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At least 235 records · Page 13

Implementation of a spark plasma sintering facility in a hermetic glovebox for compaction of toxic, radiotoxic, and air sensitive materials

Spark plasma sintering (SPS) is a rapidly developing method for densification of powders into compacts. It belongs to the so-called “field assisted sintering techniques” that enable rapid sintering at much lower temperatures than the classical approaches of pressureless sintering of green pellets or hot isostatic pressing. In this paper, we report the successful integration of a SPS device into a hermetic glovebox for the handling of highly radioactive material containing radioisotopes of U, Th, Pu, Np, and Am. The glovebox implantation has been facilitated by the replacement of the hydraulic system to apply pressure with a compact electromechanical unit. The facility has been successfully tested using UO{sub 2} powder. Pellets with 97% of the theoretical density were obtained at 1000 °C for 5 min, significantly lower than the ∼1600 °C for 5-10 h used in conventional pellet sintering.

36 MATERIALS SCIENCE↗

The influence of sintering temperature on microstructure and mechanical properties of Ni-Al intermetallics fabricated by SPS

In the present study PN85Yu15 was used as elemental powder to produce a sintered compound with Ni3Al as main phase. The Spark Plasma Sintering (SPS) technique is used to compact the powders. The powder was sintered in a temperature range between 1000°C and 1150°C to observe the influence of the sintering temperature on the microstructure and the mechanical properties. The microstructure was observed with optical microscope (OM), the phase composition was characterized by X-ray diffraction (XRD) technique. Density and microhardness were observed and compared the values with the results of other researchers. The compressive-, density- and microhardness tests show as clear result that with increasing the sintering temperature nearly all properties become better and also the microstructure studies show that porous places become less.

36 MATERIALS SCIENCE↗

Fabrication and characterization of spark plasma sintered Ce:LuAG ceramic for scintillation application

Rare earth Cerium doped Lutetium Aluminum Garnet (Ce:LuAG) ceramics are widely used as phosphor material in medical imaging and high-energy physics. Due to its technological importance, an attempt has been made to fabricate Ce:LuAG ceramics by using spark plasma sintering (SPS) technique. XRD patterns of SPS sintered Ce:LuAG ceramics reveals a mixed LuAG and CeO{sub 2} (antisite defect) phases. The microstructures of SPS sintered Ce:LuAG ceramics shows limited densification, inappropriate compaction of particles and existence of residual pores, voids between the grain boundaries affects the transparency of Ce:LuAG ceramics. Relative density and hardness of post sintered Ce:LuAG ceramic is also determined. The effect of Ce{sup 3+} doping concentration and sintering temperature on optical luminescence behavior of Ce:LuAG ceramic is presented.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Surface-selective laser sintering of thermolabile polymer particles using water as heating sensitizer

We report the implementation of a novel scheme for surface-selective laser sintering (SSLS) of polymer particles, based on using water as a sensitizer of laser heating and sintering of particles as well as laser radiation at a wavelength of 1.94 μm, corresponding to the strong absorption band of water. A method of sintering powders of poly(lactide-co-glycolide), a hydrophobic bioresorbable polymer, after modifying its surface with an aqueous solution of hyaluronic acid is developed. The sintering thresholds for wetted polymer are by 3 – 4 times lower than those for sintering in air. The presence of water restricts the temperature of the heated polymer, preventing its thermal destruction. Polymer matrices with a developed porous structure are obtained. The proposed SSLS method can be applied to produce bioresorbable polymer matrices for tissue engineering. (interaction of laser radiation with matter. laser plasma)

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

THE SINTERING REGION OF ICY DUST AGGREGATES IN A PROTOPLANETARY NEBULA

Icy grain aggregates are formed in the outer region of a protoplanetary nebula. The infall of these aggregates to the central star is due to gas drag, and their temperature increases as the infall proceeds. The icy molecules on the grain move to the neck where the grains get connected through sublimation and condensation of the molecules. This process is called sintering. As the sintering proceeds, the mechanical strength of the neck changes considerably, strongly affecting the collisional evolution of the aggregates. The timescale required for sintering is determined in this study, based on which the region where the sintering proceeds within a prescribed timescale is obtained. It is found that the region covers a substantial fraction of the protoplanetary nebula, and the location of the region depends on the temperature distribution inside the nebula. If the aggregate is stirred up and the temperature of the aggregate increases temporally, the sintering region spreads to the whole nebula.

79 ASTRONOMY AND ASTROPHYSICS↗

Thermomechanical Degradation of Sintered Copper Under High-Temperature Thermal Shock

The need for reliable bonded interface materials is critical to realize the performance benefits of wide-bandgap devices in power electronics modules, especially in operating temperatures greater than 150 degrees C. In this paper, we investigate the thermomechanical performance of sintered copper (Cu) as a large-area attachment, bonded between Cu baseplates and active-metal-bonded substrates, under accelerated thermal shock (-40 degrees C to 200 degrees C) conditions. In the fabrication phase of the samples, we used different stencil patterns and found that the grid and stripe patterns resulted in a better outgassing of the residual organics during the sintering process, thereby ensuring a substantially improved bond quality compared to a full-area print. The paste consisted of Cu microflakes, and we performed sintering using a Budatec SP300 sintering press at 275 degrees C with 15 MPa of bonding pressure for 5 minutes in a nitrogen atmosphere. Under accelerated experiments, we monitored the degradation of the sintered Cu bond in the samples through C-mode scanning acoustic microscope (C-SAM) images. To quantify the defect percentage in C-SAM images, we investigated image denoising techniques to exclude the pattern prints. Finally, we cross-sectioned a sample and obtained scanning electron microscope images, which revealed adhesive fracture as the dominant failure mechanism.

ADVANCED PROPULSION SYSTEMS,INORGANIC, ORGANIC, PH↗

Characterization of Green-Emitting Translucent Zinc Oxide Ceramics Prepared Via Spark Plasma Sintering

Translucent, green-emitting zinc oxide (ZnO) bodies, 19 mm in diameter and 0.72 mm in thickness, have been prepared via spark plasma sintering method. The consolidation of ZnO powders was investigated over the temperature range of 550-1050 C and the pressure range of 55-530 MPa. Samples sintered at temperatures >850 C and pressures of {approx}120 MPa were translucent and had densities of {approx}100%. Samples sintered at 950 C and 130 MPa showed a higher maximum transmittance than the samples sintered at higher or lower temperatures or pressures, with an excellent in-line transmission of 70% in the IR region around 2330 nm. The dense ZnO ceramics exhibited a strong green emission and a weak ultraviolet emission, and the relative intensity of the green emission increased with increasing sintering temperature.

36 MATERIALS SCIENCE↗

Structural and Phase Transformations in Alloys during Spark Plasma Sintering of Ti + 23.5 at % Al + 21 at % Nb Powder Mixtures

We have studied the effect of sintering temperature on the structural and phase transformations of alloys produced by the spark plasma sintering of Ti + 23.5 at % Al + 21 at % Nb powder mixtures at temperatures in the range 1100–1550°C. The sintered alloys have been characterized by X-ray diffraction, scanning electron microscopy, and energy dispersive X-ray spectroscopy (elemental X-ray mapping). The alloys sintered at temperatures of 1100 and 1200°C have been shown to have a nonuniform microstructure. According to electron microscopy results, the alloys consist of grains of the α{sub 2} and Nb{sub 2}Al phases and small precipitates of the O-phase (intermetallic compound Ti{sub 2}AlNb). In addition, there are particles of unreacted niobium and titanium. The alloys sintered at a temperature of 1300°C have a uniform lamellar structure.

36 MATERIALS SCIENCE↗

Laser sintering of a TiO{sub 2} nanoporous film on a flexible substrate for application in solar cells

The selective laser sintering of TiO{sub 2}-film nanoparticles on a plastic conductive substrate is considered for application in flexible dye-sensitized solar cells. It is shown that the absorbed energy of the laser radiation during laser sintering promotes electrical-contact formation between TiO{sub 2} nanoparticles without damaging the plastic conductive substrate. The choice of a near-infrared laser radiation (wavelength of 1064 nm) provides an efficient laser-sintering process. The laser-sintering method promotes a decrease in recombination losses in the TiO{sub 2} film and an improvement in the charge-collection efficiency, which can result in an increase in the efficiency of such solar cells. Furthermore, the efficient-laser sintering method has a great potential for application in the roll-to-roll technology of the fabrication of high-efficiency flexible solar cells.

36 MATERIALS SCIENCE↗

Long-Term Cr Poisoning Effect on LSCF-GDC Composite Cathodes Sintered at Different Temperatures

Here, the impact of sintering temperature on Cr-poisoning of solid oxide fuel cell (SOFC) cathodes was systematically studied. La 0.6 Sr 0.4 Fe 0.8 Co 0.2 O 3-δ - Ce 0.9 Gd 0.1 O 2-δ symmetric cells were aged at 750°C in synthetic air with the presence of Crofer 22 APU, a common high temperature interconnect, over 200 hours and electrochemical impedance spectroscopy (EIS) was used to determine the degradation process. Both the ohmic resistance (R Ω ) and polarization resistance (R P ) of LSCF-GDC cells, extracted from EIS spectra, for different sintering temperatures increase as a function of aging time. Furthermore, the Cr-related degradation rate increases with decreased cathode sintering temperature. The polarization resistance of cathode sintered at lower temperature (950°C) increases dramatically while aging with the presence of Cr and also significantly decreases the oxygen partial pressure dependence after aging. The degradation rate shows a positive correlation to the concentration of Cr. The results indicate that decreased sintering temperature increases the total surface area, leading to more available sites for Sr-Cr-O nucleation and thus greater Cr degradation.

30 DIRECT ENERGY CONVERSION↗

Oxidation Protection of Uranium Nitride Fuel using Liquid Phase Sintering

Two methods are proposed to increase the oxidation resistance of uranium nitride (UN) nuclear fuel. These paths are: (1) Addition of USi{sub x} (e.g. U3Si2) to UN nitride powder, followed by liquid phase sintering, and (2) 'alloying' UN nitride with various compounds (followed by densification via Spark Plasma Sintering or Liquid Phase Sintering) that will greatly increase oxidation resistance. The advantages (high thermal conductivity, very high melting point, and high density) of nitride fuel have long been recognized. The sodium cooled BR-10 reactor in Russia operated for 18 years on uranium nitride fuel (UN was used as the driver fuel for two core loads). However, the potential advantages (large power up-grade, increased cycle lengths, possible high burn-ups) as a Light Water Reactor (LWR) fuel are offset by uranium nitride's extremely low oxidation resistance (UN powders oxidize in air and UN pellets decompose in hot water). Innovative research is proposed to solve this problem and thereby provide an accident tolerant LWR fuel that would resist water leaks and high temperature steam oxidation/spalling during an accident. It is proposed that we investigate two methods to increase the oxidation resistance of UN: (1) Addition of USi{sub x} (e.g. U 3 Si 2 ) to UN nitride powder, followed by liquid phase sintering, and (2) 'alloying' UN nitride with compounds (followed by densification via Spark Plasma Sintering) that will greatly increase oxidation resistance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Study of the U{sub 3}O{sub 8} effect on MOX fuel sintering mechanisms

The manufacturing of uranium-plutonium mixed oxides fuel (also known as MOX) for light water reactor (LWR), starting generally from UO{sub 2} and PuO{sub 2} raw powders and resulting in (U,Pu)O{sub 2} pellets, involves several steps: i) preparation of a UO{sub 2}+PuO{sub 2} master blend with a Pu content of about 25-30 at% by milling and sieving, ii) dilution by mixing the master blend with non-milled UO{sub 2} to reach a Pu content of about 10 at%, iii) pressing and iv) sintering under Ar / 4 % H{sub 2} + H{sub 2}O gas mixture. In this paper, triuranium octoxide (U{sub 3}O{sub 8}) is used as an additional raw powder in the LWR MOX fuel manufacturing. One of the objectives of this work is to understand the sintering behavior of U{sub 3}O{sub 8} under Ar / 4 % H{sub 2} + H{sub 2}O gas mixture and its effect when added to a UO{sub 2}-PuO{sub 2} mixture. A special attention is given on U{sub 3}O{sub 8} reduction, phase transitions, redox reactions and oxygen partial pressure (pO{sub 2}) evolution during shrinkage: the impact of these phenomena on the densification kinetics is discussed, especially the de-densification phenomenon which could occur at high temperature. For that purpose a specific dilatometer, coupled with a zirconia probe implemented at furnace inlet and outlet has been used which allows following continuously and simultaneously the fuel shrinkage and the oxygen partial pressure variation as a function of temperature. The experiments have shown that, contrary to UO{sub 2}, the sintering of milled PuO{sub 2} is accompanied by a de-densification at high temperature. This de-densification phenomenon already occurs with co-milled 71 at% UO{sub 2} + 29 at% PuO{sub 2}, but with a smaller magnitude. When pure milled U{sub 3}O{sub 8} is sintered, no de-densification phenomenon is observed but the low density of the sintered pellet could hide such a phenomenon. The incorporation of U{sub 3}O{sub 8} into a UO{sub 2}-PuO{sub 2} master blend containing 29 at% of plutonium leads to an exacerbation of the de-densification phenomenon with a higher loss on ignition suggesting that U{sub 3}O{sub 8} contributes also to the de-densification phenomenon. This could be due to high temperature reactions involving the initial carbon content of the raw U{sub 3}O{sub 8} powder. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Sintering-based Metal Additive Manufacturing Methods for Magnetic Materials

In this chapter, we review the relationship between solid-state sintering and additive manufacturing (AM) methods for fabricating soft and hard magnetic materials. Heat treatment as a post-processing method has been done in conjunction with AM as a method to improve density and/or mechanical properties. In binder jetting (BJT) of metal powders, sintering is a crucial post-processing step and is necessary for obtaining the final product. This is because the parts are only in the “green” state when they leave the BJT printer, with poor mechanical properties and high porosity. Sintering densifies and strengthens the green part into the final product. A potential industrial application for sintering-based AM is the fabrication of magnetic materials. The motivation for doing so, the process and properties of the AM magnets, and the potential applications of post-sintered AM magnets are explored.

Wang, Haobo↗

An Aerosol Jet Printed Resistance Temperature Detector‐Micro Hotplate with Temperature Coefficient of Resistance Stabilized by Electrical Sintering

Abstract Aerosol jet printing (AJP) is an emerging direct write tool enabling rapid prototyping and fabrication of electronics components. AJP provides faster and less expensive production of devices with feature sizes of >10 microns compared to traditional MEMS processes. Herein, the fabrication of a resistance temperature detector‐micro hotplate (RTD‐µHP) is reported using AJP printed silver. AJP eliminates sophisticated MEMS processes such as masking, alignment, and etching. The compatibility of the AJP process with a broad range of materials is demonstrated by printing highly resolved lines on rigid and flexible substrates. Optimal thermal sintering conditions of AJP printed silver (Ag) lines are found by in situ resistance measurements. To stabilize the temperature coefficient of resistance (TCR) of the RTD‐µHP at high operating current levels, electrical sintering is performed on the RTD‐µHPs. Electrical sintering improves the conductivity of fully thermally sintered Ag RTD‐µHPs by 32% and provides a burn‐in mechanism for stabilizing the TCR. The TCR of the RTD‐µHPs after electrical sintering is 3.80 × 10 −3 at 22 °C, close to the value for bulk Ag. The performance of the RTD‐µHPs is tested using a reference thermocouple. The RTD‐µHPs show reliable and repeatable heating and temperature sensing up to 70 °C in air.

Sui, Yongkun↗

In-situ observation of oxygen mobility and abnormal lattice expansion in ceria during flash sintering

Flash sintering has been shown to be an effective method of sintering for many types of ceramics. However, the characteristics of flash sintering for each type of ceramic varies. When ionically conducting ceramics are sintered under a DC electric field, a strong dependence of densification with respect to position is observed. Microstructural analysis of the effect of electric field on oxygen ion conductors shows non-stoichiometry (oxygen deficiency) at the cathode which continues to build up over time under flash. In oxygen ion conductors, dominant charge carriers during flash are oxygen ions and the final density of the specimen is related to the availability of oxygen. This effect is no longer evident when using an AC power supply. In conclusion, use of AC instead of DC electric field is preferable for flash sintering of ionically conducting ceramics.

36 MATERIALS SCIENCE↗

Microstructure and DC electrical conductivity of spinel nickel ferrite sintered in air and nitrogen atmospheres

In recent years, the development of inert anode materials has gained considerable attention because such materials are capable of producing only environment-friendly O{sub 2} and saving energy during aluminum electrolysis. Nickel ferrite was prepared by a solid-state reaction as the inert anode in this study and its microstructures and direct current conductivities were analyzed in detail regarding the effects of different sintering atmospheres. A single-phase spinel structure was confirmed for all samples by X-ray powder diffraction. The grain sizes and the relative densities of the samples sintered in nitrogen increased by over 7 {mu}m and 10.8%, respectively, compared to those sintered in air. The direct current conductivities of the samples sintered in nitrogen showed a drastic increase compared to those sintered in air, believed to be due to the effects of increased Fe{sup 2+} ion concentration at octahedral sites and the increase of the relative density.

36 MATERIALS SCIENCE↗

Gas response properties of citrate gel synthesized nanocrystalline MgFe{sub 2}O{sub 4}: Effect of sintering temperature

Graphical abstract: Display Omitted Highlights: ► Synthesis of nanocrystalline MgFe{sub 2}O{sub 4} by economical citrate gel combustion method. ► Structural, morphological, and gas response properties of MgFe{sub 2}O{sub 4}. ► Enhancement in selectivity of MgFe{sub 2}O{sub 4} towards LPG with sintering temperature. ► Use of MgFe{sub 2}O{sub 4} to detect different gases at different operating temperatures. -- Abstract: Spinel type MgFe{sub 2}O{sub 4} material was synthesized by citrate gel combustion method. The effect of sintering temperature on structural, morphological, and gas response properties was studied. The powder X-ray diffraction pattern and transmission electron microscope study confirms nanocrystalline spinel structure of the synthesized powder. The material was tested for response properties to various reducing gases like liquid petroleum gas (LPG), acetone, ethanol, and ammonia. The results demonstrated n-type semiconducting behavior of MgFe{sub 2}O{sub 4} material. It was revealed that MgFe{sub 2}O{sub 4} sintered at 973 K was most sensitive to LPG at 648 K and to acetone at 498 K. However MgFe{sub 2}O{sub 4} sintered at 1173 K exhibited higher response and selectivity to LPG with marginal increase in the operating temperature. Furthermore, the sensor exhibited a fast response and a good recovery. It was observed that the particles size, porosity, and surface activity of the sensor material is affected by the sintering temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

In situ observations of cracking in constrained sintering

Here in this article, we examine the long-standing problem of cracking during constrained sintering of a powder aggregate. Using binder jet 3D printing, we prepare ceramic green bodies in the form of center-notched panels, then use in situ imaging to observe how cracks nucleate and grow from the notch as the material sinters under restraint. Quantitative image analysis allows us to identify important characteristics of the sinter-cracking process, indicating a framework for analyzing the problem and developing methods for avoiding it, including representation of sinter-cracking as a creep crack growth process, use of fracture mechanics parameters to design specimen geometries that do not exceed critical stress intensities, and the possibility of exploiting the inherently ductile nature of sinter-cracking to mitigate damage.

36 MATERIALS SCIENCE↗