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At least 181 records · Page 10

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↗

Characterization of the porous structures of the green body and sintered biomedical titanium scaffolds with micro-computed tomography

The present research was aimed at gaining an understanding of the porous structure changes from the green body through water leaching and sintering to titanium scaffolds. Micro-computed tomography (micro-CT) was performed to generate 3D models of titanium scaffold preforms containing carbamide space-holding particles and sintered scaffolds containing macro- and micro-pores. The porosity values and structural parameters were determined by means of image analysis. The result showed that the porosity values, macro-pore sizes, connectivity densities and specific surface areas of the titanium scaffolds sintered at 1200 °C for 3 h did not significantly deviate from those of the green structures with various volume fractions of the space holder. Titanium scaffolds with a maximum specific surface area could be produced with an addition of 60–65 vol% carbamide particles to the matrix powder. The connectivity of pores inside the scaffold increased with rising volume fraction of the space holder. The shrinkage of the scaffolds prepared with > 50 vol% carbamide space holder, occurring during sintering, was caused by the reductions of macro-pore sizes and micro-pore sizes as well as the thickness of struts. In conclusion, the final porous structural characteristics of titanium scaffolds could be estimated from those of the green body. - Highlights: •Porous structures of green body and sintered titanium scaffolds was studied. •Porous structures of both samples were quantitatively characterized with micro-CT. •Porous structures of scaffolds could be controlled from the green body. •Shrinkage mechanisms of titanium scaffolds during sintering was established.

36 MATERIALS SCIENCE↗

Structural evolution, sintering behavior and microwave dielectric properties of (1−x)Li{sub 2}TiO{sub 3} + xLiF ceramics

Graphical abstract: - Highlights: • Structure, sinterability and dielectric properties of LiF-doped Li{sub 2}TiO{sub 3} were studied. • Li{sub 2}TiO{sub 3} can be densitied (TD 98%) at lower sintering temperature by LiF additions. • Excellent microwave dielectric properties could be obtained. - Abstract: Structural evolution, sintering behavior, and microwave dielectric properties of (1−x)Li{sub 2}TiO{sub 3} + xLiF (0.05 ≤ x ≤ 0.70) ceramics have been studied by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Raman spectra, thermal dilatometry and microwave resonant measurement at the frequency of about 7–11 GHz. The results show that Li{sub 2}TiO{sub 3} can form limited solid solution with LiF (x ≤ 0.4) and LiF second phase appeared when x{sup 3}0.5. The structure of the solid solution transformed from ordered monoclinic phase (β-Li{sub 2}TiO{sub 3} (ss)) to disordered cubic rock salt (α-Li{sub 2}TiO{sub 3} (ss)) when x{sup 3}0.15. The presence of short range ordering was confirmed for the cubic phase. The sinterability was considerably improved by doping with LiF. Densified ceramics with about 95–98% theoretical density could be obtained for the doped compositions after sintering at 900–1150 °C/2 h. An optimized microwave dielectric properties with ε{sub r} of ∼23.6, Q × f of ∼108,000 GHz and τ{sub f} of ∼4.2 ppm/°C could be obtained for the x = 0.1 composition after sintering at 1100 °C/2 h.

36 MATERIALS SCIENCE↗

Reactive sintering of tungsten-doped high strength ZrB{sub 2}–SiC porous ceramics using metastable precursors

Graphical abstract: - Highlights: • Tungsten-doped porous ZrB{sub 2}–SiC specimens were fabricated by reactive sintering. • Both sintering and mechanical properties were improved by doping with tungsten. • Optimum concentration to obtain high mechanical properties was W/Zr (mol) = 0.05. • Sintering might be promoted by self-accelerated diffusion. • Mechanical properties might be improved by solid solution strengthening. - Abstract: Tungsten-doped porous ZrB{sub 2}-20 vol.% SiC specimens with a high strength skeleton were fabricated by reactive sintering using metastable reactants, i.e., as-synthesized amorphous hydrous ZrO{sub 2}–WO{sub 3}/ZrO{sub 2}, amorphous boron, nanocarbon, and β-SiC. Doping with tungsten clearly promoted sintering and improved mechanical properties; the optimum tungsten concentration to obtain high mechanical properties was investigated. A single-phase solid solution (Zr,W)B{sub 2} was formed in the specimens with tungsten. We suggest that sintering was promoted by self-accelerated diffusion owing to the formation of point defects caused by doping with tungsten. The improvement of mechanical properties could be attributed to solid solution strengthening.

36 MATERIALS SCIENCE↗

Spark Plasma Sintering of high-density fine-grained Y2.5Nd0.5Al5O12+SiC composite ceramics

Highlights: • YAG + (10, 20) wt.% α-SiC high-density ceramics obtained by SPS. • YAG + α-SiC ceramics have a more fine-grained structure than pure garnet. • The optimal sintering temperature of YAG + SiC ceramics is lower than that of garnet. • Introduction of α-SiC particles creates internal stress fields in garnet. • Introduction of α-SiC particles results in lower sintering activation energy of garnet. - Abstract: Spark Plasma Sintering (SPS) has been used to produce samples of fine-grained composites Y{sub 2.5}Nd{sub 0.5}Al{sub 5}O{sub 12} + x wt.% α-SiC (x = 1020) with ∼98–99% density. The microstructure of the composites has been studied, as well as the impact of α-SiC particles on the mechanical properties and kinetics of composite sintering. The introduction of the α-SiC part has been demonstrated to form a more fine-grained structure and under the given SPS conditions change the sintering mechanism in ceramics. The study has also demonstrated that introduction of α-SiC particles into garnet results in formation of internal stress fields, which, in turn, leads to a decrease in the activation energy of sintering of fine-grained composites at high temperatures.

36 MATERIALS SCIENCE↗

The physical chemistry and materials science behind sinter-resistant catalysts

Catalyst sintering, a main cause of the loss of catalytic activity and/or selectivity at high reaction temperatures, is a major concern and grand challenge in the general area of heterogeneous catalysis. Although all heterogeneous catalysts are inevitably subjected to sintering during their operation, the immediate and drastic consequences can be mitigated by carefully engineering the catalytic particles and their interactions with the supports. In this tutorial review, we highlight recent progress in understanding the physical chemistry and materials science involved in sintering, including the discussion of advanced techniques, such as in situ microscopy and spectroscopy, for investigating the sintering process and its rate. We also discuss strategies for the design and rational fabrication of sinter-resistant catalysts. To conclude, we showcase recent success in improving the thermal stability and thus sinter resistance of supported catalytic systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The Influence of Manganese Oxide on the Sintering Behavior of Yttria Tetragonal Zirconia

The sintering behavior of yttria-stabilized zirconia, with the influence of small additions of MnO{sub 2}(up to 1 wt %) sintered over the temperature range from 1250 deg. C to 1500 deg. C was investigated. It was found that the mechanical properties of Y-TZP were dependent on the dopant amount and sintering temperature. The results revealed that relative densities above 97.5% of theoretical (i.e. >5.95 Mgm{sup -3}) could be obtained in Y-TZPs sintered at low temperatures, 1250 deg. C and 1300 deg. C, with the additions of {<=}0.3 wt% MnO{sub 2}. In comparison to the undoped samples, the additions of up to 1 wt%MnO{sub 2} and for sintering up to 1350 deg. C was found to be beneficial in enhancing the Vickers hardness of the ceramic. The fracture toughness of Y-TZP however, was found to increase only in the 1 wt% MnO{sub 2}-doped samples when sintered above 1400 deg. C. The relation between the measured mechanical properties is discussed with the emphasis on the role of the manganese oxide.

36 MATERIALS SCIENCE↗

Sintering Effects on Morphology, Thermal Stability and Surface Area of Sol-Gel Derived Nano-Hydroxyapatite Powder

Hydroxyapatite (HAP) ceramics have been recognized as substitute materials for bone and teeth in orthopedic and dentistry field due to their chemical and biological similarity to human hard tissue. The nanosized and nanocrystalline forms of HAP have great potential to revolutionize the hard tissue-engineering field, starting from bone repair and augmentation to controlled drug delivery systems. This paper reports the synthesis of biomimetic nano-hydroxyapatite (HAP) by sol-gel method using calcium nitrate tetrahydrate (CNT) and potassium dihydrogen phosphate (KDP) as calcium and phosphorus precursors, respectively to obtain a desired Ca/P ratio of 1.67. Deionized water was used as a diluting media for HAP sol preparation and ammonia was used to adjust the pH to 11. After aging, the HAP gel was dried at 55 deg. C and sintered to different temperatures (200 deg. C, 400 deg. C, 600 deg. C, 800 deg. C, 1000 deg. C and 1200 deg. C). The dried and sintered powders were characterized for phase composition using Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). The particle size and morphology was studied using transmission electron microscopy (TEM). The thermal behavior of the dried HAP nanopowder was studied in the temperature range of 55 deg. C to 1000 deg. C using thermal gravimetric analyser (TGA). The BET surface area of absorbance was determined by Nitrogen adsorption using Brunauer-Emmett-Teller (BET) method. The presence of characteristic peaks of the phosphate and OH groups in FTIR spectrums confirmed the formation of pure HAP in dried as well as sintered powders. XRD results also confirmed the formation of stoichiometric nano-HAP. Sintering revealed that with increase in temperature, both the crystallinity and crystallite size of nano-HAP particles increased. The synthesized nano-HAP powder was found to be stable upto 1000 deg. C without any additional phase other than HAP, whereas peak of {beta}-TCP (tricalcium phosphate) was observed at 1200 deg. C. Photomicrograph of TEM showed that the nanopowder sintered at 600 deg. C is composed of hydroxyapatite nanoparticles (26.0-45.6 nm), which is well in agreement with the crystallite size calculated using XRD data. TGA study showed the thermal stability of the synthesized nano-HAP powder. The BET surface area decreased with increase in sintering temperature.

36 MATERIALS SCIENCE↗

Microwave sintering of Ag-nanoparticle thin films on a polyimide substrate

Ag-nanoparticle thin films on a polyimide substrate were subjected to microwave sintering by use of a single-mode waveguide applicator. A two-step sintering process was employed. First, at low conductivities of the film, the film sample was placed at the site of the maximum electric field and subjected to microwave irradiation. Second, when the conductivity of the film increased, the film sample was placed at the site of the maximum magnetic field and again subjected to microwave irradiation. The microwave sintering process was completed within 1.5 min, which is significantly lower than the time required for the oven heating process. The resulting conductivity of the film, albeit only 30% of that of the bulk material, was seven times that of a film annealed at the same temperature in a furnace. Scanning electron microscopy images revealed that the nanoparticles underwent both grain necking and grain growth during microwave sintering. In addition, this sintering process was equivalent to the oven heating process performed at a 50 °C higher annealing temperature. An electromagnetic wave simulation and a heat transfer simulation of the microwave sintering process were performed to gain a thorough understanding of the process.

36 MATERIALS SCIENCE↗

Effect of sintering temperature on structural and dielectric properties of Bi and Li co-substituted SrTiO{sub 3}

Sintering is an important factor that affects the microstructure development in ceramics. In this work, Bi and Li co-substituted Strontium Titanate (ST) ceramics samples sintered at different temperatures are prepared and analyzed by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). XRD was used to detect phase structure of the sintered samples and SEM was used for microstructure analysis. Dielectric properties of Bi and Li co-substituted SrTiO{sub 3} samples were measured using Agilent 4294A Impedance analyzer in the frequency range 40 Hz to 5 MHz at room temperature. The result reveals that the dielectric constant of Bi and Li co-substituted SrTiO{sub 3} ceramics increases with increasing sintering temperature up to 1250°C and then decreases beyond that. The highest value of dielectric constant obtained is 860 at 1KHz frequency and lowest dielectric loss observed is 0.04 at the same frequency for samples sintered at 1250°C. Also the grain size increases with increase of sintering temperature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Improvement of the electrochromic response of a low-temperature sintered dye-modified porous electrode using low-resistivity indium tin oxide nanoparticles

An indium tin oxide (ITO) nanoparticle-based porous electrode sintered at low temperatures was investigated as a transparent electrode for electrochromic displays (ECDs). The electrochromic (EC) response of the dye-modified ITO porous electrode sintered at 150 °C, which exhibited a generally low resistivity, was markedly superior to that of a conventional dye-modified TiO{sub 2} porous electrode sintered at the same temperature. Moreover, the EC characteristics of the dye-modified ITO porous electrode sintered at 150 °C were better than those of the high-temperature (450 °C) sintered conventional dye-modified TiO{sub 2} porous electrode. These improvements in the EC characteristics of the dye-modified ITO porous electrode are attributed to its lower resistivity than that of the TiO{sub 2} porous electrodes. In addition to its sufficiently low resistivity attained under the sintering conditions required for flexible ECD applications, the ITO porous film had superior visible-light transparency and dye adsorption capabilities. We conclude that the process temperature, resistivity, optical transmittance, and dye adsorption capability of the ITO porous electrode make it a promising transparent porous electrode for flexible ECD applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Reliability and Lifetime Prediction Model of Sintered Silver Under High-Temperature Cycling

Although excellent reliability has been reported for sintered silver as a die-attach material under both thermal and power cycling loads in power electronics applications, the promise of this material as a large-area attachment at temperatures beyond 200 degrees C needs to be investigated. This paper presents insights into the thermomechanical behavior and reliability of sintered silver under extreme thermal cycling conditions. In this study, we bonded sintered silver samples and subjected it to a thermal cycling profile of -40 °C to 200 °C with high ramp rates. We periodically monitored samples under thermal cycling to detect the presence of any failure mechanisms using a scanning acoustic microscope. We also included 95Pb5Sn solder in the study to obtain reference data. Results show the occurrence of cracks in sintered silver followed by a rapid rate of crack growth that exceeded the failure criterion in just 50 cycles. The predominant failure mechanism we observed was adhesive failure. As a large-area attachment, solder exhibited a higher reliability than sintered silver but failed within 100 cycles. Finally, we performed thermomechanical modeling to compute strain energy density values and correlated these with the experimentally observed crack growth rates to formulate a lifetime prediction model for sintered silver.

30 DIRECT ENERGY CONVERSION↗

Shrinkage, microstructure, and mechanical properties of sintered 3D-printed silica via stereolithography

Stereolithography has been used to create ceramic parts with complex geometry that is difficult to achieve with conventional fabrication techniques. Here this study used stereolithography to print silica honeycomb structures with a commercial Formlabs Form2 printer. The printed samples were sintered at different temperatures, and the print shape was retained up to 1300°C, but significant distortion from partial melting occurred at 1400°C. Higher sintering temperatures lead to more shrinkage, but it is non-uniform among directions, with the open cell plane shrinking more than the dense plane of the sample. As expected, the density of samples also increases with the sintering temperature. At higher sintering temperatures, there is an increase in cristobalite and a decrease in quartz, tridymite, and amorphous silica. Regarding mechanical properties, the out-of-plane compressive strength is approximately one order of magnitude higher than the in-plane compressive strength. When compressed along the out-of-plane direction, the samples sintered at lower temperatures surprisingly exhibit higher strength, which is explained by the micro-cracking mechanism. As expected, the samples sintered at higher temperatures display higher strength when compressed along the in-plane direction.

36 MATERIALS SCIENCE↗

Particle atomic layer deposition of alumina for sintering yttria-stabilized cubic zirconia

The addition of aluminum oxide (Al 2 O 3 ) as a sintering aid to yttria-stabilized zirconia (YSZ) reduces the required densification temperature. Sintering aids are incorporated using a number of processes which can lead to ambiguity when determining the effect of the sintering aid on the densification mechanism. In this study, a novel method for sintering aid addition, Particle Atomic Layer Deposition (ALD), was used to deposit an amorphous Al 2 O 3 thin film on YSZ particles. Transmission electron microscopy confirmed the deposition of conformal Al 2 O 3 thin films on the surface of the YSZ particles. The addition of Al 2 O 3 to YSZ reduced the temperature at which densification began by ~75 degrees C, and 2.2 wt% Al 2 O 3 addition resulted in a minimum activation energy for the intermediate stage of densification. This concentration is well in excess of the solubility limit of Al 2 O 3 in YSZ, showing that Al 2 O 3 does not enhance the densification of YSZ solely by dissolving into the YSZ lattice and activating volume diffusion. The addition of 0.7 wt% Al 2 O 3 with one Particle ALD cycle enhanced the ionic conductivity of YSZ by 23% after sintering at 1350 degrees C for 2 hours, demonstrating that dense parts with high oxygen ion conductivities can be produced after sintering at reduced temperatures. One Particle ALD cycle is a fast, easily scaled-up process that eliminates the use of solvents and has substantial cost/performance advantages over conventional processing.

36 MATERIALS SCIENCE↗

Flash Sintering of Oxide Ceramics under Microwave Heating

We report on the results of the analysis of the effect of flash sintering, which is observed upon heating compacted powder materials by high-intensity microwave radiation. Ceramic samples of Y{sub 2}O{sub 3}, MgAl{sub 2}O{sub 4}, and Yb: (LaO){sub 2}O{sub 3} were sintered to a density exceeding 98–99% of the theoretical value during 0.5–5 min without isothermal hold. The specific microwave power absorbed volumetrically in the samples was 20–400 W/cm{sup 3}. Based on the analysis of the experimental data (microwave radiation power and heating and cooling rates) and of the microstructure of the obtained materials, we propose a mechanism of flash sintering based on the evolution of the thermal instability and softening (melting) of the grain boundaries. The proposed mechanism also explains the flash sintering effect observed when a dc or a low-frequency ac voltage is applied to the samples. The microwave heating makes it possible to implement flash sintering without using electrodes for supplying energy to the articles being sintered.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Development of Macroscale Models of UO 2 Fuel Sintering and Densification using Multiscale Modeling and Simulation

Light water reactor fuel pellets are fabricated using sintering to final densities of 95% or greater. During reactor operation, the porosity remaining in the fuel after fabrication decreases further due to irradiation-assisted densification. While empirical models have been developed to describe this densification process, a mechanistic model is needed as part of the ongoing work by the NEAMS program to develop a more predictive fuel performance code. In this work we will develop a phase field model of sintering of UO 2 in the MARMOT code, and validate it by comparing to published sintering data. We will then add the capability to capture irradiation effects into the model, and use it to develop a mechanistic model of densification that will go into the BISON code and add another essential piece to the microstructure-based materials models. The final step will be to add the effects of applied fields, to model field-assisted sintering of UO 2 . The results of the phase field model will be validated by comparing to data from field-assisted sintering. Tasks over three years: 1. Develop a sintering model for UO 2 in MARMOT 2. Expand model to account for irradiation effects 3. Develop a mechanistic macroscale model of densification for BISON

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Electric-Loading Enhanced Kinetics in Oxide Ceramics: Pore Migration, Sintering and Grain Growth: Final Report

Solid oxide fuel cells and solid oxide electrolysis cells rely on solid electrolytes in which a large ionic current dominates. This project was initiated to investigate microstructural changes in such devices under electrochemical forces, because nominally insignificant processes may couple to the large ionic current to yield non-equilibrium phenomena that alter the microstructure. Our studies had focused on yttria-stabilized cubic zirconia (YSZ) widely used in these devices. The experiments have revealed enhanced grain growth at higher temperatures, pore and gas bubble migration at all temperatures, and the latter also lead to enhanced sintering of highly porous ceramics into fully dense ceramics at unprecedentedly low temperatures. These results have shed light on kinetic processes that fall completely outside the realm of classical ceramic processing. Other fast-oxygen oxide ceramics closely related to, and often used in conjunction with zirconia ceramics, have also be investigated, as are closely related scientific problems in zirconia ceramics. These include crystal structures, defects, diffusion kinetics, oxygen potentials, low temperature sintering, flash sintering, and coarsening theory, and all have resulted in greater clarity in scientific understanding. The knowledge is leveraged to provide new insight to electrode kinetics and near-electrode mixed conductivity and to new materials. In the following areas, our research has resulted in completely new knowledge that defines the state-of-the-art of the field. (a) Electrical current driven non-equilibrium phenomena, (b) Enhanced grain growth under electrochemically reducing conditions, (c) Development of oxygen potential polarization in electrically loaded electrolyte, (d) Low temperature sintering and grain growth, and (e) Structure, defects and cation kinetics of fluorite-structured oxides. Our research has also contributed to synthesis of new energy-relevant electrochemical materials and new understanding of flash sintering, which is a rapid sintering process initiated by a large electrical loading.

36 MATERIALS SCIENCE↗

On the Sintering Behavior of Nb2O5 and Ta2O5 Mixed Oxide Powders

A mixed oxide system consisting of Nb2O5 and Ta2O5, was subjected to annealing in air/hydrogen up to 950 °C for 1–4 h to study its sintering behavior. The thermogravimetric–differential scanning calorimetry (TGA–DSC) thermograms indicated the formation of multiple endothermic peaks at temperatures higher than 925 °C. Subsequently, a 30% Ta2O5 and 70% Nb2O5 (mol%) pellet resulted in good sintering behavior at both 900 and 950 °C. The scanning electron microscope (SEM) images corroborated these observations with necking and particle coarsening. The sintered pellets contained a 20.4 and 20.8% mixed oxide (Nb4Ta2O15) phase, along with Ta2O5 and Nb2O5, at both 900 and 950 °C, indicating the possibility of the formation of a solid solution phase. In situ high-temperature X-ray diffraction (XRD) scans also confirmed the formation of the ternary oxide phase at 6 and 19.8% at 890 and 950 °C, respectively. The Hume–Rothery rules could explain the good sintering behavior of the Ta2O5 and Nb2O5 mixed oxides. An oxide composition of 30% Ta2O5 and 70% Nb2O5 (mol%) and a sintering temperature of 950 °C appeared adequate for fabricating well-sintered oxide precursors for subsequent electrochemical polarization studies in fused salts.

36 MATERIALS SCIENCE↗