Search results for: liquid phase sintering

Authors: Ming-Wei Wu, Zih-Jie Lin

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Liquid phase sintering (LPS) is a feasible means for decreasing the porosity of powder metallurgy (PM) Fe-based material without substantially increase the production cost. The aim of this study was to investigate the effect of 0.6 wt% boron on the densification of PM 304L stainless steel by LPS. The results indicated that the increase in the sintered density of 304L+0.6B steel is obvious after 1250 ºC sintering, and eutectic structures with borides are observed at the interfaces of the raw steel powders. Differential scanning calorimetry (DSC) results show that liquid is generated at 1244ºC during sintering. The boride in the eutectic structure is rich in boron and chromium atoms and is deficient in nickel atoms, as identified by electron probe micro-analyzer (EPMA). Furthermore, the sintered densities of 304L and 304L+0.6B steels sintered at 1300 ºC are 6.99 g/cm3 and 7.69 g/cm3, respectively, indicating that boron is a suitable alloying element for facilitating LPS of PM 304L stainless steel.

Keywords: powder metallurgy, liquid phase sintering, stainless steel, boron, microstructure

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Authors: Ming-Wei Wu, Yu-Jin Tsai, Ching-Huai Chang

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Liquid phase sintering (LPS) is a versatile technique for achieving effective densification of powder metallurgy (PM) steels and other materials. The aim of this study was to examine the influences of 0.6 wt% boron on the microstructure and LPS behavior of boron-alloyed 410 martensitic stainless steel. The results showed that adding 0.6 wt% boron can obviously promote the LPS due to a eutectic reaction and increase the sintered density of 410 stainless steel. The density was much increased by 1.06 g/cm³ after 1225ºC sintering. Increasing the sintering temperature from 1225ºC to 1275ºC did not obviously improve the sintered density. After sintering at 1225ºC~1275ºC, the matrix was fully martensitic, and intragranular borides were extensively found due to the solidification of eutectic liquid. The microstructure after LPS consisted of the martensitic matrix and (Fe, Cr)2B boride, as identified by electron backscatter diffraction (EBSD) and electron probe micro-analysis (EPMA).

Keywords: powder metallurgy, liquid phase sintering, stainless steel, martensite, boron, microstructure

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Authors: Hamed Yaghoubi, Esmaeil Salahi, Fateme Taati

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The effective shear and bulk viscosity, as well as dynamic viscosity, describe the rheological properties of the ceramic body during the liquid phase sintering process. The rheological parameters depend on the physical and thermomechanical characteristics of the material such as relative density, temperature, grain size, and diffusion coefficient and activation energy. The main goal of this research is to acquire a comprehensive understanding of the response of an incompressible viscose ceramic material during liquid phase sintering process such as stress-strain relations, sintering and hydrostatic stress, the prediction of anisotropic shrinkage and heterogeneous densification as a function of sintering time by including the simultaneous influence of gravity field, and frictional force. After raw materials analysis, the standard hard porcelain mixture as a ceramic body was designed and prepared. Three different experimental configurations were designed including midpoint deflection, sinter bending, and free sintering samples. The numerical method for the ceramic specimens during the liquid phase sintering process are implemented in the CREEP user subroutine code in ABAQUS. The numerical-experimental procedure shows the anisotropic behavior, the complete difference in spatial displacement through three directions, the incompressibility for ceramic samples during the sintering process. The anisotropic shrinkage factor has been proposed to investigate the shrinkage anisotropy. It has been shown that the shrinkage along the normal axis of casting sample is about 1.5 times larger than that of casting direction, the gravitational force in pyroplastic deformation intensifies the shrinkage anisotropy more than the free sintering sample. The lowest and greatest equivalent creep strain occurs at the intermediate zone and around the central line of the midpoint distorted sample, respectively. In the sinter bending test sample, the equivalent creep strain approaches to the maximum near the contact area with refractory support. The inhomogeneity in Von-Misses, pressure, and principal stress intensifies the relative density non-uniformity in all samples, except in free sintering one. The symmetrical distribution of stress around the center of free sintering sample, cause to hinder the pyroplastic deformations. Densification results confirmed that the effective bulk viscosity was well-defined with relative density values. The stress analysis confirmed that the sintering stress is more than the hydrostatic stress from start to end of sintering time so, from both theoretically and experimentally point of view, the sintering process occurs completely.

Keywords: anisotropic shrinkage, ceramic material, liquid phase sintering process, rheological properties, numerical-experimental procedure

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Authors: Tadeusz Pieczonka, Jan Kazior

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The influence of SiC powder addition on densification of Al-SiC compacts during sintering in different atmospheres was investigated. It was performed in a dilatometer in flowing nitrogen, nitrogen/hydrogen (95/5 by volume) and argon. Fine, F500 grade of SiC powder was used. Mixtures containing 10 and 30 vol.% of SiC reinforcement were prepared in a Turbula mixer. Green compacts of about 82% of theoretical density were made of each mixture. For comparison, compacts made of pure aluminum powder were also investigated. It was shown that nitrogen is the best sintering atmosphere because only in this atmosphere did shrinkage take place. Its amount is lowered by ceramic powder addition, i.e. the more SiC the less densification occurs. Additionally, the formation of clusters enhanced in compacts containing 30 vol.% SiC, is also responsible for limiting the shrinkage. Microstructural examinations of sintered composites revealed that sintering of compacts occurs in the presence of the liquid phase exclusively in nitrogen.

Keywords: Al-SiC composites, densification, sintering atmosphere, materials engineering

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Authors: Bilge Yaman Islak, Erhan Ayas

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The densification behavior of TiB₂ – Ti₃SiC₂ composites is investigated for temperatures in the range of 1200°C to 1400°C, for the pressure of 40 and 50MPa, and for holding time between 15-30 min by spark plasma sintering (SPS) technique. Ti, Si, TiC and 5 wt.% TiB₂ were used to synthesize TiB₂ – Ti₃SiC₂ composites and the effect of different sintering parameters on the densification and phase evolution of these composites were investigated. The bulk densities were determined by using the Archimedes method. The polished and fractured surfaces of the samples were examined using a scanning electron microscope equipped with an energy dispersive spectroscopy (EDS). The phase analyses were accomplished by using the X-Ray diffractometer. Sintering temperature and holding time are found to play a dominant role in the phase development of composites. TiₓCᵧ and TiSi₂ secondary phases were found in 5 wt.%TiB₂ – Ti₃SiC₂ composites densified at 1200°C and 1400°C under the pressure of 40 MPa, due to decomposition of Ti₃SiC₂. The results indicated that 5 wt.%TiB₂ – Ti₃SiC₂ composites were densified into the dense parts with a relative density of 98.77% by sintering at 1300 °C, for 15 min, under a pressure of 50 MPa via SPS without the formation of any other ancillary phase. This work was funded and supported by Scientific Research Projects Commission of Eskisehir Osmangazi University with the Project Number 201915C103 (2019-2517).

Keywords: densification, phase evolution, sintering, TiB₂ – Ti₃SiC₂ composites

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Authors: Yumei Wang, Xiaoyu Xu, Li Lu

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Solid-state battery adopts solid-state electrolyte such as oxide- and composite-based solid electrolytes. With the adaption of nonflammable or less flammable solid electrolytes, the safety of solid-state batteries can be largely increased. NASICON (Na₃Zr₂Si₂PO₁₂, NZSP) is one of the sodium ion conductors that possess relatively high ionic conductivity, wide electrochemical stable range and good chemical stability. Therefore, it has received increased attention. We report the development of high-density NZSP through liquid phase sintering and its organic-inorganic composite electrolyte. Through reactive liquid phase sintering, the grain boundary conductivity can be largely enhanced while using an organic-inorganic composite electrolyte, interfacial wetting and impedance can be largely reduced hence being possible to fabricate scalable solid-state batteries.

Keywords: solid-state electrolyte, composite electrolyte, electrochemical performance, conductivity

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Authors: F. Z. Abir, M. Mesnaoui, Y. Abouliatim, L. Nibou, Y. El Hafiane, A. Smith

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The cement industry has been taking significant steps for years to reduce its carbon footprint by opting for an eco-friendly alternative such as Calcium Sulfoaluminate Cements (CSA). These binders, compared to Ordinary Portland Cements (OPC), have two advantages: reduction of the CO2 emissions and energy-saving because the sintering temperature of CSA cements is between 1250 and 1350 °C, which means 100 to 200 °C less than OPC. The aim of this work is to study the impurities effect, such as iron oxide, on the formation of the ye'elimite phase, which represents the main phase of Calcium Sulfoaluminate Cements and the consequence on its hydration. Several elaborations and characterization techniques were used to study the structure and microstructure of ye'elimite, such as X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), thermal analysis, specific surface area measurement, and electrical conductivity of diluted solutions. This study details the protocol for the solid-state synthesis of ye'elimite containing increasing amounts of iron (general formula: Ca4Al(6-2x)Fe2xSO16 with x = 0.00 to 1.13). Ye'elimite is formed by solid-state reactions between Al2O3, CaO and CaSO4 and the maximum ye'elimite content is reached at a sintering temperature of 1300 °C. The presence of iron promotes the formation of cubic ye'elimite at the expense of the orthorhombic phase. The total incorporation of iron in ye'elimite structure is possible when x < 0.12. Beyond this content, the ferritic phase (CaO)2(Al2O3,Fe2O3) appears as a minor phase and develops two different morphologies during cooling: dendritic crystals and melt morphology. The formation of the ferrous liquid phase affects the evolution of grain size of the ye’elimite and calcium aluminates.

Keywords: calcium sulfoaluminate cement, ferritic phase, sintering, solid-state synthesis, ye’elimite

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Authors: El Mehdi Haily, Lahcen Bih, Mohammed Azrour, Bouchaib Manoun

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The effects of xBi₂O₃-yBaO-zP₂O₅ (BBP) glass addition on the sintering, structural, and dielectric properties of BaTiO₃ ceramic (BT) are studied. The BT ceramic was synthesized by the conventional solid-state reaction method while the glasses BaO-Bi₂O₃-P₂O₅ (BBP) were elaborated by melting and quenching process. Different composites BT-xBBP were formed by mixing the BBP glasses with BT ceramic. For each glass composition, where the ratio (x:y:z) is maintained constant, we have developed three composites with different glass weight percentage (x = 2.5, 5, and 7.5 wt %). Addition of the glass helps in better sintering at lower temperatures with the presence of liquid phase at the respective sintering temperatures. The results showed that the sintering temperature decreased from more than 1300°C to 900°C. Density measurements of the composites are performed using the standard Archimedean method with water as medium liquid. It is found that their density and molar volume decrease and increase with glass content, respectively. Raman spectroscopy is used to characterize their structural approach. This technique has allowed the identification of different structural units of phosphate and the characteristic vibration modes of the BT. The electrical properties of the composite samples are carried out by impedance spectroscopy in the frequency range of 10 Hz to 1 MHz under various temperatures from 300 to 473 K. The obtained results show that their dielectric properties depend both on the content of the glass in the composite and the Bi/P ratio in the glasses.

Keywords: phosphate, glasses, composite, Raman spectroscopy, dielectric properties

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Authors: Iftikhar Ahmad, Abulhakim Almajid

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Alumina (Al2O3) is an attractive structural ceramic however; brittleness turns Al2O3 down for advanced applications. Development of multi-phase phase ceramics systems is promising to curtail the brittleness and the incorporation of strong/elastic graphene, as third phase, into dual phase (Al2O3-SiC) is striking for mechanical upgrading purpose. Thin graphene nanosheets (GNS) were prepared by thermal exfoliation process and reinforced into dual phase ceramic system. The hybrid nanocomposite was consolidated by novel HF-IH (high-frequency induction heating) sintering furnace at 1500 °C under 50 MPa in vacuum conditions. Structural features and grain size of the resulting nanocomposite were analyzed by SEM and TEM whilst the mechanical properties were assessed by microhardness and nanoindentation techniques. The fracture toughness of the hybrid nanocomposites was appraised by direct crack measurement method. Electron microscopic investigations confirmed the preparation of thin (< 10 nm) graphene nanosheets (GNS). HF-IH sintering route condensed the three-phase (GNS-Al2O3-SiC) hybrid nanocomposite system to > 99% relative densities. SEM of the hybrid nanocomposites fractured surfaces revealed even distribution of the nanocomposite constituents and changed in fracture-mode. Structurally, 88% grain reduction into hybrid nanocomposite was also obtained. Mechanically, enhanced fracture toughness (50%) and hardness (53%) were also achieved for hybrid nanocomposites were attained against bench marked monolithic Al2O3.

Keywords: alumina, graphene, hybrid nanocomposites, rapid sintering

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Authors: A. Yönetken, A. Erol, A. Yakar, G. Peşmen

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The microstructure, mechanical properties and metalgraphic characteristics of Ni plated AlN-Astaloy Cr-M powders were investigated using specimens produced by tube furnace sintering at 1000-1400 °C temperature. A uniform nickel layer on AlN powders was deposited prior to sintering using electroless plating technique. A composite consisting of ternary additions, metallic phase, Ni and ceramic phase AlN within a matrix of Astaloy Cr-M had been prepared under Ar shroud and then tube furnace sintered. The experimental results carried out by using XRD (X-Ray Diffraction) and SEM (Scanning Electron Microscope) for composition (10% AlN-Astaloy Cr-M) 10% Ni at 1400 °C suggest that the best properties as 132.45HB and permittivity were obtained at 1400 °C.

Keywords: composite, electroless nickel plating, powder metallurgy, sintering

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Authors: Rudolf L. Kanyane, Nicolaus Malatji, Patritia A. Popoola

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Tribological failure of materials during application can lead to catastrophic events which also carry economic penalties. High entropy alloys (HEAs) have shown outstanding tribological properties in applications such as mechanical parts were moving parts under high friction are required. This work aims to investigate the effect of sintering temperature on microhardness properties and tribological properties of novel equiatomic TiAlMoSiW HEAs fabricated via spark plasma sintering. The effect of Spark plasma sintering temperature on morphological evolution and phase formation was also investigated. The microstructure and the phases formed for the developed HEAs were examined using scanning electron microscopy (SEM) and X-ray diffractometry (XRD) respectively. The microhardness and tribological properties were studied using a diamond base microhardness tester Rtec tribometer. The developed HEAs showed improved mechanical properties as the sintering temperature increases.

Keywords: sintering, high entropy alloy, microhardness, tribology

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Authors: Indra Bahadur Bhandari, Narayan Panthi, Ishwar Koirala, Devendra Adhikari

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We have used a theoretical model based on the assumption of compound formation in binary alloys to study the thermodynamic, microscopic, and surface properties of Bi-Pb and In-Pb liquid alloys. A review of the phase diagrams for these alloys shows that one of the stable complexes for Bi-Pb liquid alloy is BiPb3; also, that InPb is a stable phase in liquid In-Pb alloys. Using the same interaction parameters that are fitted for the free energy of mixing, we have been able to compute the bulk and thermodynamic properties of the alloys. From our observations, we are able to show that the Bi-Pb liquid alloy exhibits compound formation over the whole concentration range and the In-Pb alloys undergo phase separation. With regards to surface properties, Pb segregates more to the surface in In-Pb alloys than in Bi-Pb alloys. The viscosity isotherms have a positive deviation from ideality for both Bi-Pb and In-Pb alloys.

Keywords: asymmetry, Bi-Pb, deviation, In-Pb, interaction parameters

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Authors: A. S. Hakeem, B. Ahmed, M. Ehsan, A. Ibrahim, H. M. Irshad, T. Laoui

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Alumina (Al2O3) - cubic boron nitride (cBN) ceramic composites were sintered by spark plasma sintering (SPS) using α-Al2O3 particle sizes; 150 µm, 150 nm and cBN particle size of 42 µm. Alumina-cBN composites containing 10, 20 and 30wt% cBN with and without Ni coated were sintering at an elevated temperature of 1400°C at a constant uniaxial pressure of 50 MPa. The effect of matrix particle size, cBN and Ni content on mechanical properties and thermal properties, i.e., thermal conductivity, diffusivity, expansion, densification, phase transformation, microstructure, hardness and toughness of the Al2O3-cBN/(Ni) composites under specific sintering conditions were investigated. The highest relative densification of 150 nm-Al2O3 containing 30wt% cBN (Ni coated) composite was 99% at TSPS = 1400°C. In case of 150 µm- Al2O3 compositions, the phase transformation of cBN to hBN were observed, and the relative densification decreased. Thermal conductivity depicts maximum value in case of 150 nm- Al2O3-30wt% cBN-Ni composition. The Vickers hardness of this composition at TSPS = 1400°C also showed the highest value of 29 GPa.

Keywords: alumina composite, cubic boron nitride, mechanical properties, phase transformation, Spark plasma sintering

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Authors: Shoji Mori, Kunito Okuyama

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Annular two phase flow is encountered in many industrial equipments, including flow near nuclear fuel rods in boiling water reactor (BWR). Especially, disturbance waves play important roles in the pressure drop, the generation of entrainments, and the dryout of the liquid film. Therefore, it is important to clarify the behavior of disturbance waves and base film. However, most of the previous studies have been performed under atmospheric pressure conditions that provides the properties of liquid and gas which are significantly different from those of a BWR. Therefore, the effect of properties in gas and liquid on liquid film characteristics should be clarified. In this paper we focus on the effect of gas-liquid density ratio on liquid film thickness characteristics. The experiments have been conducted at four density ratio conditions (ρL/ρG =763, 451, 231, and 31). As a result, it is found that and interfacial shear stress collapse not only tF ave but also tF max and tF min successfully under the same liquid mass flow rate conditions irrespective of ρL/ρG, and moreover a non-dimensional parameter tends to collapse tF max，tF ave，and tF min in the wide range of experimental conditions (ρL/ρG：31～763，We：10～1800，ReL:500 ～ 2200).

Keywords: two phase flow, liquid film, annular flow, disturbance wave

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Authors: Roopam Gaur, K. Chandramani Singh, Radhapiyari Laishram

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In order to produce lead free piezoceramics with optimum piezoelectric and dielectric properties, KNN modified with Li+ (as an A site dopant) and Sb5+ (as a B site dopant) (K0.49Na0.49Li0.02) (Nb0.96Sb0.04) O3 (referred as KNLNS in this paper) have been synthesized using solid state reaction method and conventional sintering technique. The ceramics were sintered in the narrow range of 10500C-10900C for 2-3 hours to get precise information about sintering parameters. Detailed study of dependence of microstructural, dielectric and piezoelectric properties on sintering conditions was then carried out. The study suggests that the volatility of the highly hygroscopic KNN ceramics is not only sensitive to sintering temperatures but also to sintering durations. By merely reducing the sintering duration for a given sintering temperature we saw an increase in the density of the samples which was supported by the increase in dielectric constants of the ceramics. And since density directly or indirectly affects almost all the associated properties, other dielectric and piezoelectric properties were also enhanced as we approached towards the most suitable sintering temperature and duration combination.

Keywords: piezoelectric, dielectric, Li, Sb, KNN, conventional sintering

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Authors: Amanda Cristina de Oliveira, Elias de Souza Monteiro Filho, Roberta Ceriani

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Liquid-liquid extraction in aqueous two-phase systems (ATPSs) constitutes a powerful tool for purifying bio-materials, such as cells, organelles, proteins, among others. In this work, the extraction of the bovine serum albumin (BSA) has been studied in systems formed by polyethylene glycol (PEG) (1500, 4000, and 6000 g.mol⁻¹) + potassium sodium tartrate + water at 303.15°K. Phase diagrams were obtained by turbidimetry and Merchuk’s method (1998). The experimental tie-lines were described using the Othmer-Tobias and Bancroft correlations. ATPSs were correlated with the nonrandom two-liquid (NRTL) model. The results were considered excellent according to global root-mean-square deviations found which were between 0,72 and 1,13%. The concentrations of the proteins in each phase were determined by spectrophotometry at 280 nm, finding partition efficiencies greater than 71%.

Keywords: aqueous two phases systems, bovine serum albumin , liquid-liquid extraction, polyethylene glycol

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Authors: K. Hiro, T. Wada

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Thermodynamic properties of liquids under negative pressures are interesting and important in fields of scienceand technology. Here, phase transitions of a thermotropic liquid crystal are investigatedin a range from positive to negative pressures with a metal Berthelot tube using a commercial pressure transducer.Two co-existinglines, namely crystal (Kr) – nematic (N), and isotropic liquid (I) - nematic (N) lines, weredrawn in a pressure - temperature plane. The I-N line was drawn to ca. -5 (MPa).

Keywords: Berthelot method, liquid crystal, negative pressure, phase transitions

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Authors: Ruitao Li, Zhili Dong, Nay Win Khun, Khiam Aik Khor

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In this study, microstructure and sintering mechanism as well as wear resistance properties of Ti/Al-Cr-Fe metal matrix composites (MMCs) fabricated by spark plasma sintering (SPS) with Ti as matrix and Al-Cr-Fe as reinforcement were investigated. Phases and microstructure of the sintered samples were analyzed using X-ray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and transmission electron microscopy (TEM). Wear resistance properties were tested by ball-on-disk method. An Al3Ti ring forms around each Al-Cr-Fe particle as the bonding layer between Ti and Al-Cr-Fe particles. The Al content in Al-Cr-Fe particles experiences a decrease from 70 at.% to 60 at.% in the sintering process. And these particles consist of quasicrystalline icosahedral AlCrFe and quasicrystal approximants γ-brass Al8(Cr,Fe)5 and Al9(Cr,Fe)4 in the sintered compact. The addition of Al-Cr-Fe particles into the Ti matrix can improve the microhardness by about 40% and the wear resistance is improved by more than 50% due to the increase in the microhardness and the change of wear mechanism.

Keywords: metal matrix composites, spark plasma sintering, phase transformation, wear

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Authors: Ahmet Yonetken, Ayhan Erol

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The microstructure, mechanical properties and corrosion characteristics of Ni plated %10Al2O3-%40Co-%20Cr and %10Ti powders were investigated using specimens produced by tube furnace sintering at 800-1200°C temperature. A uniform nickel layer on Al2O3-Co-Cr and Ti powders was deposited prior to sintering using electroless plating technique. A composite consisting of quintet additions, a metallic phase, Ti,Cr and Co including a ceramic phase, alumina, within a matrix of Ni has been prepared under Ar shroud and then tube furnace sintered. XRD, SEM (Scanning Electron Microscope), corrosion behavior in acidic media were investigated to characterize the properties of the specimens. Experimental results carried out for composition (%10Al2O3-%40Co-%20Cr- %10Ti)20Ni at 1200°C suggest that the best properties as 312.18HV were obtained at 1200°C.

Keywords: sintering, intermetallic, Electroless nickel plating, composite

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Authors: C. Milind Caspar, Valtonia Octavio Massingue, K. Maneesh Reddy, K. V. Ramesh

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Gas holdup data were obtained from measured pressure drop values in a gas-liquid upflow bubble column in the presence of string of hemispheres promoter internal. The parameters that influenced the gas holdup are gas velocity, liquid velocity, promoter rod diameter, pitch and base diameter of hemisphere. Tap water was used as liquid phase and nitrogen as gas phase. About 26 percent in gas holdup was obtained due to the insertion of promoter in in the present study in comparison with empty conduit. Pitch and rod diameter have not shown any influence on gas holdup whereas gas holdup was strongly influenced by gas velocity, liquid velocity and hemisphere base diameter. Correlation equation was obtained for the prediction of gas holdup by least squares regression analysis.

Keywords: bubble column, gas-holdup, two-phase flow, turbulent promoter

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Authors: J. H. Kim, S. Y. Park, K. M. Lim, S. K. Hyun

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The effect of sintering temperature on the magnetic and mechanical properties of Nd-Fe-B sintered magnets has been investigated in this study. The sintering temperature changed from 950°C to 1120°C. While remanence and hardness of the magnets increased with increasing sintering temperature, the coercivity first increased, and then decreased. The optimum magnetic and mechanical properties of the magnets were obtained at the sintering temperature of 1050°C. In order to clarify the reason for the variation on magnetic and mechanical properties of the magnets, we systematically analyzed the microstructure.

Keywords: magnetic and mechanical property, microstructure, permanent magnets, sintered Nd-Fe-B magnet

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Authors: Xiaopeng Shang, Xin YU, Jun CHANG

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Calcium barium sulphoaluminate (CBSA), derived from calcium sulphoaluminate(CSA), has excellent cementitious properties. In this study, the sintering system of CBSA with a theoretical stoichiometric Ca3BaAl6SO16 was investigated. Rietveld refinement was performed using TOPAS 4.2 software to quantitatively calculate the content of CBSA and the actual ionic site occupancy of Ba2+. The results indicate that the contents of Ca4-xBaxAl6SO16 increases with increasing sintering temperature in the 1200℃-1400℃ ranges. When sintered at 1400℃ for 180min, the content of CBSA reaches 88.4%. However, CBSA begins to decompose at 1440℃ and the content of which decreases. The replacement rate of Ba2+ was also enlarged by increasing sintering temperature and prolonged sintering time. Sintering at 1400℃ for 180min is considered as the optimum when replacement rate of Ba2+ and the content of CBSA were taken into account. Ca3.2Ba0.8Al6SO16 with a content of 88.4% was synthesized.

Keywords: calcium barium sulphoaluminate, sintering system, Ba2+ replacement rate, Rietveld refinement

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Authors: T. H. N. Nguyen, A. Khodan, M. Amamra, J-V. Vignes, A. Kanaev

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The ultraporous nanofibrous alumina (NOA, Al2O3·nH2O) was synthesized by oxidation of laminated aluminium plates through a liquid mercury-silver layer in a humid atmosphere ~80% at 25°C. The material has an extremely high purity (99%), porosity (90%) and specific area (300 m2/g). The subsequent annealing of raw NOA permits obtaining pure transition phase (γ and θ) nanostructured materials. In this combination, we report on chemical, structural and phase transformations of pure and modified NOA by an impregnation of trimethylethoxysilane (TMES) and tetraethoxysilane (TEOS) during thermal annealing in the temperature range between 20 and 1650°C. The mass density, specific area, average diameter and specific area are analysed. The 3D model of pure NOA monoliths and silica modified NOA is proposed, which successfully describes the evolution of specific area, mass density and phase transformations. Activation energies of the mass transport in two regimes of surface diffusion and bulk sintering were obtained based on this model. We conclude about a common origin of modifications of the NOA morphology, chemical composition and phase transition.

Keywords: nanostructured materials, alumina (Al₂O₃), morphology, phase transitions

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Authors: Hyun-Jong Choi, Minjun Kwak, Doo-Won Seo, Sang-Kuk Woo, Sun-Dong Kim

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Solid Oxide Cell(SOC) systems can contribute to the transition to the hydrogen society by utilized as a power and hydrogen generator by the electrochemical reaction with high efficiency at high operation temperature (>750 ℃). La1-xSrxCo1-yFeyO3, which is an air electrode, is occurred stability degradations due to reaction and delamination with yittria stabilized zirconia(YSZ) electrolyte in a water electrolysis mode. To complement this phenomenon SOCs need gadolinium doped ceria(GDC) buffer layer between electrolyte and air electrode. However, GDC buffer layer requires a high sintering temperature and it causes a reaction with YSZ electrolyte. This study carried out low temperature sintering of GDC layer by applying Cu-oxide as a sintering aid. The effect of a copper additive as a sintering aid to lower the sintering temperature for the construction of solid oxide fuel cells (SOFCs) was investigated. GDC buffer layer with 0.25-10 mol% CuO sintering aid was prepared by reacting GDC power and copper nitrate solution followed by heating at 600 ℃. The sintering of CuO-added GDC powder was optimized by investigating linear shrinkage, microstructure, grain size, ionic conductivity, and activation energy of CuO-GDC electrolytes at temperatures ranging from 1100 to 1400 ℃. The sintering temperature of the CuO-GDC electrolyte decreases from 1400 ℃ to 1100 ℃ by adding the CuO sintering aid. The ionic conductivity of the CuO-GDC electrolyte shows a maximum value at 0.5 mol% of CuO. However, the addition of CuO has no significant effects on the activation energy of GDC electrolyte. GDC-LSCF layers were co-sintering at 1050 and 1100 ℃ and button cell tests were carried out at 750 ℃.

Keywords: Co-Sintering, GDC-LSCF, Sintering Aid, solid Oxide Cells

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Authors: Zoran Visak, Joana Lopes, Vesna Najdanovic-Visak

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Within this study, the separation of nicotine from its aqueous solutions, using inorganic salt sodium chloride or ionic liquid (molten salt) ECOENG212® as salting-out media, was carried out. Thus, liquid-liquid equilibria of the ternary solutions (nicotine+water+NaCl) and (nicotine+water+ECOENG212®) were determined at ambient pressure, 0.1 MPa, at three temperatures. The related phase diagrams were constructed in two manners: by adding the determined cloud-points and by the chemical analysis of phases in equilibrium (tie-line data). The latter were used to calculate two important separation parameters - partition coefficients of nicotine and separation factors. The impacts of the initial compositions of the mother solutions and of temperature on the liquid-liquid phase separation and partition coefficients were analyzed and discussed. The results obtained clearly showed that both investigated salts are good salting-out media for the efficient and sustainable separation of nicotine from its solutions with water. However, when compared, sodium chloride exhibited much better separation performance than the ionic liquid.

Keywords: nicotine, liquid-liquid separation, inorganic salt, ionic liquid

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Authors: Andualem Belachew Workie

Abstract:

In a spray pyrolysis process, apatite-Wollastonite glass-ceramics (AW GC) were fabricated with the composition 8.29MgO_50.09-x CaO_34.46SiO2_7.16P2O5_xCaF₂, where x = 0, 0.54, and 5.24 (wt. %). Based on the results, it appears that the CaF2 addition lowers the glass transition temperature (Tg) and crystallization temperature (Tc) of the glasscomposition. In addition, AW GC's bioactivity increases as the soaking time in simulated body fluid (SBF) increases. Adding CaF₂ and varying sintering temperatures altered the density and linear shrinkage percentage of the samples. The formation of fluorapatite with needle-like microstructure and the formation of the wollastonite phase was enhanced with higher CaF2 content, while the growth of the whitlockite phase took place at a higher heat treatment temperature. Adding high CaF₂ content with high sintering temperatures to apatite Wollastonite glass-ceramic composition facilitates the formation of fluorapatite, which is crucial for denture glass-ceramics.

Keywords: apatite-wollastonite glass ceramics, bioactivity, hydroxyapatite, calcium fluoride

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Authors: Qianying Sun, Abdelhadi Kassiba, Guorong Li

Abstract:

ZnO with wurtzite structure is a well-known semiconducting oxide (SCO), being applied in thermoelectric devices, varistors, gas sensors, transparent electrodes, solar cells, liquid crystal displays, piezoelectric and electro-optical devices. Intrinsically, ZnO is weakly n-type SCO due to native defects (Znⱼ, Vₒ). However, the substitutional doping by metallic elements as (Al, Ti) gives rise to a high n-type conductivity ensured by donor centers. Under CO+N₂ sintering atmosphere, Schottky barriers of ZnO ceramics will be suppressed by lowering the concentration of acceptors at grain boundaries and then inducing a large increase in the Hall mobility, thereby increasing the conductivity. The presented work concerns ZnO based ceramics, which are fabricated with doping by TiO₂ (0.50mol%), Al₂O₃ (0.25mol%) and MgO (1.00mol%) and sintering in different atmospheres (Air (A), N₂ (N), CO+N₂(C)). We obtained uniform, dense ceramics with ZnO as the main phase and Zn₂TiO₄ spinel as a secondary and minor phase. An important increase of the conductivity was shown for the samples A, N, and C which were sintered under different atmospheres. The highest conductivity (σ = 1.52×10⁵ S·m⁻¹) was obtained under the reducing atmosphere (CO). The role of doping was investigated with the aim to identify the local environment and valence states of the doping elements. Thus, Electron paramagnetic spectroscopy (EPR) determines the concentration of defects and the effects of charge carriers in ZnO ceramics as a function of the sintering atmospheres. The relation between conductivity and defects concentration shows the opposite behavior between these parameters suggesting that defects act as traps for charge carriers. For Al ions, nuclear magnetic resonance (NMR) technique was used to identify the involved local coordination of these ions. Beyond the six and forth coordinated Al, an additional NMR signature of ZnO based TCO requires analysis taking into account the grain boundaries and the conductivity through the Knight shift effects. From the thermal evolution of the conductivity as a function of the sintering atmosphere, we succeed in defining the conditions to realize ZnO based TCO ceramics with an important thermal coefficient of resistance (TCR) which is promising for electrical safety of devices.

Keywords: ceramics, conductivity, defects, TCO, ZnO

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Authors: A. Bara, D. Barkat

Abstract:

The liquid-liquid extraction of copper (II) from aqueous solution by capric acid (HL) in chloroform at 25°C has been studied. The ionic strength effect of the aqueous phase shows that the extraction of copper(II) increases with the increase in ionic strength. with different ionic strengths 1, 0.5, 0.25, 0.125 and 0.1M in the aqueous phase. Cu (II) is extracted as the complex CuL2(ClO4).

Keywords: liquid-liquid extraction, ionic strength, copper (II), capric acid

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Authors: Ahmet Yönetken

Abstract:

Al metal matrix composites reinforced with AlN have been fabricated by Tube furnace sintering at various temperatures. A uniform nickel layer on Al(%1AlN)%19Ni, Al(%2AlN)%18Ni, Al(%3AlN)%17Ni, Al(%4AlN)%16Ni, Al(%5AlN)%15Ni powders were deposited prior to sintering using electroless plating technique, allowing closer surface contact than can be achieved using conventional methods such as mechanical alloying. A composite consisting of quaternary additions, a ceramic phase, AlN, within a matrix of Al, AlN, Ni has been prepared at the temperature range between 550°C and 650°C under Ar shroud. X-Ray diffraction, SEM (Scanning Electron Microscope) density, and hardness measurements were employed to characterize the properties of the specimens. Experimental results carried out for 650°C suggest that the best properties as comprehension strength σmax and hardness 681.51(HV) were obtained at 650°C, and the tube furnace sintering of electroless Al plated (%5AlN)%15Ni powders is a promising technique to produce ceramic reinforced Al (%5AlN)%15Ni composites.

Keywords: electroless nickel plating, ceramic-metal composites, powder metallurgy, sintering

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Authors: Yih-Chien Chen, Yu-Cheng You

Abstract:

The microwave dielectric properties of La2MoO6 ceramics were investigated with a view to their application in mobile communication. La2MoO6 ceramics were prepared by the conventional solid-state method with various sintering conditions. The X-ray diffraction peaks of La2MoO6 ceramic did not vary significantly with sintering conditions. The average grain size of La2MoO6 ceramics increased as the temperature and time of sintering increased. A maximum density of 5.67 g/cm3, a dielectric constants (εr) of 14.1, a quality factor (Q×f) of 68,000 GHz, and a temperature coefficient of resonant frequency (τf) of -56 ppm/℃ were obtained when La2MoO6 ceramics that were sintered at 1300 ℃ for 4h.

Keywords: ceramics, sintering, microwave dielectric properties, La2MoO6

Procedia PDF Downloads 258