Spark Plasma Sintering of LiFePO4: AC Field Suppressing Lithium Migration.
Ontology highlight
ABSTRACT:
SUBMITTER: Luo N
PROVIDER: S-EPMC8198947 | biostudies-literature |
REPOSITORIES: biostudies-literature
Similar Datasets
Project description:Sodium superionic conductor (NASICON)-type lithium aluminum germanium phosphate (LAGP) has attracted increasing attention as a solid electrolyte for all-solid-state lithium-ion batteries (ASSLIBs), due to the good ionic conductivity and highly stable interface with Li metal. However, it still remains challenging to achieve high density and good ionic conductivity in LAGP pellets by using conventional sintering methods, because they required high temperatures (>800 °C) and long sintering time (>6 h), which could cause the loss of lithium, the formation of impurity phases, and thus the reduction of ionic conductivity. Herein, we report the utilization of a spark plasma sintering (SPS) method to synthesize LAGP pellets with a density of 3.477 g cm-3, a relative high density up to 97.6%, and a good ionic conductivity of 3.29 × 10-4 S cm-1. In contrast to the dry-pressing process followed with high-temperature annealing, the optimized SPS process only required a low operating temperature of 650 °C and short sintering time of 10 min. Despite the least energy and short time consumption, the SPS approach could still achieve LAGP pellets with high density, little voids and cracks, intimate grain-grain boundary, and high ionic conductivity. These advantages suggest the great potential of SPS as a fabrication technique for preparing solid electrolytes and composite electrodes used in ASSLIBs.
| S-EPMC6722947 | biostudies-literature
Project description:This work addresses the two great challenges of the spark plasma sintering (SPS) process: The sintering of complex shapes and the simultaneous production of multiple parts. A new controllable interface method is employed to concurrently consolidate two nickel gear shapes by SPS. A graphite deformable sub-mold is specifically designed for the mutual densification of both complex parts in a unique 40 mm powder deformation space. An energy efficient SPS configuration is developed to allow the sintering of a large-scale powder assembly under electric current lower than 900 A. The stability of the developed process is studied by electro-thermal-mechanical (ETM) simulation. The ETM simulation reveals that homogeneous densification conditions can be attained by inserting an alumina powder at the sample/punches interfaces, enabling the energy efficient heating and the thermal confinement of the nickel powder. Finally, the feasibility of the fabrication of the two near net shape gears with a very homogeneous microstructure is demonstrated.
| S-EPMC6416649 | biostudies-literature
Project description:The electric field has a large effect on the stoichiometry and grain growth of UO2+x during Spark Plasma Sintering. UO2+x is gradually reduced to UO2.00 as a function of sintering temperature and time. A gradient in the oxidation state within the pellets is observed in intermediate conditions. The shape of the gradient depends unequivocally on the direction of the electrical field. The positive surface of the pellet shows a higher oxidation state compared to the negative one. An area with larger grain size is found close to the positive electrode, but not in contact with it. We interpret these findings with the redistribution of defects under an electric field, which affect the stoichiometry of UO2+x and thus the cation diffusivity. The results bear implications for understanding the electric field assisted sintering of UO2 and non-stoichiometric oxides in general.
| S-EPMC5395941 | biostudies-literature
Project description:Spark plasma sintering (SPS) is currently widely applied to existing alloys as a means of further enhancing the alloys' figure of merit. However, the determination of the optimal sintering condition is challenging in the SPS process. This report demonstrates a systematic way to independently optimize the Seebeck coefficient S and the ratio of electrical to thermal conductivity (?/?) and thus achieve the maximum figure of merit zT = S(2)(?/?)T. Sb2-xInxTe3 (x = 0-0.2) were chosen as examples to validate the method. Although high sintering temperature and pressure are helpful in enhancing the compactness and electrical conductivity of pressed samples, the resultant deteriorated Seebeck coefficient and increasing thermal conductivity eventually offset the benefit. We found that the optimal sintering temperature coincides with temperatures at which the maximum Seebeck coefficient begins to degrade, whereas the optimal sintering pressure coincided with the pressure at which the ?/? ratio reaches a maximum. Based on this principle, the optimized sintering conditions were determined, and the zT of Sb1.9In0.1Te3 is raised to 0.92 at 600 K, showing an approximately 84% enhancement. This work develops a facile strategy for selecting the optimal SPS sintering condition to further enhance the zT of bulk specimens.
| S-EPMC4791595 | biostudies-literature
Project description:Recently, spark plasma sintering (SPS) has become an attractive method for the preparation of solid-state ceramics. As SPS is a pressure-assisted low-temperature process, it is important to examine the effects of temperature and pressure on the structural properties of the prepared samples. In the present study, we examined the correlation between the preparation conditions and the physical and structural properties of SiO2 glasses prepared by SPS. Compared with the conventional SiO2 glass, the SPS-SiO2 glasses exhibit a higher density and elastic modulus, but a lower-height first sharp diffraction peak of the X-ray total structure factor. Micro-Raman and micro-IR spectra suggest the formation of heterogeneous regions at the interface between the SiO2 powders and graphite die. Considering the defect formation observed in optical absorption spectra, reduction reaction mainly affects the densification of SPS-SiO2 glass. Hence, the reaction at the interface is important for tailoring the structure and physical properties of solid-state materials prepared by the SPS technique.
| S-EPMC9427799 | biostudies-literature
Project description:ZrB₂-based nanocomposites with and without carbon nanotubes (CNTs) as reinforcement were prepared at 1600 °C by spark plasma sintering. The effects of CNTs on the microstructure and mechanical properties of nano-ZrB₂ matrix composites were studied. The results indicated that adding CNTs can inhibit the abnormal grain growth of ZrB₂ grains and improve the fracture toughness of the composites. The toughness mechanisms were crack deflection, crack bridging, debonding, and pull-out of CNTs. The experimental results of the nanograined ZrB₂-CNTs composites were compared with those of the micro-grained ZrB₂-CNTs composites. Due to the small size and surface effects, the nanograined ZrB₂-CNTs composites exhibited stronger mechanical properties: the hardness, flexural strength and fracture toughness were 18.7 ± 0.2 GPa, 1016 ± 75 MPa, and 8.5 ± 0.4 MPa·m1/2, respectively.
| S-EPMC5456984 | biostudies-other
Project description:The bimodal-grain-size 7075 aluminium alloys containing varied ratios of large and small 7075 aluminium powders were prepared by spark plasma sintering (SPS). The large powder was 100 ± 15 ?m in diameter and the small one was 10 ± 5 ?m in diameter. The 7075 aluminium alloys was completely densified under the 500 °C sintering temperature and 60 MPa pressure. The large powders constituted coarse grain zone, and the small powders constituted fine grain zone in sintered 7075 aluminium alloys. The microstructural and microchemical difference between the large and small powders was remained in coarse and fine grain zones in bulk alloys after SPS sintering, which allowed for us to investigate the effects of microstructure and microchemistry on passive properties of oxide film formed on sintered alloys. The average diameter of intermetallic phases was 201.3 nm in coarse grain zone, while its vale was 79.8 nm in fine grain zone. The alloying element content in intermetallic phases in coarse grain zone was 33% to 48% higher than that on fine grain zone. The alloying element depletion zone surrounding intermetallic phases in coarse grain zone showed a bigger width and a more severe element depletion. The coarse grain zone in alloys showed a bigger electrochemical heterogeneity as compared to fine grain zone. The passive film formed on coarse grain zone had a thicker thickness and a point defect density of 2.4 × 1024 m-3, and the film on fine grain zone had a thinner thickness and a point defect density of 4.0 × 1023 m-3. The film resistance was 3.25 × 105 ?cm2 on coarse grain zone, while it was 6.46 × 105 ?cm2 on fine grain zone. The passive potential range of sintered alloys increased from 457 mV to 678 mV, while the corrosion current density decreased from 8.59 × 10-7 A/cm2 to 6.78 × 10-7 A/cm2 as fine grain zone increasing from 0% to 100%, which implied that the corrosion resistance of alloys increased with the increasing content of fine grains. The passive film on coarse grain zone exhibited bigger corrosion cavities after pitting initiation compared to that on fine grain zone. The passive film formed on fine grain zone showed a better corrosion resistance. The protectiveness of passive film was mainly determined by defect density rather than the thickness in this work.
| S-EPMC7412012 | biostudies-literature
Project description:AbstarctIn the drive to reduce the critical Heavy Rare Earth (HRE) content of magnets for green technologies, HRE-free Nd-Fe-B has become an attractive option. HRE is added to Nd-Fe-B to enhance the high temperature performance of the magnets. To produce similar high temperature properties without HRE, a crystallographically textured nanoscale grain structure is ideal; and this conventionally requires expensive "die upset" processing routes. Here, a Flash Spark Plasma Sintering (FSPS) process has been applied to a Dy-free Nd30.0Fe61.8Co5.8Ga0.6Al0.1B0.9 melt spun powder (MQU-F, neo Magnequench). Rapid sinter-forging of a green compact to near theoretical density was achieved during the 10 s process, and therefore represents a quick and efficient means of producing die-upset Nd-Fe-B material. The microstructure of the FSPS samples was investigated by SEM and TEM imaging, and the observations were used to guide the optimisation of the process. The most optimal sample is compared directly to commercially die-upset forged (MQIII-F) material made from the same MQU-F powder. It is shown that the grain size of the FSPS material is halved in comparison to the MQIII-F material, leading to a 14% increase in coercivity (1438 kA m-1) and matched remanence (1.16 T) giving a BHmax of 230 kJ m-3.
| S-EPMC5593872 | biostudies-literature
Project description:We analyze how the changes in the dimension of carbon nanomaterial (CNM) affect their catalytic conversion of secondary aliphatic alcohols. Carbon nanotubes (CNTs) consolidated by spark plasma sintering (SPS) were inactive in the conversion of secondary C3-C4 aliphatic alcohols because of the «healing» of defects in carbon structure during SPS. Gas-phase treatment of consolidated CNTs with HNO3 vapors led to their surface oxidation without destruction of the bulk structure of pellets. The oxygen content in consolidated CNTs determined by X-ray photoelectron spectroscopy increased from 11.3 to 14.9 at. % with increasing the oxidation time from 3 to 6 h. Despite the decrease in the specific surface area, the oxidized samples showed enhanced catalytic activity in alcohol conversion because of the increased number of oxygen radicals with unpaired electrons, which was established by electron paramagnetic resonance spectroscopy. We conclude that the structure of CNM determines the content and/or ratio of sp2 and sp3-hybridized carbon atoms in the material. The experimental and literature data demonstrated that sp3-hybridized carbon atoms on the surface are probably the preferable site for catalytic conversion of alcohols.
| S-EPMC7912505 | biostudies-literature
Project description:In this study, four composites with different ZrB2 content were made by the Spark Plasma Sintering (SPS/FAST) technique. The sintering process was carried out at 1373 K for 5 min under an argon atmosphere. The effect of ZrB2 reinforcing phase content on the density, microstructure, and mechanical and tribological properties of composites was investigated. The results were compared with experimental data obtained for 316L austenitic stainless steel without the reinforcing phase. The results showed that the ZrB2 content significantly affected the tested properties. With the increasing content of the ZrB2 reinforcing phase, there was an increase in the Young's modulus and hardness and an improvement in the abrasive wear resistance of sintered composites. In all composites, new fine precipitates were formed and distributed in the steel matrix and along the grain boundaries. Microstructural analysis (Scanning Electron Microscopy (SEM), Wavelength Dispersive Spectroscopy (WDS)) has revealed that the fine precipitates chromium contained chromium as well as boron.
| S-EPMC7321174 | biostudies-literature