Pure SnO2 has proven very difficult to densify. This poor densification can be useful for the fabrication of SnO2 with a porous microstructure, which is used in electronic devices such as gas sensors. Most electronic devices based on SnO2 have a porous microstructure, with a porosity of > 40%. In pure SnO2, a high sintering temperature of approximately 1300°C is required to obtain > 40% porosity. In an attempt to reduce the required sintering temperature, the present study investigated the low-temperature sinterability of a current system. With the addition of TiO2, the compositions of the samples were Sn1-xTixO2-CoO(0.3wt%)-CuO(2wt%) in the range of x ≤ 0.04. Compared to the samples without added TiO2, densification was shown to be improved when the samples were sintered at 950°C. The dominant mass transport mechanism appears to be grain-boundary diffusion during heat treatment at 950°C.
The influence of MgO addition on the densification and microstructure of alumina (Al2O3) was studied. Compacted alumina specimens were manufactured using ball-milling and one-directional pressing followed by sintering at temperatures below 1700oC. Relative density, shrinkage, hardness, and microstructure were investigated using analytical tools such as FE-SEM, EDS, and XRD. When the MgO was added up to 5.0 wt% and sintered at 1500oC and 1600oC, the relative density exhibited an average value of 97% or more at both temperatures. The maximum density of 99.2% was with the addition of 0.5 wt% MgO at 1500oC. Meanwhile, the specimens showed significantly lower density values when sintered at 1400oC than at 1500oC and 1600oC owing to the relatively low sintering temperature. The hardness and shrinkage data also showed a similar trend in the change in density, implying that the addition of approximately 0.5 wt% MgO can promote the densification of Al2O3. Studying the microstructure confirmed the uniformity of the sintered alumina. These results can be used as basic compositional data for the development of MgOcontaining alumina as high-dielectric insulators.
In a nuclear power plant, the activated corrosion products are deposited on the reactor coolant system. The activated corrosion products must be removed to reduce the radiation exposure to workers before maintaining or decommissioning of the nuclear power plant. In order to remove the remove the activated duplex oxide layer generated on the reactor coolant system in the pressurized water reactor (PWR), the Cyclic SP (Sulfuric acid/Permanganate)-HyBRID (Hydrazine Based Reductive metal Ion Decontamination) process developed by KAERI (Korea Atomic Energy Research Institute) can be used. After applying the Cyclic SP-HyBRID process, a sulfate-rich waste powder containing the radionuclide is generated, and the radioactive powder has to be stabilized for final disposal. In the previous study, it was confirmed that the low-temperature sintering method can be applied to immobilize the sulfate-rich waste powder. Thus, immobilization of the Cyclic SP-HyBRID process waste powder was carried out by the low-temperature sintering method using a low melting point glass, and the physicochemical and radiological characteristics of a waste form were evaluated in this study. As a result, the compressive strength of the waste form increased with increasing sintering temperature and sintering time. It is considered that the result was caused by the difference in the band gap between the bismuth borate and zinc borate, which are the products during the sintering process. It was verified that the physical stability was maintained after the 107 Gy of irradiation test. In addition, it was confirmed that the radioactive metal hydroxides contained in the waste powder converted to metal oxide forms, which have the lower solubility, at the sintering temperature. Finally, the waste form was evaluated as a low-level radioactive waste from the concentration of radionuclides contained in the waste form.
Sulfate-rich waste powder containing a radioactive nuclide is generated from chemical decontamination process and radioactive liquid waste treatment using ion exchange resin. The radioactive sulfate-rich waste powder should be stabilized for final disposal. The techniques for immobilization of the radioactive sulfate-rich waste powder such as hydraulic cement, geopolymer, and iron phosphate glass have been applied, however, there are limitation in these techniques. Firstly, the hydraulic cement cannot applied to the wastes containing high concentration of sulfate because the expansion, cracks, and disintegration can be happened in the waste form. Geopolymer has a low density although they can be used as a good binder. The iron phosphate glass can be utilized, however, a considerable amount of SO2 gas is emitted due to the high sintering temperature. In this study, immobilization of radioactive sulfate-rich waste powder was carried out to resolve above problems by applying low temperature sintering method using a low-melting glass. As a result, it was confirmed that the waste form has a high bulk density. The compressive strength of the waste form was over 40 MPa, which is higher than the acceptance criteria (≥ 3.44 MPa). From ANS 16.1 test, it was verified that the waste form met the acceptance criteria of the leachability index (≥ 6). It was also confirmed that the waste form was chemically durable through product consistency test (PCT). In addition, the chemical stabilities of waste forms were compared following the sintering condition and the composition of the waste forms. The difference of the chemical stability was explained by difference in the abundance of chemical form obtained from the sequential extraction test.
This paper focuses on the electrical properties and stability against DC accelerated aging stress of ZnO-V2O5-MnO2- Nb2O5-Bi2O3-Co3O4-Dy2O3 (ZVMNBCD) varistor ceramics sintered at 850 - 925 ℃. With the increase of sintering temperature, the average grain size increases from 4.4 to 11.8 mm, and the density of the sintered pellets decreases from 5.53 to 5.40 g/ cm3 due to the volatility of V2O5, which has a low melting point. The breakdown field abruptly decreases from 8016 to 1,715 V/cm with the increase of the sintering temperature. The maximum non-ohmic coefficient (59) is obtained when the sample is sintered at 875 ℃. The samples sintered at below 900 oC exhibit a relatively low leakage current, less than 60 mA/cm2. The apparent dielectric constant increases due to the increase of the average grain size with the increase of the sintering temperature. The change tendency of dissipation factor at 1 kHz according to the sintering temperature coincides with the tendency of the leakage current. In terms of stability, the samples sintered at 900 ℃ exhibit both high non-ohmic coefficient (45) and excellent stability, 0.8% in ΔEB/EB and -0.7% in Δα/α after application of DC accelerated aging stress (0.85 EB/85 oC/24 h).
The various sintered samples comprising of 72 wt%(Al2O3) : 28 wt%(SiO2) based ceramics were fabricated using a colloidal processing route. The phase analysis of the ceramics was performed using an X-ray diffractometer (XRD) at room temperature confirming the presence of Al2O5Si and Al5.33Si0.67O9.33. The surface morphology of the fracture surface of the different sintered samples having different sizes of grain distribution. The resistive and capacitive properties of the three different sintered samples at frequency sweep (1 kHz to 1 MHz). The contribution of grain and the non-Debye relaxation process is seen for various sintered samples in the Nyquist plot. The ferroelectric loop of the various sintered sample shows a slim shape giving rise to low remnant polarization. The excitation performance of the sample at a constant electric signal has been examined utilizing a designed electrical circuit. The above result suggests that the prepared lead-free ceramic can act as a base for designing of dielectric capacitors or resonators.
The impact of different mixing methods and sintering temperatures on the microstructure and piezoelectric properties of PZNN-PZT ceramics is investigated. To improve the sinterability and piezoelectric properties of these ceramics, the composition of 0.13Pb((Zn0.8Ni0.2)1/3Nb2/3)O3-0.87Pb(Zr0.5Ti0.5)O3 (PZNN-PZT) containing a Pb-based relaxor component is selected. Two methods are used to create the powder for the PZNN-PZT ceramics. The first involves blending all source powders at once, followed by calcination. The second involves the preferential creation of columbite as a precursor, by reacting NiO with Nb2O5 powder. Subsequently, PZNN-PZT powder can be prepared by mixing the columbite powder, PbO, and other components, followed by an additional calcination step. All the PZNNPZT powder samples in this study show a nearly-pure perovskite phase. High-density PZNN-PZT ceramics can be fabricated using powders prepared by a two-step calcination process, with the addition of 0.3 wt% MnO2 at even relatively low sintering temperatures from 800℃ to 1000℃. The grain size of the ceramics at sintering temperatures above 900℃ is increased to approximately 3 μm. The optimized PZNN-PZT piezoelectric ceramics show a piezoelectric constant (d33) of 360 pC/N, an electromechanical coupling factor (kp) of 0.61, and a quality factor (Qm) of 275.
In this work, p-type Bi−Sb−Te alloys powders are prepared using gas atomization, a mass production powder preparation method involving rapid solidification. To study the effect of the sintering temperature on the microstructure and thermoelectric properties, gas-atomized powders are consolidated at different temperatures (623, 703, and 743 K) using spark plasma sintering. The crystal structures of the gas-atomized powders and sintered bulks are identified using an X-ray diffraction technique. Texture analysis by electron backscatter diffraction reveals that the grains are randomly oriented in the entire matrix, and no preferred orientation in any unique direction is observed. The hardness values decrease with increasing sintering temperature owing to a decrease in grain size. The conductivity increases gradually with increasing sintering temperature, whereas the Seebeck coefficient decreases owing to increases in the carrier mobility with grain size. The lowest thermal conductivity is obtained for the bulk sintered at a low temperature (603 K), mainly because of its fine-grained microstructure. A peak ZT of 1.06 is achieved for the sample sintered at 703 K owing to its moderate electrical conductivity and sustainable thermal conductivity.
We fabricate fine (<20 μm) powders of Bi0.5Sb1.5Te3 alloys using a large-scale production method and subsequently consolidate them at temperatures of 573, 623, and 673 K using a spark plasma sintering process. The microstructure, mechanical properties, and thermoelectric properties are investigated for each sintering temperature. The microstructural features of both the powders and bulks are characterized by scanning electron microscopy, and the crystal structures are analyzed by X-ray diffraction analysis. The grain size increases with increasing sintering temperature from 573 to 673 K. In addition, the mechanical properties increase significantly with decreasing sintering temperature owing to an increase in grain boundaries. The results indicate that the electrical conductivity and Seebeck coefficient (217 μV/K) of the sample sintered at 673 K increase simultaneously owing to decreased carrier concentration and increased mobility. As a result, a high ZT value of 0.92 at 300 K is achieved. According to the results, a sintering temperature of 673 K is preferable for consolidation of fine (<20 μm) powders.
In this study, we report the microstructure and the high-temperature oxidation behavior of Fe-Ni alloys by spark plasma sintering. Structural characterization is performed by scanning electron microscopy and X-ray diffraction. The oxidation behavior of Fe-Ni alloys is studied by means of a high-temperature oxidation test at 1000oC in air. The effect of Ni content of Fe-Ni alloys on the microstructure and on the oxidation characteristics is investigated in detail. In the case of Fe-2Ni and Fe-5Ni alloys, the microstructure is a ferrite (α) phase with body centered cubic (BCC) structure, and the microstructure of Fe-10Ni and Fe-20Ni alloys is considered to be a massive martensite (α’) phase with the same BCC structure as that of the ferrite phase. As the Ni content increases, the micro-Vickers hardness of the alloys also increases. It can also be seen that the oxidation resistance is improved by decreasing the thickness of the oxide film.
This study investigates the influence of sintering temperature on the magnetic properties and frequency dispersion of the complex permeability of Ni–Zn–Cu ferrites used for magnetic shielding in near-field communication (NFC) systems. Sintered specimens of (Ni0.7Zn0.3)0.96Cu0.04Fe2O4 are prepared by conventional ceramic processing. The complex permeability is measured by an RF impedance analyzer in the range of 1 MHz to 1.8 GHz. The real and imaginary parts of the complex permeability depend sensitively on the sintering temperature, which is closely related to the microstructure, including grain size and pore distribution. In particular, internal pores within grains produced by rapid grain growth decrease the permeability and increase the magnetic loss at the operating frequency of NFC (13.56 MHz). At the optimized sintering temperature (1225-1250°C), the highest permeability and lowest magnetic loss can be obtained.
In this study, ternary compound Max Phase Ti2AlC material was mixed by 3D ball milling as a function of ball milling time. More than 99.5 wt% pure Ti2AlC was synthesized by using spark plasma sintering method at 1000, 1100, 1200, and 1300oC for 60 min. The material characteristics of synthesized samples were examined with relative density, hardness, and electrical conductivity as a function of sintering temperature. The phase composition of bulk was identified by X-ray diffraction. On the basis of FE-SEM result, a terraced structures which consists of several laminated layers were observed. And Ti2AlC bulk material obtained a vickers hardness of 5.1 GPa at the sintering temperature of 1100oC.
The porous metals are known as relatively excellent characteristic such as large surface area, light, lower heat capacity, high toughness and permeability. The Fe-Cr-Al alloys have high corrosion resistance, heat resistance and chemical stability for high temperature applications. And then many researches are developed the Fe-Cr-Al porous metals for exhaust gas filter, hydrogen reformer catalyst support and chemical filter. In this study, the Fe-Cr-Al porous metals are developed with Fe-22Cr-6Al(wt) powder using powder compaction method. The mean size of Fe-22Cr-6Al(wt) powders is about 42.69 μm. In order to control pore size and porosity, Fe-Cr-Al powders are sintered at 1200~1450oC and different sintering maintenance as 1~4 hours. The powders are pressed on disk shapes of 3 mm thickness using uniaxial press machine and sintered in high vacuum condition. The pore properties are evaluated using capillary flow porometer. As sintering temperature increased, relative density is increased from 73% to 96% and porosity, pore size are decreased from 27 to 3.3%, from 3.1 to 1.8 μm respectively. When the sintering time is increased, the relative density is also increased from 76.5% to 84.7% and porosity, pore size are decreased from 23.5% to 15.3%, from 2.7 to 2.08 μm respectively.
The effect of sintering temperature on the microstructure, electrical and dielectric properties of (V, Mn, Co, Dy, Bi)- codoped zinc oxide ceramics was investigated in this study. An increase in the sintering temperature increased the average grain size from 4.7 to 10.4 μm and decreased the sintered density from 5.47 to 5.37 g/cm3. As the sintering temperature increased, the breakdown field decreased greatly from 6027 to 1659 V/cm. The ceramics sintered at 900 oC were characterized by the highest nonlinear coefficient (36.2) and the lowest low leakage current density (36.4 μA/cm2). When the sintering temperature increased, the donor concentration of the semiconducting grain increased from 2.49 × 1017 to 6.16 × 1017/cm3, and the density of interface state increased from 1.34 × 1012 to 1.99 × 1012/cm2. The dielectric constant increased greatly from 412.3 to 1234.8 with increasing sintering temperature.
A high temperature dilatometer attached to a graphite furnace is built and used to study the sintering behaviorof B4C. Pristine and carbon doped B4C compacts are sintered at various soaking temperatures and their shrinkage pro-files are detected simultaneously using the dilatometer. Carbon additions enhance the sinterability of B4C with sinteringto more than 97% of the theoretical density, while pristine B4C compacts could not be sintered above 91% due to par-ticle coarsening. The shrinkage profiles of B4C reveal that the effect of carbon on the sinterability of B4C can be seenmostly below 1950°C. The high temperature dilatometer delivers very useful information which is impossible to obtainwith conventional furnaces.
Microstructural and mechanical properties of Ni-YSZ fabricated using SPS processing have been investigated at various sintering temperatures. Our study shows samples to be applied as a SOFC anode have the proper porosity of 40% and high hardness when processed at 1100ºC. These results are comparable to the values obtained at 100- 200ºC higher sintering temperature reported by others. This result is important because when the fabrication processes are performed above 1100ºC, the mechanical property starts to decrease drastically. This is caused by the fast grain coarsening at the higher temperature, which initiates a mismatch between thermal expansion coefficients of Ni and YSZ and induces cracks as well.
The quartz glasses were prepared by fumed silica powders sintering method at , , in air and the effect of sintering temperature on their properties were investigated. The X-ray diffraction pattern, the OH concentration, the light transmittance, the apparent porosity and the density were analyzed. The transparent quartz glass were obtained above . The OH-group and macroscopic pores were removed above and highest density and light transmittance were obtained at .