Zirconium Carbide Produced by Spark Plasma Sintering and Hot Pressing: Densification Kinetics, Grain Growth, and Thermal Properties.
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ABSTRACT: 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. 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.
Project description:Commercial zirconium carbide (ZrC) powder is consolidated by Spark Plasma Sintering (SPS). Processing temperatures range from 1650 to 2100 °C. Specimens with various density levels are obtained when performing single-die SPS at different temperatures. Besides the single-die tooling setup, a double-die tooling setup is employed to largely increase the actual applied pressure to achieve higher densification in a shorter processing time. In order to describe the densification mechanism of ZrC powder under SPS conditions, a power-law creep constitutive equation is utilized, whose coefficients are determined by the inverse regression of the obtained experimental data. The densification of the selected ZrC powder is shown to be likely associated with grain boundary sliding and dislocation glide controlled creep. Transverse rupture strength and microhardness of sintered specimens are measured to be up to 380 MPa and 24 GPa, respectively. Mechanical properties are correlated with specimens' average grain size and relative density to elucidate the co-factor dependencies.
Project description:A new ceramic sintering approach employing plastic deformation as the dominant mechanism is proposed, at low temperature close to the onset point of grain growth and under high pressure. Based on this route, fully dense boron carbide without grain growth can be prepared at 1,675-1,700 °C and under pressure of (≥) 80 MPa in 5 minutes. The dense boron carbide shows excellent mechanical properties, including Vickers hardness of 37.8 GPa, flexural strength of 445.3 MPa and fracture toughness of 4.7 MPa•m(0.5). Such a process should also facilitate the cost-effective preparation of other advanced ceramics for practical applications.
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.
Project description:A new two-step densification method for wooden materials entitled hot isostatic pressing (HIP) is proposed. This method has the advantage over previous densification methods that can achieved almost the full densification of wood, reaching values up to 1.47 kg/m3, which exceeds any value ever reported for a hardwood species. Furthermore, it can preserve about 35% of the original volume, in comparison to other methods which typically can preserve only 20% of the volume. Although not tested in this investigation, in principle, the HIP method should be capable of densifying any shape of wood including circular and tubular cross sections because the main densification mechanism is based on gas pressure that is equally exerted in the entire surface, rather than localized mechanical compression, which can only be effective with rectangular cross sections. In the first stage of the two-step proposed method, the compressive strength of the anatomical wood structure is reduced by delignification, and, in the second, a full densification is achieved by hot isostatic pressing under argon atmosphere. Three tropical hardwood species with distinct anatomical characteristics and properties were used to test the method. The HIP-densified wood's microstructural, chemical, physical, and mechanical properties were assessed. Apart from the high densification values and volume preservation, the results indicate that proposed method was effective for all the tested species, showing homogenous density patterns, stable densification without noticeable shape recovery, and enhanced mechanical properties. Future research should test the HIP method in softwoods and consider the ring orientation in order to enhance the control of the densified geometry.
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.
Project description:With the rapid development of electronics and portable devices, polymer nanocomposites with high through-plane thermal conductivity (TC) are urgently needed. In this work, we fabricated graphene nanosheets-perfluoroalkoxy (GNs-PFA) composite sheets with high through-plane TCs via hot-pressing followed by mechanical machining. When the GNs content exceeded 10 wt%, GNs were vertically aligned in the PFA matrix, and the through-plane TCs of nanocomposites were 10-15 times higher than their in-plane TCs. In particular, the composite with 30 wt% GNs exhibited a through-plane TC of 25.57 W/(m·K), which was 9700% higher than that of pure PFA. The composite with 30 wt% GNs was attached to the surface of a high-power light-emitting diode (LED) to assess its heat-dissipation capability. The composite with vertically aligned GNs lowered the LED surface temperature by approximately 16 °C compared with pure PFA. Our facile, low-cost method allows for the large-scale production of GNs-PFA nanocomposites with high through-plane TCs, which can be used in various thermal-management applications.
Project description:To fully densify a powder compact, we should avoid two things: (i) entrapment of insoluble gases within pores and (ii) entrapment of isolated pores within grains. This paper describes general directions for promoting full densification in view of the above two points. Emphasis is placed on ways to potentially prevent pore entrapment in terms of grain growth control. Currently available techniques that can enhance densification while suppressing grain growth are briefly described, and their major mechanisms are discussed.
Project description:[1] Sintering and densification are ubiquitous processes influencing the emplacement of both effusive and explosive products of volcanic eruptions. Here we sinter ash-size fragments of a synthetic National Institute of Standards and Technology viscosity standard glass at temperatures at which the resultant melt has a viscosity of ∼108-109 Pa.s at 1bar to assess sintering dynamics under near-surface volcanic conditions. We track the strength recovery via uniaxial compressive tests. We observe that volcanic ash sintering is dominantly time dependent, temperature dependent, and grain size dependent and may thus be interpreted to be controlled by melt viscosity and surface tension. Sintering evolves from particle agglutination to viscous pore collapse and is accompanied by a reduction in connected porosity and an increase in isolated pores. Sintering and densification result in a nonlinear increase in strength. Micromechanical modeling shows that the pore-emanated crack model explains the strength of porous lava as a function of pore fraction and size.
Project description:The dependencies of the enhanced thermomechanical properties of zirconium carbide (ZrCx) with sample purity and stoichiometry are still not understood due to discrepancies in the literature. Multiple researchers have recently reported a linear relation between the carbon to zirconium atomic ratio (C/Zr) and the lattice parameter, in contrast with a more established relationship that suggests that the lattice parameter value attains a maximum value at a C/Zr ~ 0.83. In this study, the relationship between C/Zr atomic ratio and the lattice parameter is critically assessed: it is found that recent studies reporting the thermophysical properties of ZrCx have unintentionally produced and characterised samples containing zirconium oxycarbide. To avoid such erroneous characterization of ZrCx thermophysical properties in the future, we propose a method for the accurate measurement of the stoichiometry of ZrCx using three independent experimental techniques, namely: elemental analysis, thermogravimetric analysis and nuclear magnetic resonance spectroscopy. Although a large scatter in the results (ΔC/Zr = 0.07) from these different techniques was found when used independently, when combining the techniques together consistent values of x in ZrCx were obtained.