 ENERGY STORAGE↗

Fabrication and microstructures of functional gradient SiBCN–Nb composite by hot pressing

A functional gradient material with five layers composed of SiBCN ceramic and niobium (Nb) was prepared successfully by hot pressing. The phase composition, morphology features and microstructures were investigated in each layer of the gradient material. The Nb-containing compounds involving NbC, Nb{sub 6}C{sub 5}, Nb{sub 4}C{sub 3}, Nb{sub 5}Si{sub 3} and NbN increase with the volume fraction of Nb increasing in the sub-layer. They are randomly scattered (≤ 25 vol.% Nb), then strip-like, and finally distribute continuously (≥ 75 vol.% Nb). The size of BN(C) and SiC grains in Nb-containing layers is larger than in 100% SiBCN layer due to the loss of the capsule-like structures. No distinct interfaces form in the transition regions indicating the gradual changes in phase composition and microstructures. - Highlights: • A functional gradient SiBCN–Nb material was prepared successfully by hot pressing. • Phase composition, morphology features and microstructures were investigated. • Thermodynamic calculation was used to aid in the phase analysis. • No distinct interfaces form typical of the functional gradient material.

36 MATERIALS SCIENCE↗

The study of dielectric, pyroelectric and piezoelectric properties on hot pressed PZT-PMN systems

Hot uniaxial pressing technique has been adopted for the densification of PZT-PMN system with an aim to yield dense ceramics and to lower the sintering temperature and time for achieving better and reproducible electronic properties. The ceramics having >97% theoretical density and micron size grains are investigated for their dielectric, pyroelectric and piezoelectric properties. The effect of Li and Mn addition has also been studied.

36 MATERIALS SCIENCE↗

Zirconium Carbide Produced by Spark Plasma Sintering and Hot Pressing: Densification Kinetics, Grain Growth, and Thermal Properties

Spark plasma sintering (SPS) has been employed to consolidate a micron-sized zirconium carbide (ZrC) powder. ZrC pellets with a variety of relative densities are obtained under different processing parameters. The densification kinetics of ZrC powders subjected to conventional hot pressing and SPS are comparatively studied by applying similar heating and loading profiles. Due to the lack of electric current assistance, the conventional hot pressing appears to impose lower strain rate sensitivity and higher activation energy values than those which correspond to the SPS processing. A finite element simulation is used to analyze the temperature evolution within the volume of ZrC specimens subjected to SPS. The control mechanism for grain growth during the final SPS stage is studied via a recently modified model, in which the grain growth rate dependence on porosity is incorporated. Finally, the constant pressure specific heat and thermal conductivity of the SPS-processed ZrC are determined to be higher than those reported for the hot-pressed ZrC and the benefits of applying SPS are indicated accordingly.

36 MATERIALS SCIENCE↗

Fabrication, Microstructures, and Properties of 50 vol.% SiCp/6061Al Composites via Hot Pressing

Nearly fully dense 50 vol.% SiCp/6061Al composites were fabricated via hot pressing (HPing) at temperatures ranging from 610 to 650 °C, with the axial load and holding time fixed as 25 MPa and 120 min, respectively. The interfacial reactions, microstructures, and properties of the SiCp/Al alloy were studied. The interface reaction between SiCp and the Al alloy was suppressed at annealing temperatures of 620 °C and below; however, the reaction intensified as the annealing temperature increased, producing Al{sub 4}C{sub 3}, Si, and Mg{sub 2}Si. With an increase in HPing temperature from 610 to 630 °C, the 6061Al alloy melted and gradually filled the pores in the SiC particles under the applied load. The density, bending strength, and thermal conductivity (TC) of the composites increased, whereas the coefficient of thermal expansion (CTE) of the composites decreased. With an increase in HPing temperature increased from 630 to 650 °C, the 6061Al alloy melt leaked through the sintered bodies, resulting in the microstructural degradation and property reduction of the composites. The 50 vol.% SiCp/6061Al composites fabricated by HPing at 630 °C exhibited optimal comprehensive properties [bending strength, 332.4 MPa; TC, 186.3 W(m K){sup −1}; and CTE, 7.9 × 10{sup −6}/°C (20-100 °C)], which were attributed to the highest relative density and the best SiCp/Al interfacial structure of the composites.

36 MATERIALS SCIENCE↗

Chemical and Electrochemical Characterization of Hot–Pressed Li 6 PS 5 Cl Solid State Electrolyte: Operating Pressure–Invariant High Ionic Conductivity

Sulfide solid state electrolytes (SSE) are among the most promising materials in the effort to replace liquid electrolytes, largely due to their comparable ionic conductivities. Among the sulfide SSEs, Argyrodites (Li 6 PS 5 X, X=Cl, Br, I) further stand out due to their high theoretical ionic conductivity (~1×10 –2 S cm –1 ) and interfacial stability against reactive metal anodes such as lithium. Generally, solid state electrolyte pellets are pressed from powder feedstock at room temperature, however, pellets fabricated by cold pressing consistently result in low bulk density and high porosity, facilitating interfacial degradation reactions and allowing dendrites to propagate through the pores and grain boundaries. Here, we demonstrate the mechanical and electrochemical implications of hot-pressing standalone LPSCl SSE pellets with near-theoretical ionic conductivity, superior cycling performance, and enhanced mechanical stability. X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and x-ray diffraction spectroscopy (XRD) analysis reveal no chemical changes to the Argyrodite surface after hot pressing up to 250°C. Furthermore, we use electrochemical impedance spectroscopy (EIS) to understand mechanical stability of Argyrodite SSE pellets as a function of externally applied pressure, demonstrating for the first time pressed standalone Argyrodite pellets with near-theoretical conductivities at external pressures below 14 MPa.

25 ENERGY STORAGE↗

Preparation of Nb{sub 3}Al Superconducting Tapes by a Powder-in-Tube Method Combined with Hot-Pressed Sintering

The precursors of Nb-Al tape were fabricated by a powder-in-tube (PIT) technique. Supersaturated solid solutions of Nb-Al powder were obtained by high-energy ball milling, followed by a powder-in-tube process to prepare series of Nb{sub 3}Al precursor tapes. Compared with sintering under normal pressure, the hot-pressing sintering greatly increased the critical current density of the tapes. The results showed that the Nb{sub 3}Al tapes prepared via the powder-in-tube method and hot-pressed sintering could significantly improve the J{sub c} performance, and the value of J{sub c} (8 K, 0 T) was higher than 6 × 10{sup 5} A/cm{sup 2}. The Nb{sub 3}Al tapes after pressing under the pressure of 20 MPa and sintering at 950 {sup ∘}C for 3 h had the best magnetic flux pinning performance, and the sample reached the maximum flux pinning force (F{sub p,max}) of 3.28109 N/m{sup 3} in the magnetic field of 2.2 T.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A Facile, Low-Cost Hot-Pressing Process for Fabricating Lithium-Sulfur Cells with Stable Dynamic and Static Electrochemistry

Lithium–sulfur batteries are among the most promising low-cost, high-energy-density storage devices. However, the inability to host a sufficient amount of sulfur in the cathode while maintaining good electrochemical stability under a lean electrolyte condition has limited the progress. The main cause of these challenges is the sensitivity of the sulfur cathode to the cell-design parameters (i.e., the amount of sulfur and electrolyte) and the experimental testing conditions (i.e., cycling rates and analysis duration). Here, a hot-pressing method is presented that effectively encapsulates a high amount of sulfur in the cathode within only 5 s, resulting in high sulfur loading and content of, respectively, 10 mg cm -2 and 65 wt%. The hot-pressed sulfur (HPS) cathodes exhibit superior dynamic and static electrochemical performance under a broad cycling-rate (C/20–1C rates) and low electrolyte/sulfur ratio (6 µL mg -1 ) conditions. The dynamic cell stability is demonstrated by high gravimetric and areal capacities of, respectively, 415–730 mAh g -1 and 7–12 mAh cm -2 at C/20–1C rates with a high capacity retention of over 70% after 200 cycles. As a result, the static cell stability is demonstrated by excellent shelf life with low self-discharge and stable cycle life on storing for over one year.

25 ENERGY STORAGE↗

Characterization of hot-pressed von Alpen type NASICON ceramic electrolytes

The Na-ion conducting solid electrolyte NASICON is a promising solid state electrolyte (SSE) for use in Na based electrochemical systems. The effects of particle morphology and synthesis of von Alpen type NASICON via hot-pressing were investigated. Spray dried particles were shown to improve mechanical and electrochemical properties. X-ray diffraction, scanning electron microscopy, impulse excitation measurements, Vickers hardness, and impedance spectroscopy were used to correlate relationships between phase purity, microstructure, mechanical properties, and electrochemical properties. Scanning electron microscopy showed the presence of a glass phase as between 19.08% and 28.23% area percentage and a ZrO 2 phase between 0.46% and 3.51% area percentage in the hot-pressed samples. Impulse excitation showed elastic modulus varying from 83.65 to 97.65 GPa. The first values of Poisson's ratio and shear modulus of NASICON are reported as between 0.23 and 0.26 and 33.87 to 38.79 GPa, respectively. Vickers hardness and fracture toughness measurements showed Vickers hardness ranging from 4.30 to 4.68 GPa and fracture toughness ranging from 1.05 to 1.09 MPa m ½ . Impedance spectroscopy showed grain conductivities ranging from 1.023 to 1.287 mS/cm, with grain boundary resistance percentages between 73.22 and 47.5%. Total conductivities ranged from 0.292 to 0.596 mS/cm, with 0.596 mS/cm being achieved at room temperature for the spray dried powders with lower grain boundary resistance percentages.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗