Metal-Intermetallic Laminate Ti-Al3Ti Composites Produced by Spark Plasma Sintering of Titanium and Aluminum Foils Enclosed in Titanium Shells

NASA Astrophysics Data System (ADS)

Lazurenko, Daria V.; Mali, Vyacheslav I.; Bataev, Ivan A.; Thoemmes, Alexander; Bataev, Anatoly A.; Popelukh, Albert I.; Anisimov, Alexander G.; Belousova, Natalia S.

2015-09-01

Metal-intermetallic laminate composites are considered as promising materials for application in the aerospace industry. In this study, Ti-Al3Ti composites enclosed in titanium cases were produced by reactive spark plasma sintering. Sintering was carried out at 1103 K and 1323 K (830 °C and 1050 °C) for 10 minutes. In both cases, high-quality Ti-Al3Ti composites containing thin transition layers at the interfaces were obtained. Al2Ti, AlTi, and AlTi3 intermetallic phases and a solid solution of aluminum in titanium were observed in the transition layers by scanning and transmission electron microscopy. The material sintered at 1323 K (1050 °C) had higher strength in comparison with the composite obtained at 1103 K (830 °C). However, the hardness of the intermetallic component in the sample sintered at higher temperature decreased due to the grain growth. The impact toughness values of both materials were approximately identical.

Manufacturing issues and optical properties of rare-earth (Y, Lu, Sc, Nd) aluminate garnets composite transparent ceramics

NASA Astrophysics Data System (ADS)

Bonnet, Loïck; Boulesteix, Rémy; Maître, Alexandre; Sallé, Christian; Couderc, Vincent; Brenier, Alain

2015-12-01

In this work, a comparative study of reactive sintering and optical properties of three laser composite transparent ceramics doped with neodymium: Nd:YAG/Nd:YS1AG, Nd:YAG/Nd:LuAG and Nd:YS1AG/Nd:LuAG has been achieved. Samples were manufactured thanks to pressureless co-sintering under vacuum of bilayer powder compacts. The reaction sequence from primary oxides to final garnet phases has been investigated. Similar dilatometric behavior was observed during reactive-sintering for each composition. Differential shrinkage can be thus accommodated to some extent. Second, this work has shown that the intermediate zone at composites interface is composed of single-phased garnet solid-solution with continuous evolution from one side to the other. The thickness of the interdiffusion zone was found to be limited to about 100 μm in all cases and appeared to be well described by classical diffusion laws of Fick and Whipple-Le Claire. The analyses of spectroscopic properties of transparent ceramics composites have finally shown that composite ceramics should be suitable to produce dual wavelength emission for terahertz generation.

The Fabrication of All-Solid-State Lithium-Ion Batteries via Spark Plasma Sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wei, Xialu; Rechtin, Jack; Olevsky, Eugene

Spark plasma sintering (SPS) has been successfully used to produce all-solid-state lithium-ion batteries (ASSLibs). Both regular and functionally graded electrodes are implemented into novel three-layer and five-layer battery designs together with solid-state composite electrolyte. The electrical capacities and the conductivities of the SPS-processed ASSLibs are evaluated using the galvanostatic charge-discharge test. Experimental results have shown that, compared to the three-layer battery, the five-layer battery is able to improve energy and power densities. Scanning electron microscopy (SEM) is employed to examine the microstructures of the batteries especially at the electrode–electrolyte interfaces. It reveals that the functionally graded structure can eliminate themore » delamination effect at the electrode–electrolyte interface and, therefore, retains better performance.« less

The Fabrication of All-Solid-State Lithium-Ion Batteries via Spark Plasma Sintering

DOE PAGES

Wei, Xialu; Rechtin, Jack; Olevsky, Eugene

2017-09-14

Spark plasma sintering (SPS) has been successfully used to produce all-solid-state lithium-ion batteries (ASSLibs). Both regular and functionally graded electrodes are implemented into novel three-layer and five-layer battery designs together with solid-state composite electrolyte. The electrical capacities and the conductivities of the SPS-processed ASSLibs are evaluated using the galvanostatic charge-discharge test. Experimental results have shown that, compared to the three-layer battery, the five-layer battery is able to improve energy and power densities. Scanning electron microscopy (SEM) is employed to examine the microstructures of the batteries especially at the electrode–electrolyte interfaces. It reveals that the functionally graded structure can eliminate themore » delamination effect at the electrode–electrolyte interface and, therefore, retains better performance.« less

Hardness of pulsed electric current sintered and hot isostatically pressed Mo(Si,Al)2

NASA Astrophysics Data System (ADS)

Tanabe, Jun

2005-05-01

We improved the reactivity and mechanical characteristics of Mo(Si,Al)2 by pulsed electric current sintering (PECS) and hot isostatic pressing (HIP), and evaluated its reaction state and mechanical characteristics using energy dispersive spectroscopy (EDS), X-ray diffraction, and a hardness test. Mo(Si,Al)2 was generated by pretreatment using a furnace, and the application of the PECS and HIP treatments further densified the sintered body, resulting in an increase in the hardness.

Monoclinic β-Li2TiO3 nanocrystalline particles employing novel urea assisted solid state route: Synthesis, characterization and sintering behavior

NASA Astrophysics Data System (ADS)

Tripathi, Biranchi M.; Mohanty, Trupti; Prakash, Deep; Tyagi, A. K.; Sinha, P. K.

2017-07-01

Pure phase monoclinic nano-crystalline Li2TiO3 powder was synthesized by a novel urea assisted solid state synthesis method using readily available and economical precursors. A single phase and well crystalline Li2TiO3 powder has been obtained at slightly lower temperature (600-700 °C) and shorter duration (2 h) as compared to the conventional solid state method. The proposed method has significant advantages in comparison to other viable methods mainly in terms of phase purity, powder properties and sinterability. Analysis of chemical composition using inductively coupled plasma atomic emission spectroscopy (ICP-AES) shows no loss of lithium from Li2TiO3 in the proposed method. The emergence of monoclinic Li2TiO3 phase was confirmed by X-ray diffraction (XRD) pattern of as-synthesized powder. The crystallite size of Li2TiO3 powder was calculated to be in the range of 15-80 nm, which varied as a function of urea composition and temperature. The morphology of as-prepared Li2TiO3 powders was examined by scanning electron microscope (SEM). The effect of urea composition on phase and morphology was investigated so as to delineate the role of urea. Upon sintering at < 1000 °C temperature, the Li2TiO3 powder compact attained about 98% of the theoretical density with fine grained (grain size: 2-3 μm) microstructure. It indicates excellent sinter-ability of Li2TiO3 powder synthesized by the proposed method. The fine grained structure is desirable for better tritium breeding performance of Li2TiO3. Electrochemical impedance spectroscopy at variable temperature showed good electrical properties of Li2TiO3. The proposed method is simple, anticipated to be cost effective and convenient to realise for large scale production of phase pure nanocrystalline and having significantly enhanced sinter-ability Li2TiO3 powder.

Influence of sintering temperature on properties of BNKLLT-6 wt% BCTZ binary lead-free piezoelectric ceramic prepared through the solid-state combustion technique

NASA Astrophysics Data System (ADS)

Kornphom, Chittakorn; Laowanidwatana, Artid; Bongkarn, Theerachai

2017-03-01

In this work, a new binary 94 wt%[Bi0.5(Na0.68K0.22Li0.1)0.5TiO3 + 0.10 wt% of La2O3]-6 wt% [(Ba0.85Ca0.15)(Ti0.90Zr0.10)O3] [BNKLLT-6 wt% BCTZ] ceramic was fabricated by the solid-state combustion technique and glycine was used as the fuel. The effect of sintering temperature in the range of 1075-1175 °C for 2 h on phase evolution, microstructure and electrical properties was investigated. The phase formation exhibited a coexistence structure between rhombohedral and tetragonal at low sintering temperature. As the sintering temperature increased, the phase formation changed to pseudo-cubic phase. The average grain size of the ceramics was increased with the increasing sintering temperature. Density, ɛr, ɛSA and TFA of BNKLLT-6 wt% BCTZ ceramics increased while the TSA decreased when the sintering temperature increased up to 1125 °C, while after this temperature the opposite trends occurred. At a sintering temperature of 1125 °C, the BNKLLT-6 wt% BCTZ sample showed the highest theoretical density (95.8%), maximum dielectric constant ɛSA (5278), highest d33 (227 pC/N) and fair ferroelectric properties (Pr = 24.5 µC/cm2 and Ec = 15.45 kV/cm).

Structures and fabrication techniques for solid state electrochemical devices

DOEpatents

Visco, Steven J.; Jacobson, Craig P.; DeJonghe, Lutgard C.

2006-10-10

Low-cost, mechanically strong, highly electronically conductive porous substrates and associated structures for solid-state electrochemical devices, techniques for forming these structures, and devices incorporating the structures provide solid state electrochemical device substrates of novel composition and techniques for forming thin electrode/membrane/electrolyte coatings on the novel or more conventional substrates. In particular, in one aspect the invention provides techniques for co-firing of device substrate (often an electrode) with an electrolyte or membrane layer to form densified electrolyte/membrane films 5 to 20 microns thick. In another aspect, densified electrolyte/membrane films 5 to 20 microns thick may be formed on a pre-sintered substrate by a constrained sintering process. In some cases, the substrate may be a porous metal, alloy, or non-nickel cermet incorporating one or more of the transition metals Cr, Fe and Cu, or alloys thereof.

A comparative study of conventionally sintered and microwave sintered nickel zinc ferrite

NASA Astrophysics Data System (ADS)

Rani, Rekha; Juneja, J. K.; Raina, K. K.; Kotnala, R. K.; Prakash, Chandra

2014-04-01

For the present work, nickel zinc ferrite having compositional formula Ni0.8Zn0.2Fe2O4 was synthesized by conventional solid state method and sintered in conventional and microwave furnaces. Pellets were sintered with very short soaking time of 10 min at 1150 °C in microwave furnace whereas 4 hrs of soaking time was selected for conventional sintering at 1200 °C. Phase formation was confirmed by X-ray diffraction analysis technique. Scanning electron micrographs were taken for microstructural study. Dielectric properties were studied as a function of temperature. To study magnetic behavior, M-H hysteresis loops were recorded for both samples. It is observed that microwave sintered sample could obtain comparable properties to the conventionally sintered one in lesser soaking time at lower sintering temperature.

Synthesisofc-lifepo4 composite by solid state reaction method

NASA Astrophysics Data System (ADS)

Rahayu, I.; Hidayat, S.; Noviyanti, A. R.; Rakhmawaty, D.; Ernawati, E.

2017-02-01

In this research, the enhancement of LiFePO4 conductivity was conducted by doping method with carbon materials. Carbon-based materials were obtained from the mixture of sucrose, and the precursor of LiH2PO4 and α-Fe2O3 was synthesized by solid state reaction. Sintering temperature was varied at 700°C, 800°C, 900°C and 1,000°C. The result showed that C-LiFePO4 could be synthesized by using solid state reaction method. Based on the XRD and FTIR spectrums, C-LiFePO4 can be identified as the type of crystal, characterized by the appearance of sharp signal on (011), (211) and typical peak of LiFePO4 materials. The result of conductivity measurement from C-LiFePO4 at sintering temperature of 900°C and 1,000°C was 2×10-4 S/cm and 4×10-4S/cm, respectively. The conductivity value at sintering temperature of 700°C and 800°C was very small (<10-6 S/cm), which cannot be measured by the existing equipment.

2D all-solid state fabric supercapacitor fabricated via an all solution process for use in smart textiles

NASA Astrophysics Data System (ADS)

Jang, Yunseok; Jo, Jeongdai; Woo, Kyoohee; Lee, Seung-Hyun; Kwon, Sin; Kim, Kwang-Young; Kang, Dongwoo

2017-05-01

We propose a method to fabricate a supercapacitor for smart textiles using silver (Ag) nanoparticle (NP) ink, simple spray patterning systems, and intense pulsed light (IPL) sintering systems. The Ag NP current collectors provided as high conductivity as the metal current collectors. The spray patterning technique is useful for fabricating supercapacitors because it is simple, fast, and cheap. IPL systems reduced the sintering temperature of Ag NPs and prevented thermal damage to the textiles during the Ag NP sintering process. The two-dimensional (2D) all-solid state fabric supercapacitor with an interdigitated configuration, developed here, exhibited a specific capacitance of 25.7 F/g and an energy density of 1.5 Wh/kg at a power density of 64.3 W/kg. These results support the utility of our proposed method in the development of energy textiles.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sajgalik, P.; Sedlacek, J.; Lences, Z.

Densification of silicon carbide without any sintering aids by hot-pressing and rapid hot pressing was investigated. Full density (>99% t.d.) has been reached at 1850 °C, a temperature of at least 150-200 °C lower compared to the up to now known solid state sintered silicon carbide powders. Silicon carbide was freeze granulated and heat treated prior the densification. Furthermore, evolution of microstructure, mechanical properties and creep behavior were evaluated and compared to reference ceramics from as received silicon carbide powder as well as those of commercial one. Novel method results in dense ceramics with Vickers hardness and indentation fracture toughnessmore » of 29.0 GPa and 5.25 MPam 1/2, respectively. Moreover, the creep rate of 3.8 x 10 –9 s –1 at 1450 °C and the load of 100 MPa is comparable to the commercial α-SiC solid state sintered at 2150 °C.« less

Design and characterization of Yb and Nd doped transparent ceramics for high power laser applications: recent advancements

NASA Astrophysics Data System (ADS)

Lapucci, A.; Vannini, M.; Ciofini, M.; Pirri, A.; Nikl, M.; Li, J.; Esposito, L.; Biasini, V.; Hostasa, J.; Goto, T.; Boulon, G.; Maksimov, R.; Gizzi, L.; Labate, L.; Toci, G.

2017-01-01

We report a review on our recent developments in Yttebium and Neodymium doped laser ceramics, along two main research lines. The first is the design and development of Yb:YAG ceramics with non uniform doping distribution, for the management of thermo-mechanical stresses and for the mitigation of ASE: layered structures have been produced by solid state reactive sintering, using different forming processes (spray drying and cold press of the homogenized powders, tape cast of the slurry); samples have been characterized and compared to FEM analysis. The second is the investigation of Lutetium based ceramics (such as mixed garnets LuYAG and Lu2O3); this interest is mainly motivated by the favorable thermal properties of these hosts under high doping. We recently obtained for the first time high efficiency laser emission from Yb doped LuYAG ceramics. The investigation on sesquioxides has been focused on Nddoped Lu2O3 ceramics, fabricated with the Spark Plasma Sintering method (SPS). We recently achieved the first laser emission above 1 W from Nd doped Lu2O3 ceramics fabricated by SPS.

Lowering the synthesis temperature of Y3Fe5O12 by surfactant assisted solid state reaction

NASA Astrophysics Data System (ADS)

Xue, Fenghua; Huang, Ju; Li, Tianrui; Wang, Zifan; Zhou, Xiaochao; Wei, Lujun; Gao, Baizhi; Zhai, Ya; Li, Qi; Xu, Qingyu; Du, Jun

2018-01-01

There is an urgent technical requirement of lowering the sintering temperature of Y3Fe5O12 (YIG) for its practical applications. In this paper, a modified solid state reaction method is reported by adding the surfactant of cetyltrimethylammonium bromide (CTAB). A high sintering temperature of 1200 °C is required for the formation of YIG phase without adding CTAB, which is effectively decreased to 1050 °C by adding CTAB. The morphology studies show that the sintering temperature plays the main role in the crystal growth and excludes the possible contribution of CTAB. The prepared YIG ceramic samples show soft ferromagnetic properties, with coercivity of only 21.2 Oe for the sample prepared with CTAB at 1050 °C, which decreases with increasing sintering temperature. The main role of adding CTAB is preventing the agglomeration of ball milled ultrafine source particles, which may facilitate the interdiffusion among them and promote the reaction at lower temperatures. Furthermore, the Gilbert damping constant is significantly reduced for YIG prepared by adding CTAB, which is one order smaller than that without CTAB.

Structures And Fabrication Techniques For Solid State Electrochemical Devices

DOEpatents

Visco, Steven J.; Jacobson, Craig P.; DeJonghe, Lutgard C.

2005-12-27

Provided are low-cost, mechanically strong, highly electronically conductive porous substrates and associated structures for solid-state electrochemical devices, techniques for forming these structures, and devices incorporating the structures. The invention provides solid state electrochemical device substrates of novel composition and techniques for forming thin electrode/membrane/electrolyte coatings on the novel or more conventional substrates. In particular, in one embodiment the invention provides techniques for co-firing of device substrate (often an electrode) with an electrolyte or membrane layer to form densified electrolyte/membrane films 5 to 20 microns thick. In another embodiment, densified electrolyte/membrane films 5 to 20 microns thick may be formed on a pre-sintered substrate by a constrained sintering process. In some cases, the substrate may be a porous metal, alloy, or non-nickel cermet incorporating one or more of the transition metals Cr, Fe, Cu and Ag, or alloys thereof.

Structures and fabrication techniques for solid state electrochemical devices

DOEpatents

Visco, Steven J.; Jacobson, Craig P.; DeJonghe, Lutgard C.

2003-08-12

Provided are low-cost, mechanically strong, highly electronically conductive porous substrates and associated structures for solid-state electrochemical devices, techniques for forming these structures, and devices incorporating the structures. The invention provides solid state electrochemical device substrates of novel composition and techniques for forming thin electrode/membrane/electrolyte coatings on the novel or more conventional substrates. In particular, in one embodiment the invention provides techniques for co-firing of device substrate (often an electrode) with an electrolyte or membrane layer to form densified electrolyte/membrane films 5 to 20 microns thick. In another embodiment, densified electrolyte/membrane films 5 to 20 microns thick may be formed on a pre-sintered substrate by a constrained sintering process. In some cases, the substrate may be a porous metal, alloy, or non-nickel cermet incorporating one or more of the transition metals Cr, Fe, Cu and Ag, or alloys thereof.

Enhanced Multiferroic Properties of YMnO3 Ceramics Fabricated by Spark Plasma Sintering Along with Low-Temperature Solid-State Reaction

PubMed Central

Wang, Meng; Wang, Ting; Song, Shenhua; Ravi, Muchakayala; Liu, Renchen; Ji, Shishan

2017-01-01

Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid-state reaction method, phase-pure YMnO3 ceramics are fabricated using spark plasma sintering (SPS). X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YMnO3 ceramics can be prepared by SPS at 1000 °C for 5 minutes with annealing at 800 °C for 2 h. The relative density of the sample is as high as 97%, which is much higher than those of the samples sintered by other methods. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods and SPS with ball-milling precursors, and the ferroelectric loops at room temperature can be detected. These findings indicate that the YMnO3 ceramics prepared by the low temperature solid reaction method and SPS possess excellent dielectric lossy ferroelectric properties at room temperature, and magnetic properties at low temperature (10 K), making them suitable for potential multiferroic applications. PMID:28772832

Ceramic planar waveguide laser of non-aqueous tape casting fabricated YAG/Yb:YAG/YAG

PubMed Central

Wang, Chao; Li, Wenxue; Yang, Chao; Bai, Dongbi; Li, Jiang; Ge, Lin; Pan, Yubai; Zeng, Heping

2016-01-01

Ceramic YAG/Yb:YAG/YAG planar waveguide lasers were realized on continuous-wave and mode-locked operations. The straight waveguide, fabricated by non-aqueous tape casting and solid state reactive sintering, enabled highly efficient diode-pumped waveguide continuous-wave laser with the slope efficiency of 66% and average output power of more than 3 W. The influence of the waveguide structure on the wavelength tunability was also experimentally investiccgated with a dispersive prism. Passively mode-locked operation of the ceramic waveguide laser was achieved by using a semiconductor saturable absorber mirror (SESAM), output 2.95 ps pulses with maximum power of 385 mW at the central wavelength of 1030 nm. PMID:27535577

Novel Routes for Sintering of Ultra-high Temperature Ceramics and their Properties

DTIC Science & Technology

2014-10-31

H. Gocmez, Hydrothermal synthesis and properties of Ce1-xGdxO2-δ solid solutions // Solid State Sciences. – 2002. – Vol. 4. – P. 585-590. 19. E...J. Kilner, Ionic conductivity in the CeO2-Gd2O3 system (0.05≤Gd/Ce≤0.4) prepared by oxalate coprecipitation // Solid State Ionics. - 2002. – Vol

Synthesis of nano-scale fast ion conducting cubic Li7La3Zr2O12.

PubMed

Sakamoto, Jeff; Rangasamy, Ezhiylmurugan; Kim, Hyunjoung; Kim, Yunsung; Wolfenstine, Jeff

2013-10-25

A solution-based process was investigated for synthesizing cubic Li7La3Zr2O12 (LLZO), which is known to exhibit the unprecedented combination of fast ionic conductivity, and stability in air and against Li. Sol-gel chemistry was developed to prepare solid metal-oxide networks consisting of 10 nm cross-links that formed the cubic LLZO phase at 600 ° C. Sol-gel LLZO powders were sintered into 96% dense pellets using an induction hot press that applied pressure while heating. After sintering, the average LLZO grain size was 260 nm, which is 13 times smaller compared to LLZO prepared using a solid-state technique. The total ionic conductivity was 0.4 mS cm(-1) at 298 K, which is the same as solid-state synthesized LLZO. Interestingly, despite the same room temperature conductivity, the sol-gel LLZO total activation energy is 0.41 eV, which 1.6 times higher than that observed in solid-state LLZO (0.26 eV). We believe the nano-scale grain boundaries give rise to unique transport phenomena that are more sensitive to temperature when compared to the conventional solid-state LLZO.

Kinetics of dissolution of UO2 in nitric acid solutions: A multiparametric study of the non-catalysed reaction

NASA Astrophysics Data System (ADS)

Cordara, T.; Szenknect, S.; Claparede, L.; Podor, R.; Mesbah, A.; Lavalette, C.; Dacheux, N.

2017-12-01

UO2 pellets were prepared by densification of oxides obtained from the conversion of the oxalate precursor. Then characterized in order to perform a multiparametric study of the dissolution in nitric acid medium. In this frame, for each sample, the densification rate, the grain size and the specific surface area of the prepared pellets were determined prior to the final dissolution experiments. By varying the concentration of the nitric acid solution and temperature, three different and successive steps were identified during the dissolution. Under the less aggressive conditions considered, a first transient step corresponding to the dissolution of the most reactive phases was observed at the solid/solution interface. Then, for all the tested conditions, a steady state step was established during which the normalised dissolution rate was found to be constant. It was followed by a third step characterized by a strong and continuous increase of the normalised dissolution rate. The duration of the steady state, also called "induction period", was found to vary drastically as a function of the HNO3 concentration and temperature. However, independently of the conditions, this steady state step stopped at almost similar dissolved material weight loss and dissolved uranium concentration. During the induction period, no important evolution of the topology of the solid/liquid interface was evidenced authorizing the use of the starting reactive specific surface area to evaluate the normalised dissolution rates thus the chemical durability of the sintered pellets. From the multiparametric study of UO2 dissolution proposed, oxidation of U(IV) to U(VI) by nitrate ions at the solid/liquid interface constitutes the limiting step in the overall dissolution mechanism associated to this induction period.

Gravitational Role in Liquid Phase Sintering

NASA Technical Reports Server (NTRS)

Upadhyaya, Anish; Iacocca, Ronald G.; German, Randall M.

1998-01-01

To comprehensively understand the gravitational effects on the evolution of both the microstructure and the macrostructure during liquid phase sintering, W-Ni-Fe alloys with W content varying from 35 to 98 wt.% were sintered in microgravity. Compositions that slump during ground-based sintering also distort when sintered under microgravity. In ground-based sintering, low solid content alloys distort with a typical elephant-foot profile, while in microgravity, the compacts tend to spheroidize. This study shows that microstructural segregation occurs in both ground-based as well as microgravity sintering. In ground-based experiments, because of the density difference between the solid and the liquid phase, the solid content increases from top to the bottom of the sample. In microgravity, the solid content increases from periphery to the center of the samples. This study also shows that the pores during microgravity sintering act as a stable phase and attain anomalous shapes.

Oxide-Based Composite Electrolytes Using Na3Zr2Si2PO12/Na3PS4 Interfacial Ion Transfer.

PubMed

Noi, Kousuke; Nagata, Yuka; Hakari, Takashi; Suzuki, Kenji; Yubuchi, So; Ito, Yusuke; Sakuda, Atsushi; Hayashi, Akitoshi; Tatsumisago, Masahiro

2018-05-31

All-solid-state sodium batteries using Na 3 Zr 2 Si 2 PO 12 (NASICON) solid electrolytes are promising candidates for safe and low-cost advanced rechargeable battery systems. Although NASICON electrolytes have intrinsically high sodium-ion conductivities, their high sintering temperatures interfere with the immediate development of high-performance batteries. In this work, sintering-free NASICON-based composites with Na 3 PS 4 (NPS) glass ceramics were prepared to combine the high grain-bulk conductivity of NASICON and the interfacial formation ability of NPS. Before the composite preparation, the NASICON/NPS interfacial resistance was investigated by modeling the interface between the NASICON sintered ceramic and the NPS glass thin film. The interfacial ion-transfer resistance was very small above room temperature; the area-specific resistances at 25 and 100 °C were 15.8 and 0.40 Ω cm 2 , respectively. On the basis of this smooth ion transfer, NASICON-rich (70-90 wt %) NASICON-NPS composite powders were prepared by ball-milling fine powders of each component. The composite powders were well-densified by pressing at room temperature. Scanning electron microscopy observation showed highly dispersed sub-micrometer NASICON grains in a dense NPS matrix to form closed interfaces between the oxide and sulfide solid electrolytes. The composite green (unfired) compacts with 70 and 80 wt % NASICON exhibited high total conductivities at 100 °C of 1.1 × 10 -3 and 6.8 × 10 -4 S cm -1 , respectively. An all-solid-state Na 15 Sn 4 /TiS 2 cell was constructed using the 70 wt % NASICON composite electrolyte by the uniaxial pressing of the powder materials, and its discharge properties were evaluated at 100 °C. The cell showed the reversible capacities of about 120 mAh g -1 under the current density of 640 μA cm -2 . The prepared oxide-based composite electrolytes were thus successfully applied in all-solid-state sodium rechargeable batteries without sintering.

Microstructural optimization of solid-state sintered silicon carbide

NASA Astrophysics Data System (ADS)

Vargas-Gonzalez, Lionel R.

Silicon carbide armor, manufactured through solid-state sintering, liquid-phase sintering, and hot-pressing, is being used by the United States Armed Forces for personal and vehicle protection. There is a lack of consensus, however, on which process results in the best-performing ballistic armor. Previous studies have shown that hot-pressed ceramics processed with secondary oxide and/or rare earth oxides, which exhibit high fracture toughness, perform well in handling and under ballistic impact. This high toughness is due to the intergranular nature of the fracture, creating a tortuous path for cracks and facilitating crack deflection and bridging. However, it has also been shown that higher-hardness sintered SiC materials might perform similarly or better to hot-pressed armor, in spite of the large fracture toughness deficit, if the microstructure (density, grain size, purity) of these materials are improved. In this work, the development of theoretically-dense, clean grain boundary, high hardness solid-state sintered silicon carbide (SiC) armor was pursued. Boron carbide and graphite (added as phenolic resin to ensure the carbon is finely dispersed throughout the microstructure) were used as the sintering aids. SiC batches between 0.25--4.00 wt.% carbon were mixed and spray dried. Cylindrical pellets were pressed at 13.7 MPa, cold-isostatically pressed (CIP) at 344 MPa, sintered under varying sintering soaking temperatures and heating rates, and varying post hot-isostatic pressing (HIP) parameters. Carbon additive amounts between 2.0--2.5 wt.% (based on the resin source), a 0.36 wt.% B4C addition, and a 2050°C sintering soak yielded parts with high sintering densities (˜95.5--96.5%) and a fine, equiaxed microstructure (d50 = 2.525 mum). A slow ramp rate (10°C/min) prevented any occurrence of abnormal grain growth. Post-HIPing at 1900°C removed the remaining closed porosity to yield a theoretically-dense part (3.175 g/cm3, according to rule of mixtures). These parts exhibited higher density and finer microstructure than a commercially-available sintered SiC from Saint-Gobain (Hexoloy Enhanced, 3.153 g/cm3 and d50 = 4.837 mum). Due to the optimized microstructure, Verco SiC parts exhibited the highest Vickers (2628.30 +/- 44.13 kg/mm 2) and Knoop (2098.50 +/- 24.8 kg/mm2) hardness values of any SiC ceramic, and values equal to those of the "gold standard" hot-pressed boron carbide (PAD-B4C). While the fracture toughness of hot-pressed SiC materials (˜4.5 MPa m ) are almost double that of Verco SiC (2.4 MPa m ), Verco SiC is a better performing ballistic product, implying that the higher hardness of the theoretically-dense, clean-grain boundary, fine-grained SiC is the defining mechanical property for optimization of ballistic behavior.

Pulsed Laser Deposition of High Temperature Protonic Films

NASA Technical Reports Server (NTRS)

Dynys, Fred W.; Berger, M. H.; Sayir, Ali

2006-01-01

Pulsed laser deposition has been used to fabricate nanostructured BaCe(0.85)Y(0.15)O3- sigma) films. Protonic conduction of fabricated BaCe(0.85)Y(0.15)O(3-sigma) films was compared to sintered BaCe(0.85)Y(0.15)O(3-sigma). Sintered samples and laser targets were prepared by sintering BaCe(0.85)Y(0.15)O(3-sigma) powders derived by solid state synthesis. Films 1 to 8 micron thick were deposited by KrF excimer laser on porous Al2O3 substrates. Thin films were fabricated at deposition temperatures of 700 to 950 C at O2 pressures up to 200 mTorr using laser pulse energies of 0.45 - 0.95 J. Fabricated films were characterized by X-ray diffraction, electron microscopy and electrical impedance spectroscopy. Single phase BaCe(0.85)Y(0.15)O(3-sigma) films with a columnar growth morphology are observed with preferred crystal growth along the [100] or [001] direction. Results indicate [100] growth dependence upon laser pulse energy. Electrical conductivity of bulk samples produced by solid state sintering and thin film samples were measured over a temperature range of 100 C to 900 C. Electrical conduction behavior was dependent upon film deposition temperature. Maximum conductivity occurs at deposition temperature of 900 oC; the electrical conductivity exceeds the sintered specimen. All other deposited films exhibit a lower electrical conductivity than the sintered specimen. Activation energy for electrical conduction showed dependence upon deposition temperature, it varied

Molten salt synthesis of nanocrystalline phase of high dielectric constant material CaCu3Ti4O12.

PubMed

Prakash, B Shri; Varma, K B R

2008-11-01

Nanocrystalline powders of giant dielectric constant material, CaCu3Ti4O12 (CCTO), have been prepared successfully by the molten salt synthesis (MSS) using KCl at 750 degrees C/10 h, which is significantly lower than the calcination temperature (approximately 1000 degrees C) that is employed to obtain phase pure CCTO in the conventional solid-state reaction route. The water washed molten salt synthesized powder, characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) confirmed to be a phase pure CCTO associated with approximately 150 nm sized crystallites of nearly spherical shape. The decrease in the formation temperature/duration of CCTO in MSS method was attributed to an increase in the diffusion rate or a decrease in the diffusion length of reacting ions in the molten salt medium. As a consequence of liquid phase sintering, pellets of as-synthesized KCl containing CCTO powder exhibited higher sinterability and grain size than that of KCl free CCTO samples prepared by both MSS method and conventional solid-state reaction route. The grain size and the dielectric constant of KCl containing CCTO ceramics increased with increasing sintering temperature (900 degrees C-1050 degrees C). Indeed the dielectric constants of these ceramics were higher than that of KCl free CCTO samples prepared by both MSS method and those obtained via the solid-state reaction route and sintered at the same temperature. Internal barrier layer capacitance (IBLC) model was invoked to correlate the observed dielectric constant with the grain size in these samples.

Structures and fabrication techniques for solid state electrochemical devices

DOEpatents

Visco, Steven J.; Jacobson, Craig P.; DeJonghe, Lutgard C.

2012-10-09

Porous substrates and associated structures for solid-state electrochemical devices, such as solid-oxide fuel cells (SOFCs), are low-cost, mechanically strong and highly electronically conductive. Some preferred structures have a thin layer of an electrocatalytically active material (e.g., Ni--YSZ) coating a porous high-strength alloy support (e.g., SS-430) to form a porous SOFC fuel electrode. Electrode/electrolyte structures can be formed by co-firing or constrained sintering processes.

Structures and fabrication techniques for solid state electrochemical devices

DOEpatents

Visco, Steven J.; Jacobson, Craig P.; DeJonghe, Lutgard C.

2008-04-01

Porous substrates and associated structures for solid-state electrochemical devices, such as solid-oxide fuel cells (SOFCs), are low-cost, mechanically strong and highly electronically conductive. Some preferred structures have a thin layer of an electrocatalytically active material (e.g., Ni--YSZ) coating a porous high-strength alloy support (e.g., SS-430) to form a porous SOFC fuel electrode. Electrode/electrolyte structures can be formed by co-firing or constrained sintering processes.

Effect of two-stage sintering on dielectric properties of BaTi0.9Zr0.1O3 ceramics

NASA Astrophysics Data System (ADS)

Rani, Rekha; Rani, Renu; Kumar, Parveen; Juneja, J. K.; Raina, K. K.; Prakash, Chandra

2011-09-01

The effect of two-stage sintering on the dielectric properties of BaTi0.9Zr0.1O3 ceramics prepared by solid state route was investigated and is presented here. It has been found that under suitable two-stage sintering conditions, dense BaTi0.9Zr0.1O3 ceramics with improved electrical properties can be synthesized. The density was found to have a value of 5.49 g cc-1 for normally sintered samples, whereas in the case of the two-stage sintered sample it was 5.85 g cc-1. Dielectric measurements were done as a function of frequency and temperature. A small decrease in the Curie temperature was observed with modification in dielectric loss for two-stage sintered ceramic samples.

Preparation and electrochemical properties of Zr-site substituted Li7La3(Zr2-xMx)O12 (M = Ta, Nb) solid electrolytes

NASA Astrophysics Data System (ADS)

Huang, Mian; Shoji, Mao; Shen, Yang; Nan, Ce-Wen; Munakata, Hirokazu; Kanamura, Kiyoshi

2014-09-01

Li7La3Zr2O12 (LLZ) solid electrolytes with Zr site partially substituted by Ta and Nb elements were prepared via the conventional solid-state reaction. All the compositions could lead to the cubic garnet-type structure after sintering at 1150 °C. The use of γ-Al2O3 as a sintering aid in the preparation of doped LLZ was studied. It was shown that Al could help to improve the micro-structure for Nb doping, but not necessary for Ta doping. The Ta and Nb doping enhanced the ionic conductivity at 25 °C to 4.09 × 10-4 S cm-1 and 4.50 × 10-4 S cm-1, respectively. A conductivity as high as 1.23 × 10-3 S cm-1 was obtained when measured at 50 °C in air for the Nb-doped LLZ. All-solid-state batteries with LLZTa and LLZNb solid electrolytes were assembled and tested. The cyclic voltammetry (CV) measurement indicated the successful working of the batteries.

A comparative study on NbOx films reactively sputtered from sintered and cold gas sprayed targets

NASA Astrophysics Data System (ADS)

Lorenz, Roland; O'Sullivan, Michael; Fian, Alexander; Sprenger, Dietmar; Lang, Bernhard; Mitterer, Christian

2018-04-01

The aim of this work is to evaluate novel cold gas sprayed Nb targets in a reactive sputter deposition process of thin films with respect to the widely used sintered Nb targets. With the exception of a higher target discharge voltage of ∼100 V for the cold gas sprayed targets and the thus higher film growth rate compared to sintered targets, NbOx films with comparable microstructure and properties were obtained for both target variants. The amorphous films with thicknesses between 2.9 and 4.9 μm present an optical shift from dark and non-transparent towards transparent properties, as the oxygen partial pressure increases. X-ray photoelectron spectroscopy confirms the occurrence of the Nb5+ oxidation state for the highest oxygen partial pressure, while Nb4+ is additionally present at lower oxygen partial pressure settings. With a maximal transparency of ∼80% and a refractive index of ∼2.5, the transparent films show characteristics similar to Nb2O5.

Process for making dense thin films

DOEpatents

Jacobson, Craig P.; Visco, Steven J.; DeJonghe, Lutgard C.

2005-07-26

Provided are low-cost, mechanically strong, highly electronically conductive porous substrates and associated structures for solid-state electrochemical devices, techniques for forming these structures, and devices incorporating the structures. The invention provides solid state electrochemical device substrates of novel composition and techniques for forming thin electrode/membrane/electrolyte coatings on the novel or more conventional substrates. In particular, in one embodiment the invention provides techniques for firing of device substrate to form densified electrolyte/membrane films 5 to 20 microns thick. In another embodiment, densified electrolyte/membrane films 5 to 20 microns thick may be formed on a pre-sintered substrate by a constrained sintering process. In some cases, the substrate may be a porous metal, alloy, or non-nickel cermet incorporating one or more of the transition metals Cr, Fe, Cu and Ag, or alloys thereof.

Density Optimization of Lithium Lanthanum Titanate Ceramics for Lightweight Lithium-Air Batteries

DTIC Science & Technology

2014-11-01

Thangadurai V, Weppner W. Lithium lanthanum titanates: a review. Chemistry of Materials. 2003;15:3974–3990. 4. Knauth P. Inorganic solid Li ion conductors...an overview. Solid State Ionics. 2009;180:911–916. 5. Ban CW, Choi GM. The effect of sintering on the grain boundary conductivity of lithium ...lanthanum titanates. Solid State Ionics. 2001;140:285–292. 6. Inada R, Kimura K, Kusakabe K, Tojo T, Sakurai Y. Synthesis and lithium -ion conductivity

Effects of Molar Ratios and Sintering Times on Crystal Structures and Surface Morphology of Nd1+xFeO3 Oxide Alloy Prepared by using Solid Reaction Method

NASA Astrophysics Data System (ADS)

Sujiono, E. H.; Agus, J.; Samnur, S.; Triyana, K.

2018-05-01

The effects of molar ratios and sintering times on crystal structures and surface morphology on NdFeO3 oxide alloy have been studied. NdFeO3 oxide alloy formed by chemical preparation with solid reaction method using raw oxide Fe2O3 (99.9 %) and Nd2O3 (99.9 %) powders. In this article we reported the effects of molar ratios x = (–0.1, –0.2 and –0.3) and sintering times for 15 h and 20 h on crystal structures and surface morphology of Nd1+xFeO3 synthesized by solid-state reaction method. The results indicate that variation of molar ratio and sintering time has influenced the FWHM, crystalline size and grain size. The Nd1+xFeO3 have a major phase is NdFeO3, and other minor phases are Fe2O3, Nd2O3 and Nd(OH)3. The dominant intensity of hkl (121) with a value in FWHM, crystallite size, and grain size an indication the results will be applied as a gas sensor material as the focus of the further study.

Sintered Intermetallic Reinforced 434L Ferritic Stainless Steel Composites

NASA Astrophysics Data System (ADS)

Upadhyaya, A.; Balaji, S.

2009-03-01

The present study examines the effect of aluminide (Ni3Al, Fe3Al) additions on the sintering behavior of ferritic 434L stainless steels during solid-state sintering (SSS) and supersolidus liquid-phase sintering (SLPS). 434L stainless steel matrix composites containing 5 and 10 wt pct of each aluminide were consolidated at 1200 °C (SSS) and 1400 °C (SLPS). The effects of sintering and aluminide additions on the densification, microstructural evolution, mechanical, tribological, and corrosion behavior of sintered ferritic (434L) stainless steels were investigated. The performances of the 434L-aluminide composites were compared with the straight 434L stainless steels processed at similar conditions. Supersolidus sintering resulted in significant improvement in densification, mechanical, wear, and corrosion resistance in both straight 434L and 434L-aluminide composites. Fe3Al additions to 434L stainless steels result in improved wear resistance without significant degradation of corrosion resistance in 3.56 wt pct NaCl solution.

Rapid Prototyping: State of the Art

DTIC Science & Technology

2003-10-23

Rapid Prototyping SCS Solid Creation System SLM Selective Laser Melting SLP Solid Laser diode Plotter SLS Selective Laser Sintering SOAR State of the...121,000, respectively. SLP stands for Sold Laser Diode Plotter. The machines are relatively slow and parts are small, so, to date, the products have been...Gigerenzer, H., “Directed Laser Welding of Metal Matrix Composite Structures for Space Based Applications,“ Triton Systems Inc., Chelmsford, MA., 1

Method Using Water-Based Solvent to Prepare Li7La3Zr2O12 Solid Electrolytes.

PubMed

Huang, Xiao; Lu, Yang; Jin, Jun; Gu, Sui; Xiu, Tongping; Song, Zhen; Badding, Michael E; Wen, Zhaoyin

2018-05-09

Li-garnet Li 7 La 3 Zr 2 O 12 (LLZO) is a promising candidate of solid electrolytes for high-safety solid-state Li + ion batteries. However, because of its high reactivity to water, the preparation of LLZO powders and ceramics is not easy for large-scale amounts. Herein, a method applying water-based solvent is proposed to demonstrate a possible solution. Ta-doped LLZO, that is, Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 (LLZTO), and its LLZTO/MgO composite ceramics are made by attrition milling, followed by a spray-drying process using water-based slurries. The impacts of parameters of the method on the structure and properties of green and sintered pellets are studied. A relative density of ∼95%, a Li-ion conductivity of ∼3.5 × 10 -4 S/cm, and uniform grain size LLZTO/MgO garnet composite ceramics are obtained with an attrition-milled LLZTO/MgO slurry that contains 40 wt % solids and 2 wt % polyvinyl alcohol binder. Li-sulfur batteries based on these ceramics are fabricated and work under 25 °C for 20 cycles with a Coulombic efficiency of 100%. This research demonstrates a promising mass production method for the preparation of Li-garnet ceramics.

Innovative processing of dense LSGM electrolytes for IT-SOFC's

NASA Astrophysics Data System (ADS)

Rambabu, B.; Ghosh, Samrat; Zhao, Weichang; Jena, Hrudananda

This paper reports for the first time the attempted synthesis of SrO- and MgO-doped LaGaO 3 (La 1- xSr xGa 1- yMg yO 3-0.5(x+ y), LSGM) perovskite by an aqueous 'regenerative' solution route. This novel technique enabled recycling of the undesired product and subsequently yielded product with much better phase purity and density than that obtained from the solid-state route. La 0.8Sr 0.2Ga 0.85Mg 0.15O 2.825 (LSGM-2015) and LaGaO 3 were prepared using both the regenerative sol-gel (RSG) and conventional solid-state route at 1400 °C. Series of La 0.8Sr 0.2Ga 0.83Mg 0.17O 2.815 (LSGM-2017) pellets were also prepared by the RSG method at different sintering temperature (1200-1500 °C) and time. The effect of conventional and microwave sintering of samples obtained from both solid-state and regenerative route was also investigated. Microwave heating was carried out using SiC as a microwave susceptor. The LSGM pellets prepared by using different synthetic methods were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and pellet density was determined by pycnometry. The LSGM-2015 prepared by RSG route exhibited conductivity σ t = 0.066 and 0.029 S cm -1 at 800 and 700 °C, respectively, and activation energy of the bulk, grain-boundary, and total are E b = 0.97 eV, E gb = 1.03 eV and E t = 1.01 eV, respectively. The sintering temperature severely affected the grain size (<0.1-10 μm) and also the grain-boundary resistance (3-175 kΩ). The unique aspect of this RSG technique is that the final product can be recycled which makes the process cost effective and time saving compared to the solid-state ceramic technique and this technique would allow optimization of processing parameters in a cost effective and time saving manner for obtaining well sintered LSGM as an electrolyte for IT-SOFC's.

Effect of Starch on Sintering Behavior for Fabricating Porous Cordierite Ceramic

NASA Astrophysics Data System (ADS)

Li, Ye; Cao, Wei; Gong, Lunlun; Zhang, Ruifang; Cheng, Xudong

2016-10-01

Porous cordierite ceramics were prepared with starch as pore-forming agent by solid-state method. The green bodies were sintered at 1,100-1,400 °C for 2 h. The characterization was focused on thermal analysis, phase evolution, sintering behavior, porosity and micro-structural changes. The results show that cordierite becomes the main crystallization phase at 1,200 °C. The shrinkage behavior shows the most obvious dependence on the sintering temperature and starch content, and it can be divided into three stages. Moreover, the open porosity increases with the increase of starch content, but the pore-forming effectivity decreases. Nevertheless, compared with the open porosity curves, the bulk density curves are more in line with the linear rule. The microphotographs show the densification process with the sintering temperature and the variation of pore connectivity with the starch content.

Low temperature processed MnCo2O4 and MnCo1.8Fe0.2O4 as effective protective coatings for solid oxide fuel cell interconnects at 750 °C

NASA Astrophysics Data System (ADS)

Molin, S.; Jasinski, P.; Mikkelsen, L.; Zhang, W.; Chen, M.; Hendriksen, P. V.

2016-12-01

In this study two materials, MnCo2O4 and MnCo1.8Fe0.2O4 are studied as potential protective coatings for Solid Oxide Fuel Cell interconnects working at 750 °C. First powder fabrication by a modified Pechini method is described followed by a description of the coating procedure. The protective action of the coating applied on Crofer 22 APU is evaluated by following the area specific resistance (ASR) of the scale/coating for 5500 h including several thermal cycles. The coating is prepared by brush painting and has a porous structure after deposition. Post mortem microstructural characterization performed on the coated samples shows good protection against chromium diffusion from the chromia scale ensured by a formation of a dense reaction layer. This study shows, that even without high temperature sintering and/or reactive sintering it is possible to fabricate protective coatings based on MnCo spinels.

Reactive sintering process of ferromagnetic MnBi under high magnetic fields

NASA Astrophysics Data System (ADS)

Mitsui, Yoshifuru; Umetsu, Rie Y.; Takahashi, Kohki; Koyama, Keiichi

2018-05-01

The magnetic field effect on the reactive sintering process of MnBi was investigated. Magnetic-field-induced enhancement of the reaction was found to be exhibited at the initial stages. The coercivity field decreased with an increase in the in-field annealing time. The kinetics of the reaction were in good agreement with the diffusion-controlled reaction model. It is suggested that the decrease in activation energy at the initial stages of reaction increased the amount of formed MnBi phases, resulting in enhancement of the reaction Mn + Bi to MnBi phase by in-field reactive sintering.

Method of electrode fabrication for solid oxide electrochemical cells

DOEpatents

Jensen, R.R.

1990-11-20

A process for fabricating cermet electrodes for solid oxide electrochemical cells by sintering is disclosed. First, a porous metal electrode is fabricated on a solid oxide cell, such as a fuel cell by, for example, sintering, and is then infiltrated with a high volume fraction stabilized zirconia suspension. A second sintering step is used to sinter the infiltrated zirconia to a high density in order to more securely attach the electrode to the solid oxide electrolyte of the cell. High performance fuel electrodes can be obtained with this process. Further electrode performance enhancement may be achieved if stabilized zirconia doped with cerium oxide, chromium oxide, titanium oxide, and/or praseodymium oxide for electronic conduction is used. 5 figs.

Method of electrode fabrication for solid oxide electrochemical cells

DOEpatents

Jensen, Russell R.

1990-01-01

A process for fabricating cermet electrodes for solid oxide electrochemical cells by sintering is disclosed. First, a porous metal electrode is fabricated on a solid oxide cell, such as a fuel cell by, for example, sintering, and is then infiltrated with a high volume fraction stabilized zirconia suspension. A second sintering step is used to sinter the infiltrated zirconia to a high density in order to more securely attach the electrode to the solid oxide electrolyte of the cell. High performance fuel electrodes can be obtained with this process. Further electrode performance enhancement may be achieved if stabilized zirconia doped with cerium oxide, chromium oxide, titanium oxide, and/or praseodymium oxide for electronic conduction is used.

Sintering Behavior of Spark Plasma Sintered SiC with Si-SiC Composite Nanoparticles Prepared by Thermal DC Plasma Process

NASA Astrophysics Data System (ADS)

Yu, Yeon-Tae; Naik, Gautam Kumar; Lim, Young-Bin; Yoon, Jeong-Mo

2017-11-01

The Si-coated SiC (Si-SiC) composite nanoparticle was prepared by non-transferred arc thermal plasma processing of solid-state synthesized SiC powder and was used as a sintering additive for SiC ceramic formation. Sintered SiC pellet was prepared by spark plasma sintering (SPS) process, and the effect of nano-sized Si-SiC composite particles on the sintering behavior of micron-sized SiC powder was investigated. The mixing ratio of Si-SiC composite nanoparticle to micron-sized SiC was optimized to 10 wt%. Vicker's hardness and relative density was increased with increasing sintering temperature and holding time. The relative density and Vicker's hardness was further increased by reaction bonding using additional activated carbon to the mixture of micron-sized SiC and nano-sized Si-SiC. The maximum relative density (97.1%) and Vicker's hardness (31.4 GPa) were recorded at 1800 °C sintering temperature for 1 min holding time, when 0.2 wt% additional activated carbon was added to the mixture of SiC/Si-SiC.

Spark Plasma Sintering As a Solid-State Recycling Technique: The Case of Aluminum Alloy Scrap Consolidation

PubMed Central

Paraskevas, Dimos; Vanmeensel, Kim; Vleugels, Jef; Dewulf, Wim; Deng, Yelin; Duflou, Joost R.

2014-01-01

Recently, “meltless” recycling techniques have been presented for the light metals category, targeting both energy and material savings by bypassing the final recycling step of remelting. In this context, the use of spark plasma sintering (SPS) is proposed in this paper as a novel solid-state recycling technique. The objective is two-fold: (I) to prove the technical feasibility of this approach; and (II) to characterize the recycled samples. Aluminum (Al) alloy scrap was selected to demonstrate the SPS effectiveness in producing fully-dense samples. For this purpose, Al alloy scrap in the form of machining chips was cold pre-compacted and sintered bellow the solidus temperature at 490 °C, under elevated pressure of 200 MPa. The dynamic scrap compaction, combined with electric current-based joule heating, achieved partial fracture of the stable surface oxides, desorption of the entrapped gases and activated the metallic surfaces, resulting in efficient solid-state chip welding eliminating residual porosity. The microhardness, the texture, the mechanical properties, the microstructure and the density of the recycled specimens have been investigated. An X-ray computed tomography (CT) analysis confirmed the density measurements, revealing a void-less bulk material with homogeneously distributed intermetallic compounds and oxides. The oxide content of the chips incorporated within the recycled material slightly increases its elastic properties. Finally, a thermal distribution simulation of the process in different segments illustrates the improved energy efficiency of this approach. PMID:28788153

Spark Plasma Sintering As a Solid-State Recycling Technique: The Case of Aluminum Alloy Scrap Consolidation.

PubMed

Paraskevas, Dimos; Vanmeensel, Kim; Vleugels, Jef; Dewulf, Wim; Deng, Yelin; Duflou, Joost R

2014-08-06

Recently, "meltless" recycling techniques have been presented for the light metals category, targeting both energy and material savings by bypassing the final recycling step of remelting. In this context, the use of spark plasma sintering (SPS) is proposed in this paper as a novel solid-state recycling technique. The objective is two-fold: (I) to prove the technical feasibility of this approach; and (II) to characterize the recycled samples. Aluminum (Al) alloy scrap was selected to demonstrate the SPS effectiveness in producing fully-dense samples. For this purpose, Al alloy scrap in the form of machining chips was cold pre-compacted and sintered bellow the solidus temperature at 490 °C, under elevated pressure of 200 MPa. The dynamic scrap compaction, combined with electric current-based joule heating, achieved partial fracture of the stable surface oxides, desorption of the entrapped gases and activated the metallic surfaces, resulting in efficient solid-state chip welding eliminating residual porosity. The microhardness, the texture, the mechanical properties, the microstructure and the density of the recycled specimens have been investigated. An X-ray computed tomography (CT) analysis confirmed the density measurements, revealing a void-less bulk material with homogeneously distributed intermetallic compounds and oxides. The oxide content of the chips incorporated within the recycled material slightly increases its elastic properties. Finally, a thermal distribution simulation of the process in different segments illustrates the improved energy efficiency of this approach.

A microstructure-based model for shape distortion during liquid phase sintering

NASA Astrophysics Data System (ADS)

Upadhyaya, Anish

Tight dimensional control is a major concern in consolidation of alloys via liquid phase sintering. This research demonstrates the role of microstructure in controlling the bulk dimensional changes that occur during liquid phase sintering. The dimensional changes were measured using a coordinate measuring machine and also on a real-time basis using in situ video imaging. To quantify compact distortion, a distortion parameter is formulated which takes into consideration the compact distortion in radial as well as axial directions. The microstructural attributes considered in this study are as follows: solid content, dihedral angle, grain size, grain contiguity and connectivity, and solid-solubility. Sintering experiments were conducted with the W-Ni-Cu, W-Ni-Fe, Mo-Ni-Cu, and Fe-Cu systems. The alloy systems and the compositions were selected to give a range of microstructures during liquid phase sintering. The results show that distortion correlates with the measured microstructural attributes. Systems containing a high solid content, high grain coordination number and contiguity, and large dihedral angle have more structural rigidity. The results show that a minimum two-dimensional grain coordination number of 3.0 is necessary for shape preservation. Based on the experimental observations, a model is derived that relates the critical solid content required for maintaining structural rigidity to the dihedral angle. The critical solid content decreases with an increasing dihedral angle. Consequently, W-Cu alloys, which have a dihedral angle of about 95sp°, can be consolidated without gross distortion with as little as 20 vol.% solid. To comprehensively understand the gravitational effects in the evolution of both the microstructure and the macrostructure during liquid phase sintering, W-Ni-Fe alloys with W content varying from 78 to 93 wt.% were sintered in microgravity. Compositions that slump during ground-based sintering also distort when sintered under microgravity. In ground-based sintering, low solid content alloys distort with a typical elephant-foot profile, while in microgravity, the compacts tend to spheroidize. This study shows that microstructural segregation occurs in both ground-based as well as microgravity sintering. In ground-based experiments, because of the density difference between the solid and the liquid phase, the solid content increases from top to the bottom of the sample. In microgravity, the solid content increases from periphery to the center of the samples. A model is derived to show that grain agglomeration and segregation are energetically favored events and will therefore be inherent to the system, even in the absence of gravity. Real time distortion measurement in alloys having appreciable solid-solubility in the liquid phase, such as W-Ni-Fe and Fe-Cu, show that the bulk of distortion occur within the first 5 min of melt formation. Distortion in such systems can be minimized by presaturating the matrix with the solid phase.

Influence of microstructure and AlPO4 secondary-phase on the ionic conductivity of Li1.3Al0.3Ti1.7(PO4)3 solid-state electrolyte

NASA Astrophysics Data System (ADS)

Yu, Shicheng; Mertens, Andreas; Gao, Xin; Gunduz, Deniz Cihan; Schierholz, Roland; Benning, Svenja; Hausen, Florian; Mertens, Josef; Kungl, Hans; Tempel, Hermann; Eichel, Rüdiger-A.

2016-09-01

A ceramic solid-state electrolyte of lithium aluminum titanium phosphate with the composition of Li1.3Al0.3Ti1.7(PO4)3 (LATP) was synthesized by a sol-gel method using a pre-dissolved Ti-source. The annealed LATP powders were subsequently processed in a binder-free dry forming method and sintered under air for the pellet preparation. Phase purity, density, microstructure as well as ionic conductivity of the specimen were characterized. The highest density (2.77gṡcm-3) with an ionic conductivity of 1.88×10-4 Sṡcm-1 (at 30∘C) was reached at a sintering temperature of 1100∘C. Conductivity of LATP ceramic electrolyte is believed to be significantly affected by both, the AlPO4 secondary phase content and the ceramic electrolyte microstructure. It has been found that with increasing sintering temperature, the secondary-phase content of AlPO4 increased. For sintering temperatures above 1000∘C, the secondary phase has only a minor impact, and the ionic conductivity is predominantly determined by the microstructure of the pellet, i.e. the correlation between density, porosity and particle size. In that respect, it has been demonstrated, that the conductivity increases with increasing particle size in this temperature range and density.

Electrical conductivity and molten salt corrosion behavior of spinel nickel ferrite

NASA Astrophysics Data System (ADS)

Liu, Baogang; Zhang, Lei; Zhou, Kechao; Li, Zhiyou; Wang, Hao

2011-08-01

Nickel ferrite was prepared by solid-state reaction at 1300 °C as inert anode for aluminum electrolysis. DC conductivities and molten salt corrosion behavior of the samples were investigated in detail regarding the effects of different sintering atmospheres. X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray analysis were used to analyse the phase compositions and microstructures. The DC conductivities of the samples sintered in nitrogen showed a drastic increase compared to those sintered in air, and at 960 °C they increased from 1.94 S/cm to 22.65 S/cm. The samples sintered in nitrogen showed much better corrosion resistance than those sintered in air, attributing to the formation of the dense protective layers in the anode surfaces during the electrolysis at 960 °C. The conductive mechanism and molten salt corrosion behavior were also discussed.

Ash chemistry and sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skrifvars, B.J.; Backman, R.; Hupa, M.

1996-10-01

The chemistry of a fuel ash is important to consider when ash behavior in combustion or gasification is studied. Four different types of thermal behavior based bed agglomeration and deposit foliation mechanisms have been proposed to be important, (1) partial melting, (2) viscous flow, (3) chemical reaction sintering, and (4) solid state sintering. In this paper we present data from a broader study in which we have quantified the four mechanisms more in detail. The ashes from 10 different types of fuels have been tested for their sintering tendency by a compression strength sintering test. The ashes were also subjectmore » to quantitative wet chemical analyses and combined differential thermal, thermogravimetric (DT/TG) analyses. These thermal behavior predictions were compared with multi-component multi-phase thermodynamic phase equilibrium calculations and further with full scale combustion experience. The results and their relevance to full scale conversion systems are discussed in the paper.« less

Fabrication and thermoelectric properties of n-type (Sr0.9Gd0.1)TiO3 oxides

NASA Astrophysics Data System (ADS)

Li, Liangliang; Qin, Xiaoying; Liu, Yongfei; Xin, Hongxing; Zhang, Jian; Li, Di; Song, Chunjun; Guo, Guanglei; Dou, Yunchen; Zou, Tianhua

2014-02-01

The n-type oxides (Sr0.9Gd0.1)TiO3 (SGTO) have been successfully prepared via a sol-gel process followed by solid-state sintering. The effects of sintering temperature on the thermoelectric (TE) properties of the SGTO samples have been investigated. The Seebeck coefficient showed no obvious difference, while the electrical conductivity increased with increasing sintering temperature, benefiting from an enhancement of densification. The maximum power factor (PF) value, 20.5μW/K2cm at 370 K in the metallic region, was observed for the sample sintered at 1748 K. As a result, the peak figure of merit (ZT) values for the samples sintered at higher than 1673 K were in the range of 0.28-0.30. All the results indicate that such synthetic method provides a simple and effective way to prepare TE oxides.

The mechanism of vapor phase hydration of calcium oxide: implications for CO2 capture.

PubMed

Kudłacz, Krzysztof; Rodriguez-Navarro, Carlos

2014-10-21

Lime-based sorbents are used for fuel- and flue-gas capture, thereby representing an economic and effective way to reduce CO2 emissions. Their use involves cyclic carbonation/calcination which results in a significant conversion reduction with increasing number of cycles. To reactivate spent CaO, vapor phase hydration is typically performed. However, little is known about the ultimate mechanism of such a hydration process. Here, we show that the vapor phase hydration of CaO formed after calcination of calcite (CaCO3) single crystals is a pseudomorphic, topotactic process, which progresses via an intermediate disordered phase prior to the final formation of oriented Ca(OH)2 nanocrystals. The strong structural control during this solid-state phase transition implies that the microstructural features of the CaO parent phase predetermine the final structural and physicochemical (reactivity and attrition) features of the product hydroxide. The higher molar volume of the product can create an impervious shell around unreacted CaO, thereby limiting the efficiency of the reactivation process. However, in the case of compact, sintered CaO structures, volume expansion cannot be accommodated in the reduced pore volume, and stress generation leads to pervasive cracking. This favors complete hydration but also detrimental attrition. Implications of these results in carbon capture and storage (CCS) are discussed.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, I-Wei

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 densemore » 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.« less

Influence of the sintering temperature on the electrical properties of Ce-doped WO3 ceramics prepared from nano-powders

NASA Astrophysics Data System (ADS)

Dong, Liang; Chen, Han-Jun; Wang, Yu; Li, De-Zhu; Li, Tong-Ye; Zhao, Yong

2007-04-01

Using a nm-level powder fabricated by a wet chemical method as precursor, the CeO2-doped WO3 ceramics were prepared by the conventional solid state reaction at sintering temperatures from 600 to 1100 °C. The x-ray diffraction analysis reveals the coexistence of different WO3 phases in the samples sintered at temperatures below 900 °C, whereas a single phase appears in the samples sintered above 1000 °C. No new Ce-W compound appears. As the sintering temperature increases, the electrical properties of the samples display an interesting transformation from linear to nonlinear behaviour. The measurements of scanning electron microscope, complex impedance and electrical stability indicate that a lot of grain boundary regions in the samples sintered at low temperatures strongly influences the electrical transportation. Therefore, the electrical nonlinearity is due to a basic process controlled by the back-to-back Schottky barriers at grain boundaries with suitable thickness as well as the coexistence of phases.

Microstructural development of cobalt ferrite ceramics and its influence on magnetic properties

NASA Astrophysics Data System (ADS)

Kim, Gi-Yeop; Jeon, Jae-Ho; Kim, Myong-Ho; Suvorov, Danilo; Choi, Si-Young

2013-11-01

The microstructural evolution and its influence on magnetic properties in cobalt ferrite were investigated. The cobalt ferrite powders were prepared via a solid-state reaction route and then sintered at 1200 °C for 1, 2, and 16 h in air. The microstructures from sintered samples represented a bimodal distribution of grain size, which is associated with abnormal grain growth behavior. And thus, with increasing sintering time, the number and size of abnormal grains accordingly increased but the matrix grains were frozen with stagnant grain growth. In the sample sintered for 16 h, all of the matrix grains were consumed and the abnormal grains consequently impinged on each other. With the appearance of abnormal grains, the magnetic coercivity significantly decreased from 586.3 Oe (1 h sintered sample) to 168.3 Oe (16 h sintered sample). This is due to the magnetization in abnormal grains being easily flipped. In order to achieve high magnetic coercivity of cobalt ferrite, it is thus imperative to fabricate the fine and homogeneous microstructure.

Correlation between structural, electrical and magnetic properties of GdMnO3 bulk ceramics

NASA Astrophysics Data System (ADS)

Samantaray, S.; Mishra, D. K.; Pradhan, S. K.; Mishra, P.; Sekhar, B. R.; Behera, Debdhyan; Rout, P. P.; Das, S. K.; Sahu, D. R.; Roul, B. K.

2013-08-01

This paper reports the effect of sintering temperature on ferroelectric properties of GdMnO3 (GMO) bulk ceramics at room temperature prepared by the conventional solid state reaction route following slow step sintering schedule. Ferroelectric hysteresis loop as well as sharp dielectric anomaly in pure (99.999%) GMO sintered ceramics has been clearly observed. Samples sintered at 1350 °C become orthorhombic with Pbnm space group and showed frequency independent sharp dielectric anomalies at 373 K and a square type of novel ferroelectric hysteresis loop was observed at room temperature. Interestingly, dielectric anomalies and ferroelectric behavior were observed to be dependent upon sintering temperature of GdMnO3. Room temperature dielectric constant (ɛr) value at different frequencies is observed to be abnormally high. The magnetic field and temperature dependent magnetization show antiferromagnetic behavior at 40 K for both 1350 °C and 1700 °C sintered GMO. Present findings showed the possibility of application of GdMnO3 at room temperature as multifunctional materials.

Improved Properties of Pb Based BLZT Ferroelectric Ceramics

NASA Astrophysics Data System (ADS)

Kumar, Parveen; Singh, Sangeeta; Juneja, J. K.; Raina, K. K.; Prakash, Chandra

2011-11-01

Present report is concerning with investigation of effect of different sintering profiles on Pb based BLZT ceramics. The material powder of selected composition (Ba0.795La0.005Pb0.20Ti0.90Zr0.10O3) was prepared by solid state reaction route and then powder was compacted in the form of circular discs. The discs were then sintered at different temperatures (1325 °C for 4h, 1325 °C for 15min+1200 °C for 4h). Improved dielectric and ferroelectric properties were observed for samples sintered at 1200 °C. Shifting in Tc to higher temperature could be related to enhanced tetragonality, which was further confirmed by X-ray diffraction analysis. All these improvements evidences that there is less Pb loss in case of modified sintering profile.

A Fully Coupled Simulation and Optimization Scheme for the Design of 3D Powder Injection Molding Processes

NASA Astrophysics Data System (ADS)

Ayad, G.; Song, J.; Barriere, T.; Liu, B.; Gelin, J. C.

2007-05-01

The paper is concerned with optimization and parametric identification of Powder Injection Molding process that consists first in injection of powder mixture with polymer binder and then to the sintering of the resulting powders parts by solid state diffusion. In the first part, one describes an original methodology to optimize the injection stage based on the combination of Design Of Experiments and an adaptive Response Surface Modeling. Then the second part of the paper describes the identification strategy that one proposes for the sintering stage, using the identification of sintering parameters from dilatometer curves followed by the optimization of the sintering process. The proposed approaches are applied to the optimization for manufacturing of a ceramic femoral implant. One demonstrates that the proposed approach give satisfactory results.

A new ferroelectric solid solution system of LaCrO 3-BiCrO 3

NASA Astrophysics Data System (ADS)

Chen, J. I. L.; Kumar, M. Mahesh; Ye, Z.-G.

2004-04-01

A new perovskite solid solution system of (1- x)LaCrO 3- xBiCrO 3 has been prepared by conventional solid-state reaction and sintering processes at 1200°C in a sealed Pt tube or a Bi 2O 3-rich environment. A clean orthorhombic phase of LaCrO 3-type structure is established at room temperature for compositions with 0⩽ x⩽0.35. The relative density, lattice parameters, sintering mechanism, microstructure and ferroelectricity of the compounds are investigated. The substitution of Bi 2O 3 for La 2O 3 is found to decrease the unit cell volume and increase the grain size of the ceramics. The relative density of the ceramics sintered at 1200°C is significantly improved from 40% for LaCrO 3 up to about 90% for La 0.65Bi 0.35CrO 3 through a liquid phase sintering mechanism. The ferroelectricity is revealed in La 1- xBi xCrO 3 with 0.1⩽ x⩽0.35 by dielectric hysteresis loops displayed at 77 K. The remnant polarization is found to increase with increasing Bi 3+ content. The origin of the ferroelectricity is attributed to the structural distortion induced by the stereochemically active Bi 3+ ion on the A site.

Synthesis cathode material LiNi0.80Co0.15Al0.05O2 with two step solid-state method under air stream

NASA Astrophysics Data System (ADS)

Xia, Shubiao; Zhang, Yingjie; Dong, Peng; Zhang, Yannan

2014-01-01

A facile generic strategy of solid-state reaction under air atmosphere is employed to prepare LiNi0.8Co0.15Al0.05O2 layer structure micro-sphere as cathodes for Li-ion batteries. The impurity phase has been eliminated wholly without changing the R-3m space group of LiNi0.8Co0.15Al0.05O2. The electrochemical performance of LiNi0.8Co0.15Al0.05O2 cathodes depend on the sintering step, temperature, particle size and uniformity. The sample pre-sintered at 540 °C for 12 h and then sintered at 720 °C for 28 h exhibits the best electrochemical performance, which delivers a reversible capacity of 180.4, 165.8, 154.7 and 135.6 mAhg-1 at 0.2 C, 1 C, 2 C and 5 C, respectively. The capacity retention keeps over 87% after 76 cycles at 1 C. This method is simple, cheap and mass-productive, and thus suitable to large scale production of NCA cathodes directly used for lithium ion batteries.

In situ fabrication of high-performance Ni-GDC-nanocube core-shell anode for low-temperature solid-oxide fuel cells

PubMed Central

Yamamoto, Kazuhiro; Qiu, Nan; Ohara, Satoshi

2015-01-01

A core–shell anode consisting of nickel–gadolinium-doped-ceria (Ni–GDC) nanocubes was directly fabricated by a chemical process in a solution containing a nickel source and GDC nanocubes covered with highly reactive {001} facets. The cermet anode effectively generated a Ni metal framework even at 500 °C with the growth of the Ni spheres. Anode fabrication at such a low temperature without any sintering could insert a finely nanostructured layer close to the interface between the electrolyte and the anode. The maximum power density of the attractive anode was 97 mW cm–2, which is higher than that of a conventional NiO–GDC anode prepared by an aerosol process at 55 mW cm–2 and 600 °C, followed by sintering at 1300 °C. Furthermore, the macro- and microstructure of the Ni–GDC-nanocube anode were preserved before and after the power-generation test at 700 °C. Especially, the reactive {001} facets were stabled even after generation test, which served to reduce the activation energy for fuel oxidation successfully. PMID:26615816

Sintering Behavior of Spark Plasma Sintered SiC with Si-SiC Composite Nanoparticles Prepared by Thermal DC Plasma Process.

PubMed

Yu, Yeon-Tae; Naik, Gautam Kumar; Lim, Young-Bin; Yoon, Jeong-Mo

2017-11-25

The Si-coated SiC (Si-SiC) composite nanoparticle was prepared by non-transferred arc thermal plasma processing of solid-state synthesized SiC powder and was used as a sintering additive for SiC ceramic formation. Sintered SiC pellet was prepared by spark plasma sintering (SPS) process, and the effect of nano-sized Si-SiC composite particles on the sintering behavior of micron-sized SiC powder was investigated. The mixing ratio of Si-SiC composite nanoparticle to micron-sized SiC was optimized to 10 wt%. Vicker's hardness and relative density was increased with increasing sintering temperature and holding time. The relative density and Vicker's hardness was further increased by reaction bonding using additional activated carbon to the mixture of micron-sized SiC and nano-sized Si-SiC. The maximum relative density (97.1%) and Vicker's hardness (31.4 GPa) were recorded at 1800 °C sintering temperature for 1 min holding time, when 0.2 wt% additional activated carbon was added to the mixture of SiC/Si-SiC.

Production of sintered porous metal fluoride pellets

DOEpatents

Anderson, L.W.; Stephenson, M.J.

1973-12-25

Porous pellets characterized by a moderately reactive crust and a softer core of higher reactivity are produced by forming agglomerates containing a metal fluoride powder and a selected amount ofwater. The metal fluoride is selected to be sinterable and essentially non-reactive with gaseous fluorinating agents. The agglomerates are contacted with a gaseous fluorinating agent under controlled conditions whereby the heat generated by localized reaction of the agent and water is limited to values effccting bonding by localized sintering. Porous pellets composed of cryolite (Na/sub 3/AlF/sub 6/) can be used to selectively remove trace quantities of niobium pentafluoride from a feed gas consisting predominantly of uranium hexafluoride. (Official Gazette)

Pressureless sintered beta prime-Si3N4 solid solution: Fabrication, microstructure, and strength

NASA Technical Reports Server (NTRS)

Dutta, S.

1977-01-01

Si3N4, AlN, and Al2O3 were used as basic constituents in a study of the pressureless sintering of beta prime-Si3N4 solid solution as a function of temperature. Y2O3-SiO2 additions were used to promote liquid-phase sintering. The sintered specimens were characterized with respect to density, microstructure, strength, oxidation, and thermal shock resistance. Density greater than 98 percent of theoretical was achieved by pressureless sintering at 1750 C. The microstructure consisted essentially of fine-grained beta prime-Si3N4 solid solution as the major phase. Modulus of rupture strengths up to 483 MPa were achieved at moderate temperature (1000 C), but decreased to 228 MPa at 1380 C. This substantial strength loss was attributed to a glassy grain boundary phase formed during cooling from the sintering temperature. The best oxidation resistance was exhibited by a composition containing 3 mol % Y2O3-SiO2 additives. Water quench thermal shock resistance was equivalent to that of reaction sintered silicon nitride but lower than hot-pressed silicon nitride.

Optimal Design of Material and Process Parameters in Powder Injection Molding

NASA Astrophysics Data System (ADS)

Ayad, G.; Barriere, T.; Gelin, J. C.; Song, J.; Liu, B.

2007-04-01

The paper is concerned with optimization and parametric identification for the different stages in Powder Injection Molding process that consists first in injection of powder mixture with polymer binder and then to the sintering of the resulting powders part by solid state diffusion. In the first part, one describes an original methodology to optimize the process and geometry parameters in injection stage based on the combination of design of experiments and an adaptive Response Surface Modeling. Then the second part of the paper describes the identification strategy that one proposes for the sintering stage, using the identification of sintering parameters from dilatometeric curves followed by the optimization of the sintering process. The proposed approaches are applied to the optimization of material and process parameters for manufacturing a ceramic femoral implant. One demonstrates that the proposed approach give satisfactory results.

Irradiation resistance of silicon carbide joint at light water reactor–relevant temperature

DOE PAGES

Koyanagi, T.; Katoh, Y.; Kiggans, J. O.; ...

2017-03-10

We fabricated and irradiated monolithic silicon carbide (SiC) to SiC plate joints with neutrons at 270–310 °C to 8.7 dpa for SiC. The joining methods included solid state diffusion bonding using titanium and molybdenum interlayers, SiC nanopowder sintering, reaction sintering with a Ti-Si-C system, and hybrid processing of polymer pyrolysis and chemical vapor infiltration (CVI). All the irradiated joints exhibited apparent shear strength of more than 84 MPa on average. Significant irradiation-induced cracking was found in the bonding layers of the Ti and Mo diffusion bonds and Ti-Si-C reaction sintered bond. Furthermore, the SiC-based bonding layers of the SiC nanopowdermore » sintered and hybrid polymer pyrolysis and CVI joints all showed stable microstructure following the irradiation.« less

Pulsed Laser Deposition of BaCe(sub 0.85)Y(sub 0.15)0(sub 3) FILMS

NASA Technical Reports Server (NTRS)

Dynys, F. W.; Sayir, A.

2006-01-01

Pulsed laser deposition has been used to grow nanostructured BaCe(sub 0.85)Y(sub 0.15)0(sub 3) films. The objective is to enhance protonic conduction by reduction of membrane thickness. Sintered samples and laser targets were prepared by sintering BaCe(sub 0.85)Y(sub 0.15)O(sub 3) powders derived by solid state synthesis. Films 2 to 6 m thick were deposited by KrF excimer laser on Si and porous Al2O3 substrates. Nanocrystalline films were fabricated at deposition temperatures of 600-800 C deg at O2 pressure of 30 mTorr and laser fluence of 1.2 J/cm square. Films were characterized by x-ray diffraction, scanning electron microscopy and electrical impedance spectroscopy. Dense single phase BaCe(sub 0.85)Y((sub 0.15) 0(sub 3) films with a columnar growth morphology is observed, preferred crystal growth was found to be dependent upon deposition temperature and substrate type. Electrical conductivity of bulk samples produced by solid state sintering and thin film samples were measured over a temperature range of 100 C deg to 900 C deg in moist argon. Electrical conduction of the fabricated films was 1 to 4 orders of magnitude lower than the sintered bulk samples. With respect to the film growth direction, activation energy for electrical conduction is 3 times higher in the perpendicular direction than the parallel direction.

Benchmarking the expected stack manufacturing cost of next generation, intermediate-temperature protonic ceramic fuel cells with solid oxide fuel cell technology

NASA Astrophysics Data System (ADS)

Dubois, Alexis; Ricote, Sandrine; Braun, Robert J.

2017-11-01

Recent progress in the performance of intermediate temperature (500-600 °C) protonic ceramic fuel cells (PCFCs) has demonstrated both fuel flexibility and increasing power density that approach commercial application requirements. These developments may eventually position the technology as a viable alternative to solid oxide fuel cells (SOFCs) and molten carbonate fuel cells (MCFCs). The PCFCs investigated in this work are based on a BaZr0.8Y0.2O3-δ (BZY20) thin electrolyte supported by BZY20/Ni porous anodes, and a triple conducting cathode material comprised of BaCo0.4Fe0.4Zr0.1Y0.1O3-δ (BCFZY0.1). These cells are prepared using a low-cost solid-state reactive sintering (SSRS) process, and are capable of power densities of 0.156 W cm-2 at 500 °C operating directly from methane fuel. We develop a manufacturing cost model to estimate the Nth generation production costs of PCFC stack technology using high volume manufacturing processes and compare them to the state-of-the-art in SOFC technology. The low-cost cell manufacturing enabled by the SSRS technique compensates for the lower PCFC power density and the trade-off between operating temperature and efficiency enables the use of lower-cost stainless steel materials. PCFC stack production cost estimates are found to be as much as 27-37% lower at 550 °C than SOFCs operating at 800 °C.

Effect of various sintering temperature on resistivity behaviour and magnetoresistance of La{sub 0.67}Ba{sub 0.33}MnO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pratama, R.; Kurniawan, B., E-mail: bkuru07@gmail.com; Manaf, A.

2016-04-19

A detail work was conducted in order to investigate effect of various sintering temperature on resistivity behavior and its relation with the magneto-resistance effect of La{sub 0.67}Ba{sub 0.33}MnO{sub 3} (LBMO). The LBMO samples were synthesized using solid state reaction. Characterization using X-ray diffraction shows that all LBMO samples have a single phase for each variation. Variation of sintering temperature on the LBMO samples affects its lattice parameters. The resistivity measurement in an absence and under applied magnetic field resulted in a highly significant different values. In one of the sintering temperature variation of LBMO, an increasing resistivity had shown atmore » a low temperature and had reached its maximum value at a specific temperature, and then the resistivity decreases to the lowest value near the room temperature. Similar result observed at higher varieties of sintering temperature but with significant lower maximum resistivity.« less

Fabrication and study of double sintered TiNi-based porous alloys

NASA Astrophysics Data System (ADS)

Sergey, Anikeev; Valentina, Hodorenko; Timofey, Chekalkin; Victor, Gunther; Ji-hoon, Kang; Ji-soon, Kim

2017-05-01

Double-sintered porous TiNi-based alloys were fabricated and their structural characteristics and physico-mechanical properties were investigated. A fabrication technology of powder mixtures is elaborated in this article. Sintering conditions were chosen experimentally to ensure good structure and properties. The porous alloys were synthesized by solid-state double diffusion sintering (DDS) of Ti-Ni powder and prepare to obtain dense, crack-free, and homogeneous samples. The Ti-Ni compound sintered at various temperatures was investigated by scanning electron microscopy. Phase composition of the sintered alloys was determined by x-ray diffraction. Analysis of the data confirmed the morphology and structural parameters. Mechanical and physical properties of the sintered alloys were evaluated. DDS at 1250 °C was found to be optimal to produce porous samples with a porosity of 56% and mean pore size of 90 μm. Pore size distribution was unimodal within the narrow range of values. The alloys present enhanced strength and ductility, owing to both the homogeneity of the macrostructure and relative elasticity of the bulk, which is hardened by the Ni-rich precipitates. These results suggest the possibility to manufacture porous TiNi-based alloys for application as a new class of dental implants.

Process Developed for Generating Ceramic Interconnects With Low Sintering Temperatures for Solid Oxide Fuel Cells

NASA Technical Reports Server (NTRS)

Zhong, Zhi-Min; Goldsby, Jon C.

2005-01-01

Solid oxide fuel cells (SOFCs) have been considered as premium future power generation devices because they have demonstrated high energy-conversion efficiency, high power density, and extremely low pollution, and have the flexibility of using hydrocarbon fuel. The Solid-State Energy Conversion Alliance (SECA) initiative, supported by the U.S. Department of Energy and private industries, is leading the development and commercialization of SOFCs for low-cost stationary and automotive markets. The targeted power density for the initiative is rather low, so that the SECA SOFC can be operated at a relatively low temperature (approx. 700 C) and inexpensive metallic interconnects can be utilized in the SOFC stack. As only NASA can, the agency is investigating SOFCs for aerospace applications. Considerable high power density is required for the applications. As a result, the NASA SOFC will be operated at a high temperature (approx. 900 C) and ceramic interconnects will be employed. Lanthanum chromite-based materials have emerged as a leading candidate for the ceramic interconnects. The interconnects are expected to co-sinter with zirconia electrolyte to mitigate the interface electric resistance and to simplify the processing procedure. Lanthanum chromites made by the traditional method are sintered at 1500 C or above. They react with zirconia electrolytes (which typically sinter between 1300 and 1400 C) at the sintering temperature of lanthanum chromites. It has been envisioned that lanthanum chromites with lower sintering temperatures can be co-fired with zirconia electrolyte. Nonstoichiometric lanthanum chromites can be sintered at lower temperatures, but they are unstable and react with zirconia electrolyte during co-sintering. NASA Glenn Research Center s Ceramics Branch investigated a glycine nitrate process to generate fine powder of the lanthanum-chromite-based materials. By simultaneously doping calcium on the lanthanum site, and cobalt and aluminum on the chromium site, we could sinter the materials below 1400 C. The doping concentrations were adjusted so that the thermal expansion coefficient matched that of the zirconia electrolyte. Also, the investigation was focused on stoichiometric compositions so that the materials would have better stability. Co-sintering and chemical compatibility with zirconia electrolyte were examined by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy (line scanning and dot map). The results showed that the materials bond well, but do not react, with zirconia electrolyte. The electric conductivity of the materials measured at 900 C in air was about 20 S/cm.

Fabrication of Fe1.1Se0.5Te0.5 bulk by a high energy ball milling technique

NASA Astrophysics Data System (ADS)

Liu, Jixing; Li, Chengshan; Zhang, Shengnan; Feng, Jianqing; Zhang, Pingxiang; Zhou, Lian

2017-11-01

Fe1.1Se0.5Te0.5 superconducting bulks were successfully synthesized by a high energy ball milling (HEBM) aided sintering technique. Two advantages of this new technique have been revealed compared with traditional solid state sintering method. One is greatly increased the density of sintered bulks. It is because the precursor powders with β-Fe(Se, Te) and δ-Fe(Se, Te) were obtained directly by the HEBM process and without formation of liquid Se (and Te), which could avoid the huge volume expansion. The other is the obvious decrease of sintering temperature and dwell time due to the effective shortened length of diffusion paths. The superconducting critical temperature Tc of 14.2 K in our sample is comparable with those in previous reports, and further optimization of chemical composition is on the way.

Hybrid deposition of thin film solid oxide fuel cells and electrolyzers

DOEpatents

Jankowski, A.F.; Makowiecki, D.M.; Rambach, G.D.; Randich, E.

1998-05-19

The use of vapor deposition techniques enables synthesis of the basic components of a solid oxide fuel cell (SOFC); namely, the electrolyte layer, the two electrodes, and the electrolyte-electrode interfaces. Such vapor deposition techniques provide solutions to each of the three critical steps of material synthesis to produce a thin film solid oxide fuel cell (TFSOFC). The electrolyte is formed by reactive deposition of essentially any ion conducting oxide, such as defect free, yttria stabilized zirconia (YSZ) by planar magnetron sputtering. The electrodes are formed from ceramic powders sputter coated with an appropriate metal and sintered to a porous compact. The electrolyte-electrode interface is formed by chemical vapor deposition of zirconia compounds onto the porous electrodes to provide a dense, smooth surface on which to continue the growth of the defect-free electrolyte, whereby a single fuel cell or multiple cells may be fabricated. 8 figs.

Hybrid deposition of thin film solid oxide fuel cells and electrolyzers

DOEpatents

Jankowski, Alan F.; Makowiecki, Daniel M.; Rambach, Glenn D.; Randich, Erik

1999-01-01

The use of vapor deposition techniques enables synthesis of the basic components of a solid oxide fuel cell (SOFC); namely, the electrolyte layer, the two electrodes, and the electrolyte-electrode interfaces. Such vapor deposition techniques provide solutions to each of the three critical steps of material synthesis to produce a thin film solid oxide fuel cell (TFSOFC). The electrolyte is formed by reactive deposition of essentially any ion conducting oxide, such as defect free, yttria stabilized zirconia (YSZ) by planar magnetron sputtering. The electrodes are formed from ceramic powders sputter coated with an appropriate metal and sintered to a porous compact. The electrolyte-electrode interface is formed by chemical vapor deposition of zirconia compounds onto the porous electrodes to provide a dense, smooth surface on which to continue the growth of the defect-free electrolyte, whereby a single fuel cell or multiple cells may be fabricated.

Hybrid deposition of thin film solid oxide fuel cells and electrolyzers

DOEpatents

Jankowski, Alan F.; Makowiecki, Daniel M.; Rambach, Glenn D.; Randich, Erik

1998-01-01

The use of vapor deposition techniques enables synthesis of the basic components of a solid oxide fuel cell (SOFC); namely, the electrolyte layer, the two electrodes, and the electrolyte-electrode interfaces. Such vapor deposition techniques provide solutions to each of the three critical steps of material synthesis to produce a thin film solid oxide fuel cell (TFSOFC). The electrolyte is formed by reactive deposition of essentially any ion conducting oxide, such as defect free, yttria stabilized zirconia (YSZ) by planar magnetron sputtering. The electrodes are formed from ceramic powders sputter coated with an appropriate metal and sintered to a porous compact. The electrolyte-electrode interface is formed by chemical vapor deposition of zirconia compounds onto the porous electrodes to provide a dense, smooth surface on which to continue the growth of the defect-free electrolyte, whereby a single fuel cell or multiple cells may be fabricated.

The thermal stability of hydroxyapatite in biphasic calcium phosphate ceramics.

PubMed

Nilen, R W N; Richter, P W

2008-04-01

Biphasic calcium phosphate ceramics (BCP) comprising a mix of non-resorbable hydroxyapatite (HA) and resorbable beta-tricalcium phosphate (beta-TCP) are particularly suitable materials for synthetic bone substitute applications. In this study, HA synthesised by solid state reaction was mechanically mixed with beta-TCP, then sintered to form a suite of BCP materials with a wide range of HA/beta-TCP phase content ratios. The influence of sintering temperature and composition on the HA thermal stability was quantified by X-ray diffraction (XRD). The pre-sinter beta-TCP content was found to strongly affect the post-sinter HA/beta-TCP ratio by promoting the thermal decomposition of HA to beta-TCP, even at sintering temperatures as low as 850 degrees C. For BCP material with pre-sinter HA/beta-TCP = 40/60 wt%, approximately 80% of the HA decomposed to beta-TCP during sintering at 1000 degrees C. Furthermore, the HA content appeared to influence the reverse transformation of alpha-TCP to beta-TCP expected upon gradual cooling from sintering temperatures greater than 1125 degrees C. Because the HA/beta-TCP ratio dominantly determines the rate and extent of BCP resorption in vivo, the possible thermal decomposition of HA during BCP synthesis must be considered, particularly if high temperature treatments are involved.

Reactive solid surface morphology variation via ionic diffusion.

PubMed

Sun, Zhenchao; Zhou, Qiang; Fan, Liang-Shih

2012-08-14

In gas-solid reactions, one of the most important factors that determine the overall reaction rate is the solid morphology, which can be characterized by a combination of smooth, convex and concave structures. Generally, the solid surface structure varies in the course of reactions, which is classically noted as being attributed to one or more of the following three mechanisms: mechanical interaction, molar volume change, and sintering. Here we show that if a gas-solid reaction involves the outward ionic diffusion of a solid-phase reactant then this outward ionic diffusion could eventually smooth the surface with an initial concave and/or convex structure. Specifically, the concave surface is filled via a larger outward diffusing surface pointing to the concave valley, whereas the height of the convex surface decreases via a lower outward diffusion flux in the vertical direction. A quantitative 2-D continuum diffusion model is established to analyze these two morphological variation processes, which shows consistent results with the experiments. This surface morphology variation by solid-phase ionic diffusion serves to provide a fourth mechanism that supplements the traditionally acknowledged solid morphology variation or, in general, porosity variation mechanisms in gas-solid reactions.

A Novel Solid State Ultracapacitor

NASA Technical Reports Server (NTRS)

Cortes-Pena, A. Y.; Rolin, T. D.; Hill, C. W.

2017-01-01

Novel dielectric materials were researched to develop an internal barrier layer capacitor that is fully solid state. These materials included reduced nanoparticles of barium titanate that were coated with various atomic layer deposited oxides. The nanoparticle powders were then densified into pellets and characterized using a dielectric test fixture over a frequency range of 20 Hz to 2 MHz. Densification and sintering were evaluated using scanning electron microscopic techniques. Ultimately, the samples showing the most promising electrical characteristics of permittivity, dissipation factor and equivalent series resistance were chosen to manufacture devices for subsequent testing.

CALCINATION AND SINTERING OF SORBENTS DURING BOILER INJECTION FOR DRY SULFUR DIOXIDE CONTROL

EPA Science Inventory

The paper discusses the calcination and sintering of sorbents during boiler injection for dry sulfur dioxide (S02) control, with emphasis on calcium hydroxide--Ca(OH)2--because of its superior reactivity with S02 and its wide commercial availability. Calcination and sintering are...

Fuel electrode containing pre-sintered nickel/zirconia for a solid oxide fuel cell

DOEpatents

Ruka, Roswell J.; Vora, Shailesh D.

2001-01-01

A fuel cell structure (2) is provided, having a pre-sintered nickel-zirconia fuel electrode (6) and an air electrode (4), with a ceramic electrolyte (5) disposed between the electrodes, where the pre-sintered fuel electrode (6) contains particles selected from the group consisting of nickel oxide, cobalt and cerium dioxide particles and mixtures thereof, and titanium dioxide particles, within a matrix of yttria-stabilized zirconia and spaced-apart filamentary nickel strings having a chain structure, and where the fuel electrode can be sintered to provide an active solid oxide fuel cell.

Phase transformations in the reaction cell of TiNi-based sintered systems

NASA Astrophysics Data System (ADS)

Artyukhova, Nadezhda; Anikeev, Sergey; Yasenchuk, Yuriy; Chekalkin, Timofey; Gunther, Victor; Kaftaranova, Maria; Kang, Ji-Hoon; Kim, Ji-Soon

2018-05-01

The present work addresses the structural-phase state changes of porous TiNi-based compounds fabricated by reaction sintering (RS) of Ti and Ni powders with Co, Mo, and no additives introduced. The study also emphasizes the features of a reaction cell (RC) during the transition from the solid- to liquid-phase sintering. Mechanisms of phase transformations occurring in the solid phase, involving the low-melting Ti2Ni phase within the RC, have been highlighted. Also, the intermediate Ti2Ni phase had a crucial role to provide both the required RS behavior and modified phase composition of RS samples, and besides, it is found to be responsible for the near-equiatomic TiNi saturation of the melt. Both cobalt and molybdenum additives are shown to cause additional structuring of the transition zone (TZ) at the Ti2Ni‑TiNi interface and broadening of this zone. The impact of Co and Mo on the Ti2Ni phase is evident through fissuring of this phase layer, which is referred to solidified stresses increased in the layer due to post-alloying defects in the structure.

Sintered Cathodes for All-Solid-State Structural Lithium-Ion Batteries

NASA Technical Reports Server (NTRS)

Huddleston, William; Dynys, Frederick; Sehirlioglu, Alp

2017-01-01

All-solid-state structural lithium ion batteries serve as both structural load-bearing components and as electrical energy storage devices to achieve system level weight savings in aerospace and other transportation applications. This multifunctional design goal is critical for the realization of next generation hybrid or all-electric propulsion systems. Additionally, transitioning to solid state technology improves upon battery safety from previous volatile architectures. This research established baseline solid state processing conditions and performance benchmarks for intercalation-type layered oxide materials for multifunctional application. Under consideration were lithium cobalt oxide and lithium nickel manganese cobalt oxide. Pertinent characteristics such as electrical conductivity, strength, chemical stability, and microstructure were characterized for future application in all-solid-state structural battery cathodes. The study includes characterization by XRD, ICP, SEM, ring-on-ring mechanical testing, and electrical impedance spectroscopy to elucidate optimal processing parameters, material characteristics, and multifunctional performance benchmarks. These findings provide initial conditions for implementing existing cathode materials in load bearing applications.

Sintered electrode for solid oxide fuel cells

DOEpatents

Ruka, Roswell J.; Warner, Kathryn A.

1999-01-01

A solid oxide fuel cell fuel electrode is produced by a sintering process. An underlayer is applied to the electrolyte of a solid oxide fuel cell in the form of a slurry, which is then dried. An overlayer is applied to the underlayer and then dried. The dried underlayer and overlayer are then sintered to form a fuel electrode. Both the underlayer and the overlayer comprise a combination of electrode metal such as nickel, and stabilized zirconia such as yttria-stabilized zirconia, with the overlayer comprising a greater percentage of electrode metal. The use of more stabilized zirconia in the underlayer provides good adhesion to the electrolyte of the fuel cell, while the use of more electrode metal in the overlayer provides good electrical conductivity. The sintered fuel electrode is less expensive to produce compared with conventional electrodes made by electrochemical vapor deposition processes. The sintered electrodes exhibit favorable performance characteristics, including good porosity, adhesion, electrical conductivity and freedom from degradation.

Sintered electrode for solid oxide fuel cells

DOEpatents

Ruka, R.J.; Warner, K.A.

1999-06-01

A solid oxide fuel cell fuel electrode is produced by a sintering process. An underlayer is applied to the electrolyte of a solid oxide fuel cell in the form of a slurry, which is then dried. An overlayer is applied to the underlayer and then dried. The dried underlayer and overlayer are then sintered to form a fuel electrode. Both the underlayer and the overlayer comprise a combination of electrode metal such as nickel, and stabilized zirconia such as yttria-stabilized zirconia, with the overlayer comprising a greater percentage of electrode metal. The use of more stabilized zirconia in the underlayer provides good adhesion to the electrolyte of the fuel cell, while the use of more electrode metal in the overlayer provides good electrical conductivity. The sintered fuel electrode is less expensive to produce compared with conventional electrodes made by electrochemical vapor deposition processes. The sintered electrodes exhibit favorable performance characteristics, including good porosity, adhesion, electrical conductivity and freedom from degradation. 4 figs.

Mechanochemical stabilization and sintering of nanocrystalline the (ZrO2)0.97 (Y2O3)0.03 solid solution from pure oxides

NASA Astrophysics Data System (ADS)

Rendtorff, N. M.; Suárez, G.; Sakka, Y.; Aglietti, E. F.

2011-10-01

The mechanochemical activation processing has proved to be an effective technique to enhance a solid-state reaction at relatively low temperatures. In such a process, the mechanical effects of milling, such as reduction of particle size and mixture homogenization, are accompanied by chemical effects, such as partial decomposition of salts or hydroxides resulting in very active reactants. The objective of the present work is to obtain (ZrO2)0.97(Y2O3)0.03 nanocrystalline tetragonal solid solution powders directly using a high energy milling on a mixture of the pure oxides. A second objective is to evaluate the efficiency of the processing proposed and to characterize both textural and structural evolution of the mixtures during the milling processes and throughout posterior low temperature treatments. The Textural and structural evolution were studied by XRD analysis, specific area measurements (BET) and SEM. Firstly a decrease of the crystallinity of the reactants was observed, followed by the disappearance of Y2O3 diffraction peaks and the partial appearance of the tetragonal phase at room temperature. The solid solution proportion was increased with the high energy milling time, obtaining complete stabilization of the tetragonal solid solution with long milling treatments (60 min).The obtained powders were uniaxially pressed and sintered at different temperatures (600-1400°C) the influence of the milling time was correlated with the sinterization degree and final crystalline composition of the materials. Finally, fully stabilized nanocrystalline zirconia materials were obtained satisfactorily by the proposed method.

Vacuum-sintered body of a novel apatite for artificial bone

NASA Astrophysics Data System (ADS)

Tamura, Kenichi; Fujita, Tatsushi; Morisaki, Yuriko

2013-12-01

We produced regenerative artificial bone material and bone parts using vacuum-sintered bodies of a novel apatite called "Titanium medical apatite (TMA®)" for biomedical applications. TMA was formed by chemically connecting a Ti oxide molecule with the reactive [Ca10(PO4)6] group of Hydroxyapatite (HAp). The TMA powders were kneaded with distilled water, and solid cylinders of compacted TMA were made by compression molding at 10 MPa using a stainless-steel vessel. The TMA compacts were dried and then sintered in vacuum (about 10-3 Pa) or in air using a resistance heating furnace in the temperature range 1073-1773 K. TMA compacts were sintered at temperatures greater than 1073 K, thus resulting in recrystallization. The TMA compact bodies sintered in the range 1273-1773 K were converted into mixtures composed of three crystalline materials: α-TCP (tricalcium phosphate), β-TCP, and Perovskite-CaTiO3. The Perovskite crystals were stable and hard. In vacuum-sintering, the Perovskite crystals were transformed into fibers (approximately 1 µm in diameter × 8 µm in length), and the fiber distribution was uniform in various directions. We refer to the TMA vacuum-sintered bodies as a "reinforced composite material with Perovskite crystal fibers." However, in atmospheric sintering, the Perovskite crystals were of various sizes and were irregularly distributed as a result of the effect of oxygen. After sintering temperature at 1573 K, the following results were obtained: the obtained TMA vacuum-sintered bodies (1) were white, (2) had a density of approximately 2300 kg/m3 (corresponding to that of a compact bone or a tooth), and had a thermal conductivity of approximately 31.3 W/(m·K) (corresponding to those of metal or ceramic implants). Further, it was possible to cut the TMA bodies into various forms with a cutting machine. An implant made of TMA and inserted into a rabbit jaw bone was covered by new bone tissues after just one month because of the high biocompatibility of the TMA implant. TMA vacuum-sintered bodies are promising biomaterials for use as artificial bone materials to regenerate bone parts and produce bone reinforcement structures that are used for bone junctions in dental and orthopedic surgery.

Effect of microwave-assisted sintering on dielectric properties of CaCu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Rani, Suman; Ahlawat, Neetu; Punia, R.; Kundu, R. S.; Ahlawat, N.

2016-05-01

In this present work, CaCu3Ti4O12 (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It was observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.

High-Temperature Proton-Conducting Ceramics Developed

NASA Technical Reports Server (NTRS)

Sayir, Ali; Dynys, Frederick W.; Berger, M. H.

2005-01-01

High-temperature protonic conductors (HTPC) are needed for hydrogen separation, hydrogen sensors, fuel cells, and hydrogen production from fossil fuels. The HTPC materials for hydrogen separation at high temperatures are foreseen to be metal oxides with the perovskite structure A(sup 2+)B(sup 4+)C(sup 2-, sub 3) and with the trivalent cation (M(sup 3+)) substitution at the B(sup 4+)-site to introduce oxygen vacancies. The high affinity for hydrogen ions (H(sup +)) is advantageous for protonic transport, but it increases the reactivity toward water (H2O) and carbon dioxide (CO2), which can lead to premature membrane failure. In addition, there are considerable technological challenges related to the processing of HTPC materials. The high melting point and multi-cation chemistry of HTPC materials creates difficulties in in achieving high-density, single-phase membranes by solid-state sintering. The presence of secondary phases and grain-boundary interfaces are detrimental to the protonic conduction and environmental stability of polycrystalline HTPC materials.

3D-Printing Electrolytes for Solid-State Batteries.

PubMed

McOwen, Dennis W; Xu, Shaomao; Gong, Yunhui; Wen, Yang; Godbey, Griffin L; Gritton, Jack E; Hamann, Tanner R; Dai, Jiaqi; Hitz, Gregory T; Hu, Liangbing; Wachsman, Eric D

2018-05-01

Solid-state batteries have many enticing advantages in terms of safety and stability, but the solid electrolytes upon which these batteries are based typically lead to high cell resistance. Both components of the resistance (interfacial, due to poor contact with electrolytes, and bulk, due to a thick electrolyte) are a result of the rudimentary manufacturing capabilities that exist for solid-state electrolytes. In general, solid electrolytes are studied as flat pellets with planar interfaces, which minimizes interfacial contact area. Here, multiple ink formulations are developed that enable 3D printing of unique solid electrolyte microstructures with varying properties. These inks are used to 3D-print a variety of patterns, which are then sintered to reveal thin, nonplanar, intricate architectures composed only of Li 7 La 3 Zr 2 O 12 solid electrolyte. Using these 3D-printing ink formulations to further study and optimize electrolyte structure could lead to solid-state batteries with dramatically lower full cell resistance and higher energy and power density. In addition, the reported ink compositions could be used as a model recipe for other solid electrolyte or ceramic inks, perhaps enabling 3D printing in related fields. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of the addition of municipal solid waste incineration fly ash on the behavior of polychlorinated dibenzo-p-dioxins and furans in the iron ore sintering process.

PubMed

Min, Yi; Liu, Chengjun; Shi, Peiyang; Qin, Chongda; Feng, Yutao; Liu, Baichen

2018-04-11

Raw materials were co-sintered with municipal solid waste incineration (MSWI) fly ash through iron ore sintering to promote the safe treatment and utilization of MSWI fly ash. To assess the feasibility of this co-sintering method, in this study, the effects of the addition of MSWI fly ash on the formation and emission of polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs) were estimated via iron ore sintering pot experiments. During co-sintering, most of the PCDD/Fs in the added MSWI fly ash were decomposed and transformed into PCDD/Fs associated with iron sintering, and the concentrations of lower- and mid-chlorinated congeners increased. As there was a sufficient chlorine source and the sintering bed permeability was decreased by the addition of MSWI fly ash, the PCDD/F concentration in the exhaust gas increased. The mass emission of PCDD/Fs decreased; however, the emission of toxic PCDD/Fs increased beyond the total emissions from the independent MSW incineration and iron ore sintering processes due to the transformation of PCDD/F congeners. The co-sintering may be an important solution after technological improvements in the flue gas cleaning system and PCDD/F formation inhibition procedures. Copyright © 2018. Published by Elsevier Ltd.

Optimum Conditions for Preparation of High-Performance (Ba0.97Ca0.03)(Ti0.94Sn0.06)O3 Ceramics by Solid-State Combustion

NASA Astrophysics Data System (ADS)

Chootin, Suphornphun; Bongkarn, Theerachai

2017-08-01

The effects of calcination conditions (950°C to 1200°C for 2 h to 6 h) and sintering temperature (1300°C to 1500°C for 2 h) on phase formation, microstructure, and electrical behavior of lead-free piezoelectric (Ba0.97Ca0.03)(Ti0.94Sn0.06)O3 (BCTS) ceramics produced by solid-state combustion using glycine as fuel have been investigated. BCTS powder with pure perovskite structure was obtained by calcination at 1100°C for 4 h. The microstructure of the BCTS powders showed almost spherical shape with average particle size increasing from 184 nm to 320 nm as the calcination temperature and soaking time were increased. The XRD patterns of all ceramics exhibited single perovskite structure. Rietveld refinement analysis indicated that the BCTS ceramics exhibited coexistence of orthorhombic and tetragonal phase in all samples with increased tetragonal phase content with increasing sintering temperature. The average grain size, density, dielectric constants at room ( ɛ r) and Curie temperature ( ɛ C), remanent polarization ( P r), and piezoelectric constant ( d 33) increased as the sintering temperature was increased up to 1400°C, then decreased. BCTS ceramic sintered at 1400°C exhibited the highest relative density (98%), highest dielectric response ( ɛ r = 4951, ɛ C = 19,185), good ferroelectric behavior ( P r = 12.74 μC/cm2 and coercive field E c = 1.60 kV/cm), and highest d 33 value (528 pC/N). The large piezoelectricity of BCTS ceramics makes them good candidates for use in lead-free applications to replace Pb-based ceramics.

Rapid, cool sintering of wet processed yttria-stabilized zirconia ceramic electrolyte thin films.

PubMed

Park, Jun-Sik; Kim, Dug-Joong; Chung, Wan-Ho; Lim, Yonghyun; Kim, Hak-Sung; Kim, Young-Beom

2017-09-29

Here we report a photonic annealing process for yttria-stabilized zirconia films, which are one of the most well-known solid-state electrolytes for solid oxide fuel cells (SOFCs). Precursor films were coated using a wet-chemical method with a simple metal-organic precursor solution and directly annealed at standard pressure and temperature by two cycles of xenon flash lamp irradiation. The residual organics were almost completely decomposed in the first pre-annealing step, and the fluorite crystalline phases and good ionic conductivity were developed during the second annealing step. These films showed properties comparable to those of thermally annealed films. This process is much faster than conventional annealing processes (e.g. halogen furnaces); a few seconds compared to tens of hours, respectively. The significance of this work includes the treatment of solid-state electrolyte oxides for SOFCs and the demonstration of the feasibility of other oxide components for solid-state energy devices.

Sintering Theory and Practice

NASA Astrophysics Data System (ADS)

German, Randall M.

1996-01-01

Although sintering is an essential process in the manufacture of ceramics and certain metals, as well as several other industrial operations, until now, no single book has treated both the background theory and the practical application of this complex and often delicate procedure. In Sintering Theory and Practice, leading researcher and materials engineer Randall M. German presents a comprehensive treatment of this subject that will be of great use to manufacturers and scientists alike. This practical guide to sintering considers the fact that while the bonding process improves strength and other engineering properties of the compacted material, inappropriate methods of control may lead to cracking, distortion, and other defects. It provides a working knowledge of sintering, and shows how to avoid problems while accounting for variables such as particle size, maximum temperature, time at that temperature, and other problems that may cause changes in processing. The book describes the fundamental atomic events that govern the transformation from particles to solid, covers all forms of the sintering process, and provides a summary of many actual production cycles. Building from the ground up, it begins with definitions and progresses to measurement techniques, easing the transition, especially for students, into advanced topics such as single-phase solid-state sintering, microstructure changes, the complications of mixed particles, and pressure-assisted sintering. German draws on some six thousand references to provide a coherent and lucid treatment of the subject, making scientific principles and practical applications accessible to both students and professionals. In the process, he also points out and avoids the pitfalls found in various competing theories, concepts, and mathematical disputes within the field. A unique opportunity to discover what sintering is all about--both in theory and in practice What is sintering? We see the end product of this thermal process all around us--in manufactured objects from metals, ceramics, polymers, and many compounds. From a vast professional literature, Sintering Theory and Practice emerges as the only comprehensive, systematic, and self-contained volume on the subject. Covering all aspects of sintering as a processing topic, including materials, processes, theories, and the overall state of the art, the book Offers numerous examples, illustrations, and tables that detail actual processing cycles, and that stress existing knowledge in the field Uses the specifics of various consolidation cycles to illustrate the basics Leads the reader from the fundamentals to advanced topics, without getting bogged down in various mathematical disputes over treatments and measurements Supports the discussion with critically selected references from thousands of sources Examines the sintering behavior of a wide variety of engineered materials--metals, alloys, oxide ceramics, composites, carbides, intermetallics, glasses, and polymers Guides the reader through the sintering processes for several important industrial materials and demonstrates how to control these processes effectively and improve present techniques Provides a helpful reference for specific information on materials, processing problems, and concepts For practitioners and researchers in ceramics, powder metallurgy, and other areas, and for students and faculty in materials science and engineering, this book provides the know-how and understanding crucial to many industrial operations, offers many ideas for further research, and suggests future applications of this important technology. This book offers an unprecedented opportunity to explore sintering in both practical and theoretical terms, whether at the lab or in real-world applications, and to acquire a broad, yet thorough, understanding of this important technology.

Modified Ion-Conducting Ceramics Based on Lanthanum Gallate: Synthesis, Structure, and Properties

NASA Astrophysics Data System (ADS)

Kaleva, G. M.; Politova, E. D.; Mosunov, A. V.; Sadovskaya, N. V.

2018-06-01

A review is presented of the synthesis and complex investigation of modified ion-conducting ceramics based on heterosubstituted lanthanum gallate as a promising electrolyte material for solid oxide fuel cells. The effect the composition of multicomponent complex oxides has on the structure, microstructure, and electrophysical properties of ceramics is examined. Samples of ceramics with new compositions are produced via solid-state synthesis and modified with lithium fluoride. A drop is observed in the sintering temperature of the ceramics, caused by the liquid phase mechanism of sintering as a result of the low-melting superstoichiometric quantities of the additive. The effect lithium fluoride has on the process of phase formation, microstructure, and conductivity of the ceramics is investigated. It is found that samples modified with lithium fluoride display high density, dense grain packing, and high values of electrical conductivity at high temperatures.

Synthesis and photocatalytic activity of sepiolite supportednano-TiO2 composites prepared by a mild solid-state sintering process

NASA Astrophysics Data System (ADS)

Liao, L. M.; Wang, Z. Q.; Liang, H.; Feng, J.; Zhang, D.

2016-08-01

Supported nano-TiO2photocatalysts play an important role in water environment restoration because of their potential application to photocatalytic degradation of organic contaminants in waste water. With sepiolite as the support, the nano-TiO2/sepiolite composite photocatalysts were synthesized by an easily operated and mild solid-state sintering process.The microstructureand photocatalytic property of the sepiolite supportednano-TiO2 composites were characterized and analyzed by X-ray diffraction spectroscopy, UV-Visible spectroscopy and fluorescence spectroscopy. In addition, the influences of calcination temperature and load ratios on the photocatalytic activity of sepiolite supported nano-TiO2 composites were studied.The results indicated that appropriate ratios of sepiolite supports to nano-TiO2contributed to uniform dispersion of nanoparticles, and enhanced the absorption ability within the UV-Vis range, and consequently increased the photocatalytic activity of the composites.Under the preparation conditions of 90 wt. % TiO2 loading and calcinated at 400 °C, a maximum in photocatalytic activity ofnano-TiO2 sepiolite composite was obtained.

Symmetrical, bi-electrode supported solid oxide fuel cell

NASA Technical Reports Server (NTRS)

Sofie, Stephen W. (Inventor); Cable, Thomas L. (Inventor)

2009-01-01

The present invention is a symmetrical bi-electrode supported solid oxide fuel cell comprising a sintered monolithic framework having graded pore electrode scaffolds that, upon treatment with metal solutions and heat subsequent to sintering, acquire respective anodic and cathodic catalytic activity. The invention is also a method for making such a solid oxide fuel cell. The graded pore structure of the graded pore electrode scaffolds in achieved by a novel freeze casting for YSZ tape.

High hardness BaCb-(BxOy/BN) composites with 3D mesh-like fine grain-boundary structure by reactive spark plasma sintering.

PubMed

Vasylkiv, Oleg; Borodianska, Hanna; Badica, Petre; Grasso, Salvatore; Sakka, Yoshio; Tok, Alfred; Su, Liap Tat; Bosman, Michael; Ma, Jan

2012-02-01

Boron carbide B4C powders were subject to reactive spark plasma sintering (also known as field assisted sintering, pulsed current sintering or plasma assisted sintering) under nitrogen atmosphere. For an optimum hexagonal BN (h-BN) content estimated from X-ray diffraction measurements at approximately 0.4 wt%, the as-prepared BaCb-(BxOy/BN) ceramic shows values of Berkovich and Vickers hardness of 56.7 +/- 3.1 GPa and 39.3 +/- 7.6 GPa, respectively. These values are higher than for the vacuum SPS processed B4C pristine sample and the h-BN -mechanically-added samples. XRD and electronic microscopy data suggest that in the samples produced by reactive SPS in N2 atmosphere, and containing an estimated amount of 0.3-1.5% h-BN, the crystallite size of the boron carbide grains is decreasing with the increasing amount of N2, while for the newly formed lamellar h-BN the crystallite size is almost constant (approximately 30-50 nm). BN is located at the grain boundaries between the boron carbide grains and it is wrapped and intercalated by a thin layer of boron oxide. BxOy/BN forms a fine and continuous 3D mesh-like structure that is a possible reason for good mechanical properties.

Effect of sintering temperature on the microstructure, electrical and magnetic properties of Zn0.98 Mn0.02O material

NASA Astrophysics Data System (ADS)

Sebayang, K.; Aryanto, D.; Simbolon, S.; Kurniawan, C.; Hulu, S. F.; Sudiro, T.; Ginting, M.; Sebayang, P.

2018-02-01

Zn0.98Mn0.02O material was synthesized from ZnO and MnO2 powders using solid state reaction method. The microstructure, electrical and magnetic properties of Zn0.98Mn0.02O were studied as a function of sintering temperature. The X-ray diffraction analysis indicates that the main phase of synthesized sample is composed of hexagonal wurtzite ZnO phase. While the secondary phase of ZnMnO3 were found at the sintering temperature of 700°C and 900°C. The electrical properties measurement of Zn0.98Mn0.02O sample revealed that the resistivity and the dielectric constant of samples increase with the increase of sintering temperature. The ferromagnetic properties at room temperature were observed in the Zn0.98Mn0.02O samples sintered at 500°C and 700°C. It also found that the increase in sintering temperature leads to a tendency toward the changes in the magnetic properties into paramagnetic. The presence of ZnMnO3 secondary phases in Zn0.98Mn0.02O system is believed to be a factor that affects the decrease of the electrical and magnetic properties of the sample.

Mechanical Properties of β-Ti-35Nb-2.5Sn Alloy Synthesized by Mechanical Alloying and Pulsed Current Activated Sintering

NASA Astrophysics Data System (ADS)

Omran, Abdel-Nasser; Woo, Kee-Do; Lee, Hyun Bom

2012-12-01

A developed Ti-35 pct Nb-2.5 pct Sn (wt pct) alloy was synthesized by mechanical alloying using high-energy ball-milled powders, and the powder consolidation was done by pulsed current activated sintering (PCAS). The starting powder materials were mixed for 24 hours and then milled by high-energy ball milling (HEBM) for 1, 4, and 12 hours. The bulk solid samples were fabricated by PCAS at 1073 K to 1373 K (800 °C to 1100 °C) for a short time, followed by rapid cooling to 773 K (500 °C). The relative density of the sintered samples was about 93 pct. The Ti was completely transformed from α to β-Ti phase after milling for 12 hours in powder state, and the specimen sintered at 1546 K (1273 °C) was almost transformed to β-Ti phase. The homogeneity of the sintered specimen increased with increasing milling time and sintering temperature, as did its hardness, reaching 400 HV after 12 hours of milling. The Young's modulus was almost constant for all sintered Ti-35 pct Nb-2.5 pct Sn specimens at different milling times. The Young's modulus was low (63.55 to 65.3 GPa) compared to that of the standard alloy of Ti-6Al-4V (100 GPa). The wear resistance of the sintered specimen increased with increasing milling time. The 12-hour milled powder exhibited the best wear resistance.

Grain Boundary Engineering of Lithium-Ion-Conducting Lithium Lanthanum Titanate for Lithium-Air Batteries

DTIC Science & Technology

2015-01-01

Tojo T, Sakurai Y. Synthesis and lithium - ion conductivity for perovskite-type Li3/8Sr7/16Ta3/4Zr1/4O3 solid electrolyte by powder-bed sintering...battery performance is limited by the electrolytic membrane, which needs high Li-ionic conductivity. Lithium lanthanum titanate (Li3xLa(2/3)-xTiO3, or...of the A-site ions and lithium ion conductivity in the perovskite solid solution La0.67-xLi3xTiO3 (x=0.11). Journal of Solid State Ionics. 1999;121

On the microstructure analysis of FSW joints of aluminium components made via direct metal laser sintering

NASA Astrophysics Data System (ADS)

Scherillo, Fabio; Astarita, Antonello; di Martino, Daniela; Contaldi, Vincenzo; di Matteo, Luca; di Petta, Paolo; Casarin, Renzo; Squillace, Antonino; Langella, Antonio

2017-10-01

Additive Manufacturing (AM), applied to metal industry, is a family of processes that allow complex shape components to be realized from raw materials in the form of powders. The compaction of the powders can be achieved by local melting of the powder bed or by solid state sintering. Direct Metal Laser Sintering (DMLS) is an additive manufacturing process in which a focalized laser beam is the heat source that allows the powders to be compacted. By DMLS it is possible to realize complex shape components. One of the limits of DMLS, as for every additive layer manufacturing techniques, is the unfeasibility to realize large dimension parts. Due to this limit the study of joining process of parts made via ALM is of great interest. One of the most promising options is the Friction Stir Welding (FSW), a solid state welding technique that has been proven to be very effective in the welding of metals difficult to weld, above all aluminium alloys. Since FSW is a solid-state technique, the microstructure of the various zone of the weld bead depends not only by the process itself but also by the parent microstruct ure of the parts to be welded. Furthermore, parts made of aluminium alloy via DMLS have a particular microstructure that is the result of repeated severe thermal cycles. In the present work the authors, starting from the description of the parent microstructure of parts made of AlSi10Mg aluminium alloy, study the microstructure evolution occurred within the joint made by Friction Stir Welding, analysing in details the microstructure of the main well recognized zone of the weld bead. The structure of the parent material is characterized by the presence of melting pools with a very fine microstructure. In the joint the recrystallization, the grain refinement and, above all, the redistribution of intermetallic phases occurs, resulting in an homogenization of the microstructure and in an increase of micro hardness.

Effect of microwave-assisted sintering on dielectric properties of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rani, Suman, E-mail: sumanranigju@gmail.com; Ahlawat, Neetu; Punia, R.

2016-05-23

In this present work, CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It wasmore » observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.« less

TOPICAL REVIEW: Sintering and microstructure of ice: a review

NASA Astrophysics Data System (ADS)

Blackford, Jane R.

2007-11-01

Sintering of ice is driven by the thermodynamic requirement to decrease surface energy. The structural morphology of ice in nature has many forms—from snowflakes to glaciers. These forms and their evolution depend critically on the balance between the thermodynamic and kinetic factors involved. Ice is a crystalline material so scientific understanding and approaches from more conventional materials can be applied to ice. The early models of solid state ice sintering are based on power law models originally developed in metallurgy. For pressure sintering of ice, these are based on work on hot isostatic pressing of metals and ceramics. Recent advances in recognizing the grain boundary groove geometry between sintering ice particles require models that use new approaches in materials science. The newer models of sintering in materials science are beginning to incorporate more realistic processing conditions and microstructural complexity, and so there is much to be gained from applying these to ice in the future. The vapour pressure of ice is high, which causes it to sublime readily. The main mechanism for isothermal sintering of ice particles is by vapour diffusion; however other transport mechanisms certainly contribute. Plastic deformation with power law creep combined with recrystallization become important mechanisms in sintering with external pressure. Modern experimental techniques, low temperature scanning electron microscopy and x-ray tomography, are providing new insights into the evolution of microstructures in ice. Sintering in the presence of a small volume fraction of the liquid phase causes much higher bond growth rates. This may be important in natural snow which contains impurities that form a liquid phase. Knowledge of ice microstructure and sintering is beneficial in understanding mechanical behaviour in ice friction and the stability of snow slopes prone to avalanches.

Correlation of Intermolecular Acyl Transfer Reactivity with Noncovalent Lattice Interactions in Molecular Crystals: Toward Prediction of Reactivity of Organic Molecules in the Solid State.

PubMed

Krishnaswamy, Shobhana; Shashidhar, Mysore S

2018-04-06

Intermolecular acyl transfer reactivity in several molecular crystals was studied, and the outcome of the reactivity was analyzed in the light of structural information obtained from the crystals of the reactants. Minor changes in the molecular structure resulted in significant variations in the noncovalent interactions and packing of molecules in the crystal lattice, which drastically affected the facility of the intermolecular acyl transfer reactivity in these crystals. Analysis of the reactivity vs crystal structure data revealed dependence of the reactivity on electrophile···nucleophile interactions and C-H···π interactions between the reacting molecules. The presence of these noncovalent interactions augmented the acyl transfer reactivity, while their absence hindered the reactivity of the molecules in the crystal. The validity of these correlations allows the prediction of intermolecular acyl transfer reactivity in crystals and co-crystals of unknown reactivity. This crystal structure-reactivity correlation parallels the molecular structure-reactivity correlation in solution-state reactions, widely accepted as organic functional group transformations, and sets the stage for the development of a similar approach for reactions in the solid state.

Compression Molding and Novel Sintering Treatments for Alnico Type-8 Permanent Magnets in Near-Final Shape with Preferred Orientation

NASA Astrophysics Data System (ADS)

Kassen, Aaron G.; White, Emma M. H.; Tang, Wei; Hu, Liangfa; Palasyuk, Andriy; Zhou, Lin; Anderson, Iver E.

2017-09-01

Economic uncertainty in the rare earth (RE) permanent magnet marketplace, as well as in an expanding electric drive vehicle market that favors permanent magnet alternating current synchronous drive motors, motivated renewed research in RE-free permanent magnets like "alnico," an Al-Ni-Co-Fe alloy. Thus, high-pressure, gas-atomized isotropic type-8H pre-alloyed alnico powder was compression molded with a clean burn- out binder to near-final shape and sintered to density >99% of cast alnico 8 (full density of 7.3 g/cm3). To produce aligned sintered alnico magnets for improved energy product and magnetic remanence, uniaxial stress was attempted to promote controlled grain growth, avoiding directional solidification that provides alignment in alnico 9. Successful development of solid-state powder processing may enable anisotropically aligned alnico magnets with enhanced energy density to be mass-produced.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Hui; Chen, Yan; Hood, Zachary D.

All-solid-state sodium batteries, using abundant sodium resources and solid electrolyte, hold much promise for safe, low cost, large-scale energy storage. To realize the practical applications of all solid Na-ion batteries at ambient temperature, the solid electrolytes are required to have high ionic conductivity, chemical stability, and ideally, easy preparation. Ceramic electrolytes show higher ionic conductivity than polymers, but they often require extremely stringent synthesis conditions, either high sintering temperature above 1000 C or long-time, low-energy ball milling. Herein, we report a new synthesis route for Na 3SbS 4, a novel Na superionic conductor that needs much lower processing temperature belowmore » 200 C and easy operation. This new solid electrolyte exhibits a remarkable ionic conductivity of 1.05 mS cm -1 at 25 °C and is chemically stable under ambient atmosphere. In conclusion, this synthesis process provides unique insight into the current state-of-the-art solid electrolyte preparation and opens new possibilities for the design of similar materials.« less

Optimization of sintering conditions for cerium-doped yttrium aluminum garnet

NASA Astrophysics Data System (ADS)

Cranston, Robert Wesley McEachern

YAG:Ce phosphors have become widely used as blue/yellow light converters in camera projectors, white light emitting diodes (WLEDs) and general lighting applications. Many studies have been published on the production, characterization, and analysis of this optical ceramic but few have been done on determining optimal synthesis conditions. In this work, YAG:Ce phosphors were synthesized through solid state mixing and sintering. The synthesized powders and the highest quality commercially available powders were pressed and sintered to high densities and their photoluminescence (PL) intensity measured. The optimization process involved the sintering temperature, sintering time, annealing temperature and the level of Ce concentration. In addition to the PL intensity, samples were also characterized using particle size analysis, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The PL data was compared with data produced from a YAG:Ce phosphor sample provided by Christie Digital. The peak intensities of the samples were converted to a relative percentage of this industry product. The highest value for the intensity of the commercial powder was measured for a Ce concentration of 0.3 mole% with a sintering temperature of 1540°C and a sintering dwell time of 7 hours. The optimal processing parameters for the in-house synthesized powder were slightly different from those of commercial powders. The optimal Ce concentration was 0.4 mole% Ce, sintering temperature was 1560°C and sintering dwell time was 10 hours. These optimal conditions produced a relative intensity of 94.20% and 95.28% for the in-house and commercial powders respectively. Polishing of these samples resulted in an increase of 5% in the PL intensity.

Synthesis of azines in solid state: reactivity of solid hydrazine with aldehydes and ketones.

PubMed

Lee, Byeongno; Lee, Kyu Hyung; Cho, Jaeheung; Nam, Wonwoo; Hur, Nam Hwi

2011-12-16

Highly conjugated azines were prepared by solid state grinding of solid hydrazine and carbonyl compounds such as aldehydes and ketones, using a mortar and a pestle. Complete conversion to the azine product is generally achieved at room temperature within 24 h, without using solvents or additives. The solid-state reactions afford azines as the sole products with greater than 97% yield, producing only water and carbon dioxide as waste.

Methods of flash sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raj, Rishi; Cologna, Marco; Francis, John S.

2016-05-10

This disclosure provides methods of flash sintering and compositions created by these methods. Methods for sintering multilayered bodies are provided in which a sintered body is produced in less than one minute. In one aspect, each layer is of a different composition, and may be constituted wholly from a ceramic or from a combination of ceramic and metallic particles. When the body includes a layer of an anode composition, a layer of an electrolyte composition and a layer of a cathode composition, the sintered body can be used to produce a solid oxide fuel cell.

Thermoelectric Properties of Hot-Pressed and PECS-Sintered Magnesium-Doped Copper Aluminum Oxide

NASA Astrophysics Data System (ADS)

Liu, Chang; Morelli, Donald T.

2011-05-01

Copper aluminum oxide (CuAlO2) is considered as a potential candidate for thermoelectric applications. Partially magnesium-doped CuAlO2 bulk pellets were fabricated using solid-state reactions, hot-pressing, and pulsed electric current sintering (PECS) techniques. X-ray diffraction and scanning electron microscopy were adopted for structural analysis. High-temperature transport property measurements were performed on hot-pressed samples. Electrical conductivity increased with Mg doping before secondary phases became significant, while the Seebeck coefficient displayed the opposite trend. Thermal conductivity was consistently reduced as the Mg concentration increased. Effects of Mg doping, preparation conditions, and future modification on this material's properties are discussed.

One Step Combustion Synthesis Of YAG:Ce Phosphor For Solid State Lighting

NASA Astrophysics Data System (ADS)

Yadav, Pooja; Gupta, K. Vijay Kumar; Muley, Aarti; Joshi, C. P.; Moharil, S. V.

2011-10-01

YAG:Ce is an important phosphor having applications in various fields ranging from solid state lighting to scintillation detectors. YAG phosphors doped with activators are mainly synthesized by solid state reaction techniques that require high sintering temperatures (above 1500°C) to eliminate YAM and YAP phases. Though several soft chemical routes have been explored for synthesis of YAG, most of these methods are complex and phase pure materials are not obtained in one step, but prolonged annealing at temperatures around 1000 C or above becomes necessary. One step combustion synthesis of YAG:Ce3+ and related phosphors carried out at 500 C furnace temperature is reported here. Activation with Ce3+ could be achieved during the synthesis without taking recourse to any post-combustion thermal treatment. LEDs prepared from the combustion synthesized YAG:Ce3+, exhibited properties comparable to those produced from the commercial phosphor.

Single-phase ceramics with La 1- xSr xGa 1- yMg yO 3- δ composition from precursors obtained by mechanosynthesis

NASA Astrophysics Data System (ADS)

Moure, A.; Castro, A.; Tartaj, J.; Moure, C.

Dense ceramics with La 0.80Sr 0.20Ga 0.85Mg 0.15O 2.825 and La 0.80Sr 0.15Ga 0.85Mg 0.20O 2.825 compositions have been prepared by sintering of mechanosynthesized precursors. The perovskite is synthesized after 85 h of milling in a planetary mill. Single phases have been obtained at conditions that are not possible if traditional solid-state reaction (SSR) method is used. The influence of milling time and composition in the reactivity of the precursors is studied. Highest purity is obtained in Sr = 0.15 and Mg = 0.20 composition, with relative density higher than 97%. The total elimination of typical secondary phases for these compositions, as SrLaGaO 4 and SrLaGa 3O 7, allows the total conductivity of the ceramics to be improved. The influence of the grain size and the nature of the grain boundaries on the electrical characteristic of the ceramics are also discussed.

Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO₃ Ceramics Fabricated by Spark Plasma Sintering.

PubMed

Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

2017-03-07

Based on precursor powders with a size of 200-300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO₃ ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO₃ ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe 3+ to Fe 2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO₃ ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage.

Peridynamic Theory as a New Paradigm for Multiscale Modeling of Sintering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Silling, Stewart A.; Abdeljawad, Fadi; Ford, Kurtis Ross

2017-09-01

Sintering is a component fabrication process in which powder is compacted by pressing or some other means and then held at elevated temperature for a period of hours. The powder grains bond with each other, leading to the formation of a solid component with much lower porosity, and therefore higher density and higher strength, than the original powder compact. In this project, we investigated a new way of computationally modeling sintering at the length scale of grains. The model uses a high-fidelity, three-dimensional representation with a few hundred nodes per grain. The numerical model solves the peridynamic equations, in whichmore » nonlocal forces allow representation of the attraction, adhesion, and mass diffusion between grains. The deformation of the grains is represented through a viscoelastic material model. The project successfully demonstrated the use of this method to reproduce experimentally observed features of material behavior in sintering, including densification, the evolution of microstructure, and the occurrence of random defects in the sintered solid.« less

Na3Si2Y0.16Zr1.84PO12-ionic liquid hybrid electrolytes: An approach for realizing solid-state sodium-ion batteries?

NASA Astrophysics Data System (ADS)

de la Torre-Gamarra, Carmen; Appetecchi, Giovanni Battista; Ulissi, Ulderico; Varzi, Alberto; Varez, Alejandro; Passerini, Stefano

2018-04-01

Ceramic electrolytes are prepared through sintering processes which are carried out at high temperatures and require prolonged operating times, resulting unwelcome in industrial applications. We report a physicochemical characterization on hybrid, sodium conducting, electrolyte systems obtained by coating NASICON ceramic powders with the N-butyl-N-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide ionic liquid. The goal is to realize a ceramic-IL interface with improved sodium mobility, aiming to obtain a solid electrolyte with high ion transport properties but avoiding sintering thermal treatment. The purpose of the present work, however, is showing how simply combining NASICON powder and Py14TFSI does not lead to any synergic effect on the resulting hybrid electrolyte, evidencing that an average functionalization of the ceramic powder surface and/or ionic liquid is needed. Also, the processing conditions for preparing the hybrid samples are found to affect their ion transport properties.

Spatially Resolved Quantification of the Surface Reactivity of Solid Catalysts.

PubMed

Huang, Bing; Xiao, Li; Lu, Juntao; Zhuang, Lin

2016-05-17

A new property is reported that accurately quantifies and spatially describes the chemical reactivity of solid surfaces. The core idea is to create a reactivity weight function peaking at the Fermi level, thereby determining a weighted summation of the density of states of a solid surface. When such a weight function is defined as the derivative of the Fermi-Dirac distribution function at a certain non-zero temperature, the resulting property is the finite-temperature chemical softness, termed Fermi softness (SF ), which turns out to be an accurate descriptor of the surface reactivity. The spatial image of SF maps the reactive domain of a heterogeneous surface and even portrays morphological details of the reactive sites. SF analyses reveal that the reactive zones on a Pt3 Y(111) surface are the platinum sites rather than the seemingly active yttrium sites, and the reactivity of the S-dimer edge of MoS2 is spatially anisotropic. Our finding is of fundamental and technological significance to heterogeneous catalysis and industrial processes demanding rational design of solid catalysts. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Key parameters governing the densification of cubic-Li7La3Zr2O12 Li+ conductors

NASA Astrophysics Data System (ADS)

Yi, Eongyu; Wang, Weimin; Kieffer, John; Laine, Richard M.

2017-06-01

Cubic-Li7La3Zr2O12 (LLZO) is regarded as one of the most promising solid electrolytes for the construction of inherently safe, next generation all-solid-state Li batteries. Unfortunately, sintering these materials to full density with controlled grain sizes, mechanical and electrochemical properties relies on energy and equipment intensive processes. In this work, we elucidate key parameters dictating LLZO densification by tracing the compositional and structural changes during processing calcined and ball-milled Al3+ doped LLZO powders. We find that the powders undergo ion (Li+/H+) exchange during room temperature processing, such that on heating, the protonated LLZO lattice collapses and crystallizes to its constituent oxides, leading to reaction driven densification at < 1000 °C, prior to sintering of LLZO grains at higher temperatures. It is shown that small particle sizes and protonation cannot be decoupled, and actually aid densification. We conclude that using fully decomposed nanoparticle mixtures, as obtained by liquid-feed flame spray pyrolysis, provides an ideal approach to use high surface and reaction energy to drive densification, resulting in pressureless sintering of Ga3+ doped LLZO thin films (25 μm) at 1130 °C/0.3 h to ideal microstructures (95 ± 1% density, 1.2 ± 0.2 μm average grain size) normally accessible only by pressure-assisted sintering. Such films offer both high ionic conductivity (1.3 ± 0.1 mS cm-1) and record low ionic area specific resistance (2 Ω cm2).

Preparation and properties of a MnCo2O4 for ceramic interconnect of solid oxide fuel cell via glycine nitrate process

NASA Astrophysics Data System (ADS)

Yoon, Mi Young; Lee, Eun Jung; Song, Rak Hyun; Hwang, Hae Jin

2011-12-01

MnCo2O4 powder was prepared by a wet chemistry method using metal nitrates and glycine in an aqueous solution. The phase stability, sintering behavior, thermal expansion and electrical conductivity were examined to characterize powder suitability as an interconnect material in solid oxide fuel cells (SOFCs). X-ray diffraction indicated that the MnCo2O4 spinel synthesized by the glycine nitrate process was stable until 1100 °C and it was possible to obtain a fully densified single phase spinel. On the other hand, the MnCo2O4 synthesized by a solid state reaction decomposed into a cubic spinel and CoO after being sintered at 1100 °C. This might be associated with the reduction of Co3+ in the octahedral site of the cubic spinel phase. MnCo2O4 showed a thermal expansion coefficient comparable to that of other SOFCs components, as well as good electrical conductivity. Therefore, MnCo2O4 is a potential candidate for the ceramic interconnects in SOFCs, provided the phase instability under reducing environments can be improved.

Processing of solid solution, mixed uranium/refractory metal carbides for advanced space nuclear power and propulsion systems

NASA Astrophysics Data System (ADS)

Knight, Travis Warren

Nuclear thermal propulsion (NTP) and space nuclear power are two enabling technologies for the manned exploration of space and the development of research outposts in space and on other planets such as Mars. Advanced carbide nuclear fuels have been proposed for application in space nuclear power and propulsion systems. This study examined the processing technologies and optimal parameters necessary to fabricate samples of single phase, solid solution, mixed uranium/refractory metal carbides. In particular, the pseudo-ternary carbide, UC-ZrC-NbC, system was examined with uranium metal mole fractions of 5% and 10% and corresponding uranium densities of 0.8 to 1.8 gU/cc. Efforts were directed to those methods that could produce simple geometry fuel elements or wafers such as those used to fabricate a Square Lattice Honeycomb (SLHC) fuel element and reactor core. Methods of cold uniaxial pressing, sintering by induction heating, and hot pressing by self-resistance heating were investigated. Solid solution, high density (low porosity) samples greater than 95% TD were processed by cold pressing at 150 MPa and sintering above 2600 K for times longer than 90 min. Some impurity oxide phases were noted in some samples attributed to residual gases in the furnace during processing. Also, some samples noted secondary phases of carbon and UC2 due to some hyperstoichiometric powder mixtures having carbon-to-metal ratios greater than one. In all, 33 mixed carbide samples were processed and analyzed with half bearing uranium as ternary carbides of UC-ZrC-NbC. Scanning electron microscopy, x-ray diffraction, and density measurements were used to characterize samples. Samples were processed from powders of the refractory mono-carbides and UC/UC 2 or from powders of uranium hydride (UH3), graphite, and refractory metal carbides to produce hypostoichiometric mixed carbides. Samples processed from the constituent carbide powders and sintered at temperatures above the melting point of UC showed signs of liquid phase sintering and were shown to be largely solid solutions. Pre-compaction of mixed carbide powders prior to sintering was shown to be necessary to achieve high densities. Hypostoichiometric, samples processed at 2500 K exhibited only the initial stage of sintering and solid solution formation. Based on these findings, a suggested processing methodology is proposed for producing high density, solid solution, mixed carbide fuels. Pseudo-binary, refractory carbide samples hot pressed at 3100 K and 6 MPa showed comparable densities (approximately 85% of the theoretical value) to samples processed by cold pressing and sintering at temperatures of 2800 K.

Silicon nitride-aluminum oxide solid solution (SiAION) formation and densification by pressure sintering

NASA Technical Reports Server (NTRS)

Yeh, H. C.; Sanders, W. A.; Fiyalko, J. L.

1975-01-01

Stirred-ball-mill-blended Si3N4 and Al2O3 powders were pressure sintered in order to investigate the mechanism of solid solution formation and densification in the Si3N4-Al2O3 system. Powder blends with Si3N4:Al2O3 mole ratios of 4:1, 3:2, and 2:3 were pressure sintered at 27.6-MN/sq m pressure at temperatures to 17000 C (3090 F). The compaction behavior of the powder blends during pressure sintering was determined by observing the density of the powder compact as a function of temperature and time starting from room temperature. This information, combined with the results of X-ray diffraction and metallographic analyses regarding solutioning and phase transformation phenomena in the Si3N4-Al2O3 system, was used to describe the densification behavior.

Infiltration sintering properties of Ni-4B-4Si(wt.%) alloy powders

NASA Astrophysics Data System (ADS)

Yang, Q.; Zhang, X. C.; Wang, F. L.; Zou, J. T.

2018-01-01

The Ni-4B-4Si(wt.%) alloy powders were infiltrated into the nickel skeletons, the effects of sintering temperatures (1050-1150 °C) and skeletons (loose and compact nickel powders) on the microstructures and hardness of the sintered alloys were investigated. The Ni-B-Si alloy sintered at 1100 °C consisted of γ-Ni and Ni3B, and Si mainly solid soluted in the γ-Ni. The loose nickel powders favored to the infiltration of Ni-B-Si liquid alloy into the nickel skeletons, the sintered alloys exhibited dense microstructures and good interfacial bonding with Ni substrates. The interfacial hardness was equal to that of the sintered alloys and Ni substrates. Loose nickel powders ensured the density and interfacial bonding of the sintered alloys, the infiltration sintering process can be simplified and easily applied to practice.

Pore Formation Process of Porous Ti3SiC2 Fabricated by Reactive Sintering

PubMed Central

Zhang, Huibin; Liu, Xinli; Jiang, Yao

2017-01-01

Porous Ti3SiC2 was fabricated with high purity, 99.4 vol %, through reactive sintering of titanium hydride (TiH2), silicon (Si) and graphite (C) elemental powders. The reaction procedures and the pore structure evolution during the sintering process were systematically studied by X-ray diffraction (XRD) and scanning electron microscope (SEM). Our results show that the formation of Ti3SiC2 from TiH2/Si/C powders experienced the following steps: firstly, TiH2 decomposed into Ti; secondly, TiC and Ti5Si3 intermediate phases were generated; finally, Ti3SiC2 was produced through the reaction of TiC, Ti5Si3 and Si. The pores formed in the synthesis procedure of porous Ti3SiC2 ceramics are derived from the following aspects: interstitial pores left during the pressing procedure; pores formed because of the TiH2 decomposition; pores formed through the reactions between Ti and Si and Ti and C powders; and the pores produced accompanying the final phase synthesized during the high temperature sintering process. PMID:28772515

Development of a sintering process for recycling oil shale fly ash and municipal solid waste incineration bottom ash into glass ceramic composite.

PubMed

Zhang, Zhikun; Zhang, Lei; Li, Aimin

2015-04-01

Oil shale fly ash and municipal solid waste incineration bottom ash are industrial and municipal by-products that require further treatment before disposal to avoid polluting the environment. In the study, they were mixed and vitrified into the slag by the melt-quench process. The obtained vitrified slag was then mixed with various percentages of oil shale fly ash and converted into glass ceramic composites by the subsequent sintering process. Differential thermal analysis was used to study the thermal characteristics and determine the sintering temperatures. X-ray diffraction analysis was used to analyze the crystalline phase compositions. Sintering shrinkage, weight loss on ignition, density and compressive strength were tested to determine the optimum preparation condition and study the co-sintering mechanism of vitrified amorphous slag and oil shale fly ash. The results showed the product performances increased with the increase of sintering temperatures and the proportion of vitrified slag to oil shale fly ash. Glass ceramic composite (vitrified slag content of 80%, oil shale fly ash content of 20%, sintering temperature of 1000 °C and sintering time of 2h) showed the properties of density of 1.92 ± 0.05 g/cm(3), weight loss on ignition of 6.14 ± 0.18%, sintering shrinkage of 22.06 ± 0.6% and compressive strength of 67 ± 14 MPa. The results indicated that it was a comparable waste-based material compared to previous researches. In particular, the energy consumption in the production process was reduced compared to conventional vitrification and sintering method. Chemical resistance and heavy metals leaching results of glass ceramic composites further confirmed the possibility of its engineering applications. Copyright © 2015 Elsevier Ltd. All rights reserved.

Synthesis of Y1BaCu3O(x) superconducting powders by intermediate phase reactions

NASA Technical Reports Server (NTRS)

Moure, C.; Fernandez, J. F.; Tartaj, J.; Recio, P.; Duran, P.

1991-01-01

A procedure for synthesizing Y1Ba2Cu3O(x) by solid state reactions was developed. The method is based on the use of barium compounds, previously synthesized, as intermediate phases for the process. The reaction kinetics of this procedure were established between 860 C and 920 C. The crystal structure and the presence of second phases were studied by means of XRD. The sintering behavior and ceramic parameters were also determined. The orthorhombic type-I structure was obtained on the synthesized bodies after a cooling cycle in an air atmosphere. Superconducting transition took place at 91 K. Sintering densities higher than 95 percent D sub th were attained at temperatures below 940 C.

Melt-Infiltration Process For SiC Ceramics And Composites

NASA Technical Reports Server (NTRS)

Behrendt, Donald R.; Singh, Mrityunjay

1994-01-01

Reactive melt infiltration produces silicon carbide-based ceramics and composites faster and more economically than do such processes as chemical vapor infiltration (CVI), reaction sintering, pressureless sintering, hot pressing, and hot isostatic pressing. Process yields dense, strong materials at relatively low cost. Silicon carbide ceramics and composites made by reactive melt infiltration used in combustor liners of jet engines and in nose cones and leading edges of high-speed aircraft and returning spacecraft. In energy industry, materials used in radiant-heater tubes, heat exchangers, heat recuperators, and turbine parts. Materials also well suited to demands of advanced automobile engines.

From dense monomer salt crystals to CO2 selective microporous polyimides via solid-state polymerization.

PubMed

Unterlass, Miriam M; Emmerling, Franziska; Antonietti, Markus; Weber, Jens

2014-01-14

Fully aromatic polyimides are synthesized via solid-state polymerization of the corresponding monomer salts. The crystal structure of salts shows strong hydrogen bonding of the reactive groups and thereby paves the way for solid-state transformations. The polycondensation yields copies of the initial salt crystallite habits, accompanied by the development of a porosity especially suited for CO2.

Method to synthesize bulk iron nitride

DOE Office of Scientific and Technical Information (OSTI.GOV)

Monson, Todd; Lavernia, Enrique J.; Zheng, Baolong

Bulk iron nitride can be synthesized from iron nitride powder by spark plasma sintering. The iron nitride can be spark plasma sintered at a temperature of less than 600°C. and a pressure of less than 600 MPa, with 400 MPa or less most often being sufficient. High pressure SPS can consolidate dense iron nitrides at a lower temperature to avoid decomposition. The higher pressure and lower temperature of spark discharge sintering avoids decomposition and limits grain growth, enabling enhanced magnetic properties. The method can further comprise synthesis of nanocrystalline iron nitride powders using two-step reactive milling prior to high-pressure sparkmore » discharge sintering.« less

Compression Molding and Novel Sintering Treatments for Alnico Type-8 Permanent Magnets in Near-Final Shape with Preferred Orientation

DOE PAGES

Kassen, Aaron G.; White, Emma M. H.; Tang, Wei; ...

2017-07-14

We present economic uncertainty in the rare earth (RE) permanent magnet marketplace, as well as in an expanding electric drive vehicle market that favors permanent magnet alternating current synchronous drive motors, motivated renewed research in RE-free permanent magnets like “alnico,” an Al-Ni-Co-Fe alloy. Thus, high-pressure, gas-atomized isotropic type-8H pre-alloyed alnico powder was compression molded with a clean burn-out binder to near-final shape and sintered to density >99% of cast alnico 8 (full density of 7.3 g/cm 3). To produce aligned sintered alnico magnets for improved energy product and magnetic remanence, uniaxial stress was attempted to promote controlled grain growth, avoidingmore » directional solidification that provides alignment in alnico 9. Lastly, successful development of solid-state powder processing may enable anisotropically aligned alnico magnets with enhanced energy density to be mass-produced.« less

Low-Temperature Sintering Li3Mg1.8Ca0.2NbO6 Microwave Dielectric Ceramics with LMZBS Glass

NASA Astrophysics Data System (ADS)

Wang, Gang; Zhang, Huaiwu; Liu, Cheng; Su, Hua; Jia, Lijun; Li, Jie; Huang, Xin; Gan, Gongwen

2018-05-01

Li3Mg1.8Ca0.2NbO6 ceramics doped with Li2O-MgO-ZnO-B2O3-SiO2 glass (LMZBS) were prepared via a solid-state route. The LMZBS glass effectively reduced the sintering temperature of Li3Mg1.8Ca0.2NbO6 ceramics to 950°C. The effects of the LMZBS glass on the sintering behavior, microstructures and microwave dielectric properties of Li3Mg1.8Ca0.2NbO6 ceramics are discussed in detail. Among all the LMZBS doped Li3Mg1.8Ca0.2NbO6 ceramics, the sample with 1 wt.% of LMZBS glass sintered at 950°C for 4 h exhibited good dielectric properties: ɛ r = 16.7, Q × f = 31,000 GHz (9.92 GHz), τ f = - 1.3 ppm/°C. The Li3Mg1.8Ca0.2NbO6 ceramics possessed excellent chemical compatibility with Ag electrodes, and could be applied in low temperature co-fired ceramics (LTCC) applications.

Nano-Hydroxyapatite/Fluoridated and Unfluoridated Bioactive Glass Composites: Structural Analysis and Bioactivity Evaluation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Batra, Uma; Kapoor, Seema; Sharma, J. D.

2011-12-12

Biphasic bioceramic composites containing nano-hydroxyapatite (HAP) and nanosized bioactive glasses have been prepared in the form of pellets and have been examined for the effects of bioglass concentrations and sintering temperature on the structural transformations and bioactivity behavior. Pure stoichiometric nano-HAP was synthesized using sol-gel technique. Two bioglasses synthesized in this work--fluoridated bioglass (Cao-P{sub 2}O{sub 5}-Na{sub 2}O{sub 3}-CaF{sub 2}) and unfluoridated bioglass (Cao-P{sub 2}O{sub 5}-Na{sub 2}O{sub 3}) designated as FBG and UFBG respectively, were added to nano-HAP with concentrations of 5, 10, 12 and 15%. The average particle sizes of synthesized HAP and bioglasses were 23 nm and 35 nm,more » respectively. The pellets were sintered at four different temperatures i.e. 1000 deg. C, 1150 deg. C, 1250 deg. C and 1350 deg. C. The investigations involved study of structural and bioactivity behavior of green and sintered pellets and their deviations from original materials i.e. HAP, FBG and UFBG, using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The phase composition of the sintered pellets was found to be non-stoichiometric HAP with {alpha}-TCP (tricalcium phosphate) and {beta}-TCP. It was revealed from SEM images that bonding mechanism was mainly solid state sintering for all pellets sintered at 1000 deg. C and 1150 deg. C and also for pellets with lower concentrations of bioglass i.e. 5% and 10% sintered at 1250 deg. C. Partly liquid phase sintering was observed for pellets with higher bioglass concentrations of 12% and 15% sintered at 1250 deg. C and same behaviour was noted for pellets at all concentrations of bioglasses at 1350 deg. C. The sintered density, hardness and compression strength of pellets have been influenced both by the concentration of the bioglasses and sintering temperature. It was observed that the biological HAP layer formation was faster on the green pellets surface than on pure HAP and sintered pellets, showing higher bioactivity in the green pellets.« less

Effect of Sintering Temperature on Structural, Dielectric, and Magnetic Properties of Multiferroic YFeO3 Ceramics Fabricated by Spark Plasma Sintering

PubMed Central

Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen

2017-01-01

Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO3 ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO3 ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe3+ to Fe2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO3 ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage. PMID:28772626

Developing Cost-Effective Dense Continuous SDC Barrier Layers for SOFCs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nguyen, Hoang Viet P.; Hardy, John S.; Coyle, Christopher A.

Significantly improved performance during electrochemical testing of a cell with a dense continuous pulsed laser deposited (PLD) samarium doped ceria (SDC) layer spurred investigations into the fabrication of dense continuous SDC barrier layers by means of cost-effective deposition using screen printing which is amenable to industrial production of SOFCs. Many approaches to improve the SDC density have been explored including the use of powder with reduced particle sizes, inks with increased solids loading, and doping with sintering aids (1). In terms of sintering aids, dopants like Mo or binary systems of Mo+Cu or Fe+Co greatly enhance SDC sinterability. In fact,more » adding dopants to a screen printed, prefired, porous SDC layer made it possible to achieve a dense continuous barrier layer atop the YSZ electrolyte without sintering above 1200°C. Although the objective of fabricating a dense continuous layer was achieved, additional studies have been initiated to improve the cell performance. Underlying issues with constrained sintering and dopant-enhanced ceria-zirconia solid solubility are also addressed in this paper.« less

An air-stable Na 3SbS 4 superionic conductor prepared by a rapid and economic synthetic procedure

DOE PAGES

Wang, Hui; Chen, Yan; Hood, Zachary D.; ...

2016-01-01

All-solid-state sodium batteries, using abundant sodium resources and solid electrolyte, hold much promise for safe, low cost, large-scale energy storage. To realize the practical applications of all solid Na-ion batteries at ambient temperature, the solid electrolytes are required to have high ionic conductivity, chemical stability, and ideally, easy preparation. Ceramic electrolytes show higher ionic conductivity than polymers, but they often require extremely stringent synthesis conditions, either high sintering temperature above 1000 C or long-time, low-energy ball milling. Herein, we report a new synthesis route for Na 3SbS 4, a novel Na superionic conductor that needs much lower processing temperature belowmore » 200 C and easy operation. This new solid electrolyte exhibits a remarkable ionic conductivity of 1.05 mS cm -1 at 25 °C and is chemically stable under ambient atmosphere. In conclusion, this synthesis process provides unique insight into the current state-of-the-art solid electrolyte preparation and opens new possibilities for the design of similar materials.« less

Synthesis of nanopowders of the aluminum-substituted lanthanum gallate solid electrolyte by mechanochemical route

NASA Astrophysics Data System (ADS)

Domingues, Eddy M.; Gonçalves, Priscila; Figueiredo, Filipe M.

2012-07-01

The room temperature mechanosynthesis of La1-xSrxGa1-y-zMgyAlzO3-δ nanopowders is successfully demonstrated for a broad compositional range (x ≤ 0.1; y ≤ 0.2, z ≤ 0.4) by resorting to a nearly amorphous alumina precursor with enhanced reactivity. It is shown that ceramics with one single phase and free from open porosity can be obtained by sintering these nanopowders at 1350-1450 °C. Microstructural data show that the substitution of Ga by Al hinders densification and decreases the grain size of ceramics. This is explained assuming the segregation of aluminum cations to the grain boundaries as a result of the decrease of the cationic diffusion coefficients.

High-temperature mechanical properties of a solid oxide fuel cell glass sealant in sintered forms

NASA Astrophysics Data System (ADS)

Chang, Hsiu-Tao; Lin, Chih-Kuang; Liu, Chien-Kuo; Wu, Szu-Han

High-temperature mechanical properties of a silicate-based glass sealant (GC-9) for planar solid oxide fuel cell have been studied in sintered forms. Ring-on-ring biaxial flexural tests are carried out at room temperature to 800 °C for the sintered GC-9 glass. The results are also compared with those in cast bulk forms. From the force-displacement curves, the glass transition temperature (T g) of the non-aged, sintered GC-9 glass is estimated to be between 700 °C and 750 °C, while that of the aged one is between 750 °C and 800 °C. Due to a crack healing effect of the residual glass at high temperature, the flexural strength of the sintered GC-9 glass at temperature of 650 °C to T g point is greater than that at room temperature. At temperature above T g, the flexural strength and stiffness are considerably reduced to a level lower than the room-temperature one. The sintered GC-9 glass with pores and crystalline phases has a flexural strength lower than the cast bulk one at temperature of 650 °C and below. Due to a greater extent of crystallization, the flexural strength and stiffness of the sintered GC-9 glass are greater than those of the cast bulk one at 700-800 °C.

Fabrication and spectroscopic properties of Co:MgAl2O4 transparent ceramics by the HIP post-treatment

NASA Astrophysics Data System (ADS)

Luo, Wei; Ma, Peng; Xie, Tengfei; Dai, Jiawei; Pan, Yubai; Kou, Huamin; Li, Jiang

2017-07-01

Cobalt-doped magnesium aluminate spinel (Co:MgAl2O4) is one of the most important saturable absorbers for the passive Q-switching of solid-state lasers operating at eye-safe wavelength of 1.5 μm. In this work, highly transparent Co:MgAl2O4 ceramics were fabricated by vacuum sintering combined with hot isostatic pressing (HIP) post-treatment, using the mixture of the commercial spinel and the lab-made Co:MgAl2O4 powder as the raw materials. The densification mechanism of Co:MgAl2O4 transparent ceramics was discussed. The microstructure and optical properties of the samples were investigated. The ground state absorption cross section (σGSA) was calculated from the fitted curve of the absorption coefficient spectrum. The results show that Co:MgAl2O4 ceramics fabricated by vacuum sintering at 1500 °C for 5 h and then HIP post-treatment at 1650 °C for 3 h perform good transparency, whose in-line transmittance exceeds 80% at 2500 nm. Moreover, the ground state absorption cross section of 0.02 at.% Co:MgAl2O4 ceramics is calculated to be 3.35 × 10-19 cm2 at the wavelength of 1540 nm, which is promising for the application to the passive Q-switching of solid-state laser operating in the near infrared region (NIR).

Effects of PbO-B2O3 Glass Doping on the Sintering Temperature and Piezoelectric Properties of 0.35Pb (Ni1/3Nb2/3)O3-0.65Pb(Zr0.41Ti0.59)O3 Ceramics

NASA Astrophysics Data System (ADS)

Yi, Jinqiao; Shen, Meng; Liu, Sisi; Jiang, Shenglin

2015-12-01

0.35Pb(Ni1/3Nb2/3)O3-0.65Pb(Zr0.41Ti0.59)O3 (PNN-PZT) ceramics doped with 0.5PbO-0.5B2O3 glass have been synthesized by the conventional solid-state sintering technique. The effects of 0.5PbO-0.5B2O3 glass on the sintering temperature and piezoelectric properties of PNN-PZT ceramics were studied. The results indicated that the sintering temperature of PNN-PZT was significantly reduced due to the incorporation of 0.5PbO-0.5B2O3 glass dopant. When the content of 0.5PbO-0.5B2O3 glass was 0.5 wt.%, the sintering temperature of PNN-PZT was observed to reduce from above 1200°C to 920°C while the samples maintained high density (7.91 g/cm3), excellent piezoelectric constant ( d 33 = 479 pC/N), large electromechanical coupling coefficient ( K p = 0.55), and relatively low electromechanical quality factor ( Q m = 79). Moreover, large dielectric constant ( ɛ 33 T / ɛ 0 = 2904) and low dielectric loss (tan δ = 0.0166) were obtained in this work.

Microstructure, Hardness, and Corrosion Behavior of TiC-Duplex Stainless Steel Composites Fabricated by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Han, Ying; Zhang, Wei; Sun, Shicheng; Chen, Hua; Ran, Xu

2017-08-01

Duplex stainless steel composites with various weight fractions of TiC particles are prepared by spark plasma sintering. Ferritic 434L and austenitic 316L stainless steel powders are premixed in a 50:50 weight ratio and added with 3-9 wt.% TiC. The compacts are sintered in the solid state under vacuum conditions at 1223 K for 5 min. The effects of TiC content on the microstructure, hardness, and corrosion resistance of duplex stainless steel composites fabricated by powder metallurgy are evaluated. The results indicate that the TiC particulates as reinforcements can be distributed homogeneously in the steel matrix. Densification of sintered composites decreases with increasing TiC content. M23C6 carbide precipitates along grain boundary, and its neighboring Cr-Mo-depleted region is formed in the sintered microstructure, which can be eliminated subsequently with appropriate heat treatment. With the addition of TiC, the hardness of duplex stainless steel fabricated by powder metallurgy can be markedly enhanced despite increased porosity in the composites. However, TiC particles increase the corrosion rate and degrade the passivation capability, particularly for the composite with TiC content higher than 6 wt.%. Weakened metallurgical bonding in the composite with high TiC content provides the preferred sites for pitting nucleation and/or dissolution.

Reactive Desorption of CO Hydrogenation Products under Cold Pre-stellar Core Conditions

NASA Astrophysics Data System (ADS)

Chuang, K.-J.; Fedoseev, G.; Qasim, D.; Ioppolo, S.; van Dishoeck, E. F.; Linnartz, H.

2018-02-01

The astronomical gas-phase detection of simple species and small organic molecules in cold pre-stellar cores, with abundances as high as ∼10‑8–10‑9 n H, contradicts the generally accepted idea that at 10 K, such species should be fully frozen out on grain surfaces. A physical or chemical mechanism that results in a net transfer from solid-state species into the gas phase offers a possible explanation. Reactive desorption, i.e., desorption following the exothermic formation of a species, is one of the options that has been proposed. In astronomical models, the fraction of molecules desorbed through this process is handled as a free parameter, as experimental studies quantifying the impact of exothermicity on desorption efficiencies are largely lacking. In this work, we present a detailed laboratory study with the goal of deriving an upper limit for the reactive desorption efficiency of species involved in the CO–H2CO–CH3OH solid-state hydrogenation reaction chain. The limit for the overall reactive desorption fraction is derived by precisely investigating the solid-state elemental carbon budget, using reflection absorption infrared spectroscopy and the calibrated solid-state band-strength values for CO, H2CO and CH3OH. We find that for temperatures in the range of 10 to 14 K, an upper limit of 0.24 ± 0.02 for the overall elemental carbon loss upon CO conversion into CH3OH. This corresponds with an effective reaction desorption fraction of ≤0.07 per hydrogenation step, or ≤0.02 per H-atom induced reaction, assuming that H-atom addition and abstraction reactions equally contribute to the overall reactive desorption fraction along the hydrogenation sequence. The astronomical relevance of this finding is discussed.

Characterization of SrCo1.5Ti1.5Fe9O19 hexagonal ferrite synthesized by sol-gel combustion and solid state route

NASA Astrophysics Data System (ADS)

Vinaykumar, R.; Mazumder, R.; Bera, J.

2017-05-01

Co-Ti co-substituted SrM hexagonal ferrite (SrCo1.5Ti1.5Fe9O19) was synthesized by sol-gel combustion and solid state route. The effects of sources of TiO2 raw materials; titanium tetra-isopropoxide (TTIP) and titanyl nitrate (TN) on the phase formation behavior and properties of the ferrite were studied. The thermal decomposition behavior of the gel was studied using TG-DSC. The phase formation behavior of the ferrite was studied by using X-ray powder diffraction and FTIR analysis. Phase formation was comparatively easier in the TN-based sol-gel process. The morphology of powder and sintered ferrite was investigated using scanning electron microscope. Magnetic properties like magnetization, coercivity, permeability, tan δμ and dielectric properties were investigated. The ferrite synthesized by sol-gel based chemical route showed higher saturation magnetization, permeability and permittivity compared to the ferrite synthesized by solid state route.

Development of SiAlON materials

NASA Technical Reports Server (NTRS)

Layden, G. K.

1977-01-01

Cold pressing and sintering techniques were used to produce ceramic bodies in which the major phase was beta prime Si3-Al-O-N4 solid solution. A variety of foreign oxides were used to promote liquid phase sintering, and this resulted in the incorporation of additional solid phases in the ceramic bodies which controlled elevated temperature properties. None of the bodies studied to date exhibited both adequate high temperature mechanical properties and oxidation resistance. Criteria are suggested to guide the formulation of bodies with improved high temperature properties.

Spark plasma sintering of highly dense fine-grained mineral aggregates

NASA Astrophysics Data System (ADS)

Koizumi, S.; Suzuki, T. S.; Sakka, Y.; Hiraga, T.

2017-12-01

To obtain highly dense and fine-grained mineral aggregates, which are suitable for laboratory measurements of their physical and chemical properties, we applied spark plasma sintering (SPS) to synthetic mineral powders and powders originated from naturally derived crystals. SPS is an emerging consolidation technique which has been applied to various metals and ceramics and rarely to geomaterials (e.g., Guignard et al., 2011). The technique uses spark plasma created by a pulse direct current during heat treatment of powders in a graphite die. It has been found that the technique provides better densification with little grain growth during sintering compared to a conventional sintering technique in many materials. To obtain ideal highly dense fine-grained materials, it is essential to prepare starting powders suitable for the sintering and also to find appropriate sintering conditions of applied uniaxial pressures, pulsed current patterns and heating rates. We prepared synthetic mineral powers through solid state reaction of source powders at high temperature well developed by our group (Koizumi et al. 2010). We also used jet milling at wet condition and subsequent elutriation to prepare olivine powders with sub-micron particle size and equiaxed particle shape. At heating rate of ≦10°C/min and an achievement of highest temperature of 1150°C, Fe-free olivine aggregate with average grain size of 200 nm with porosity of 0.003% was obtained. We also could obtain olivine aggregate, which was sintered from powders of Horoman peridotite, with average grain size of 500 nm and porosity of 0.2%. We will show results of other minerals including major rock forming minerals of the Earth's crust.

High temperature resistant cermet and ceramic compositions

NASA Technical Reports Server (NTRS)

Phillips, W. M. (Inventor)

1978-01-01

Cermet compositions having high temperature oxidation resistance, high hardness and high abrasion and wear resistance, and particularly adapted for production of high temperature resistant cermet insulator bodies are presented. The compositions are comprised of a sintered body of particles of a high temperature resistant metal or metal alloy, preferably molybdenum or tungsten particles, dispersed in and bonded to a solid solution formed of aluminum oxide and silicon nitride, and particularly a ternary solid solution formed of a mixture of aluminum oxide, silicon nitride and aluminum nitride. Also disclosed are novel ceramic compositions comprising a sintered solid solution of aluminum oxide, silicon nitride and aluminum nitride.

NiFe2O4 Spinel Protection Coating for High-Temperature Solid Oxide Fuel Cell Interconnect Application

NASA Astrophysics Data System (ADS)

Irankhah, Reza; Raissi, Babak; Maghsoudipour, Amir; Irankhah, Abdullah; Ghashghai, Sasan

2016-04-01

In the present study, Ni-Fe spinel powder was synthesized via a solid state reaction. In the next step, the electrophoretic deposition (EPD) method was used to apply the NiFe2O4 spinel, as an oxidation-resistant layer, on a commercially available stainless steel (SUS 430) in a potential range of 100 to 300 V. Microscopic studies of the deposited layers showed that crack-free NiFe2O4 films were obtained at 100 V. The coated and uncoated samples were then pre-sintered in air and 5% H2 bal Ar atmospheres at 900 °C for 3 h followed by cyclic oxidation at 800 °C for 500 h. The investigation of the oxidation resistance of the samples using Energy Dispersive Spectroscopy (EDS) revealed that the NiFe2O4 coating acted as an effective barrier against chromium migration into the coating. The oxidation resistance of 5% H2 bal Ar pre-sintered sample was enhanced with an oxidation rate constant ( K P) of 8.9 × 10-15 g2 cm-4 s-1.

Electric Properties of Pb(Sb1/2Nb1/2)O3 PbTiO3 PbZrO3 Ceramics

NASA Astrophysics Data System (ADS)

Kawamura, Yasushi; Ohuchi, Hiromu

1994-09-01

Solid-solution ceramics of ternary system xPb(Sb1/2Nb1/2)O3 yPbTiO3 zPbZrO3 were prepared by the solid-state reaction of powder materials. Ceramic, electric, dielectric and piezoelectric properties and crystal structures of the system were studied. Sintering of the system xPb(Sb1/2Nb1/2)O3 yPbTiO3 zPbZrO3 is much easier than that of each end composition, and well-sintered high-density ceramics were obtained for the compositions near the morphotropic transformation. Piezoelectric ceramics with high relative dielectric constants, high radial coupling coefficient and low resonant resistance were obtained for the composition near the morphotropic transformation. The composition Pb(Sb1/2Nb1/2)0.075Ti0.45Zr0.475O3 showed the highest dielectric constant (ɛr=1690), and the composition Pb(Sb1/2Nb1/2)0.05Ti0.45Zr0.5O3 showed the highest radial coupling coefficient (kp=64%).

Structural and low temperature dielectric studies on Pb0.8Bi0.2Fe0.6Nb0.4O3 multiferroic solid solution

NASA Astrophysics Data System (ADS)

Dadami, Sunanda T.; Matteppanvar, Shidaling; Shivaraja, I.; Rayaprol, Sudhindra; Deshapande, S. K.; Angadi, Basavaraj

2018-05-01

In this paper the structural and low temperature dielectric properties of Pb0.8Bi0.2Fe0.6Nb0.4O3 (PBFNO) multiferroic solid solution were reported. PBFNO multiferroic was synthesized by single step solid state reaction method. Calcination was carried out at 700 °/2hr with different sintering temperature (800 °C, 850 °C, 900 °C, 950 °C, 1000 °C and 1050 °C for 1 hr) and time duration (800 °C for 1 to 5 hr). Single phase was confirmed through room temperature (RT) X-ray Diffraction (XRD). It was found that sintering carried out at 800°C/3 hr gives single phase. Rietveld refined lattice parameters using monoclinic structure are: a = 5.6663(1) Å, b = 5.6694(1) Å, c = 4.0112(1) Å and β = 90.038(1)° with the average grain size as 2.987 µm. The dielectric properties studied over a wide range of frequency (100 Hz - 5 MHz) and temperature (133 K - 293 K). Dielectric constant and loss tangent exhibits frequency dispersion nature at low frequency region. AC conductivity increases with increase in temperature corresponds to negative temperature coefficient of resistance (NTCR) behaviour.

Effect of ca+2 addition on the properties of ce0.8gd0.2o2-δ for it-sofc

NASA Astrophysics Data System (ADS)

Koteswararao, P.; Buchi Suresh, M.; Wani, B. N.; Bhaskara Rao, P. V.; Varalaxmi, P.

2018-03-01

This paper reports the effect of Ca2+ addition on the structural and electrical properties of Ce0.8Gd0.2O2-δ(GDC) electrolyte for low temperature solid oxide fuel cell application. The Ca (0, 0.5, 1 and 2 mol %) doped GDC solid electrolytes have been prepared by solid state method. The sintered densities of the samples are greater than 95%. XRD study reveals the cubic fluorite structure. The microstructure of the samples sintered at 1400°C resulted into grain sizes in the range of 1.72 to 10.20 μm. Raman spectra show the presence of GDC single phase. AC impedance analysis is used to measure the ionic conductivity of the electrolyte. Among all the compositions, the highest conductivity is observed in the GDC sample with 0.5 mol% Ca addition. Nyquist plots resulted in multiple redoxation process such as grain and grain boundary conductions to final conductivity. Estimated blocking factor is lower for the GDC electrolyte with 0.5mol% Ca, indicating that Ca addition was promoted grain boundary conduction. Activation energies were calculated from Arrhenius plot and are found in the range of 1eV.

Densification of LSGM electrolytes using activated microwave sintering

NASA Astrophysics Data System (ADS)

Kesapragada, S. V.; Bhaduri, S. B.; Bhaduri, S.; Singh, P.

Lanthanum gallate doped with alkaline rare earths (LSGM) powders were densified using an activated microwave sintering process for developing a dense stable electrolyte layer for applications in intermediate temperature-solid oxide fuel cells (IT-SOFCs). Due to heat generation in situ, the process of sintering gets activated with faster kinetics compared to a conventional sintering process. The effect of various microwave process parameters on the microstructure and phase formation was studied. The sintered pellets were characterized using scanning electron microscopy-energy dispersive analysis (SEM-EDAX), and X-ray diffraction (XRD). The density of LSGM pellets microwave sintered at 1350 °C for 20 min is greater than 95% theoretical density with a fine grained microstructure (˜2-3 μm) and without the presence of other phase(s).

Physical properties of inorganic PMW-PNN-PZT ceramics

NASA Astrophysics Data System (ADS)

Sin, Sang-Hoon; Yoo, Ju-hyun; Kim, Yong-Jin; Baek, Sam-ki; Ha, Jun-Soo; No, Chung-Han; Song, Hyun-Seon; Shin, Dong-Chan

2015-07-01

In this work, inorganic Pb(Mg1/2W1/2)0.03(Ni1/3Nb2/3)x(Zr0.5Ti0.5)0.97-xO3 (x = 0.02 ∼ 0.12) composition ceramics were fabricated by the conventional solid state reaction method. And then their micro structure and ferroelectric properties were investigated according to the amount of PNN substitution. Small amounts of Li2CO3 and CaCO3 were used in order to decrease the sintering temperature of the ceramics. The 0.10 mol PNN-substituted PMW-PNN- PZT ceramics sintered at 920°C showed the excellent physical properties of piezoelectric constant (d33), electromechanical coupling factor (kp), mechanical quality coefficient (Qm), and dielectric constant of 566 pC/N, 0.61, 73, and 2183, respectively.

End-Member Formulation of Solid Solutions and Reactive Transport

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lichtner, Peter C.

2015-09-01

A model for incorporating solid solutions into reactive transport equations is presented based on an end-member representation. Reactive transport equations are solved directly for the composition and bulk concentration of the solid solution. Reactions of a solid solution with an aqueous solution are formulated in terms of an overall stoichiometric reaction corresponding to a time-varying composition and exchange reactions, equivalent to reaction end-members. Reaction rates are treated kinetically using a transition state rate law for the overall reaction and a pseudo-kinetic rate law for exchange reactions. The composition of the solid solution at the onset of precipitation is assumed tomore » correspond to the least soluble composition, equivalent to the composition at equilibrium. The stoichiometric saturation determines if the solid solution is super-saturated with respect to the aqueous solution. The method is implemented for a simple prototype batch reactor using Mathematica for a binary solid solution. Finally, the sensitivity of the results on the kinetic rate constant for a binary solid solution is investigated for reaction of an initially stoichiometric solid phase with an undersaturated aqueous solution.« less

Mathematical model of the stack region of a commercial lead blast furnace

NASA Astrophysics Data System (ADS)

Hussain, Mansoor M.; Morris, David R.

1989-02-01

A mathematical model of the stack region of a commercial lead blast furnace is presented. The mass and heat balance equations were solved in conjunction with the kinetic expression for the rate of re-duction of the solids based upon the grain model, utilizing the measured structural parameters of the sinter feed and the measured kinetic parameters. Satisfactory agreement has been achieved between the computed and experimental axial profiles of gas and solids temperature, pressure, gas composi-tion, and condensed phases composition. The model is used to predict the effects of changes of bed voidage, physical properties, and chemical constitution of the sinter and the effects of gas and solids flow maldistribution on the operation of the furnace. In particular, it is noted that for a sinter with the typical physical properties of a commercial sinter, improved conversion in the upper reaches of the furnace is predicted when lead is in the form of lead oxide rather than as the relatively unreac-tive lead calcium silicates. The improved conversion is accompanied by better utilization of carbon monoxide. Further, the model suggests that the formation of scaffolds in the furnace may be due to flow maldistribution causing high temperatures in the vicinity of the furnace wall.

A method for phenomenological and chemical kinetics study of autocatalytic reactive dissolution by optical microscopy. The case of uranium dioxide dissolution in nitric acid media

NASA Astrophysics Data System (ADS)

Marc, Philippe; Magnaldo, Alastair; Godard, Jérémy; Schaer, Éric

2018-03-01

Dissolution is a milestone of the head-end of hydrometallurgical processes, as the stabilization rates of the chemical elements determine the process performance and hold-up. This study aims at better understanding the chemical and physico-chemical phenomena of uranium dioxide dissolution reactions in nitric acid media in the Purex process, which separates the reusable materials and the final wastes of the spent nuclear fuels. It has been documented that the attack of sintering-manufactured uranium dioxide solids occurs through preferential attack sites, which leads to the development of cracks in the solids. Optical microscopy observations show that in some cases, the development of these cracks leads to the solid cleavage. It is shown here that the dissolution of the detached fragments is much slower than the process of the complete cleavage of the solid, and occurs with no disturbing phenomena, like gas bubbling. This fact has motivated the measurement of dissolution kinetics using optical microscopy and image processing. By further discriminating between external resistance and chemical reaction, the "true" chemical kinetics of the reaction have been measured, and the highly autocatalytic nature of the reaction confirmed. Based on these results, the constants of the chemical reactions kinetic laws have also been evaluated.

Enery Efficient Press and Sinter of Titanium Powder for Low-Cost Components in Vehicle Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas Zwitter; Phillip Nash; Xiaoyan Xu

2011-03-31

This is the final technical report for the Department of Energy NETL project NT01931 Energy Efficient Press and Sinter of Titanium Powder for Low-Cost Components in Vehicle Applications. Titanium has been identified as one of the key materials with the required strength that can reduce the weight of automotive components and thereby reduce fuel consumption. Working with newly developed sources of titanium powder, Webster-Hoff will develop the processing technology to manufacture low cost vehicle components using the single press/single sinter techniques developed for iron based powder metallurgy today. Working with an automotive or truck manufacturer, Webster-Hoff will demonstrate the feasibilitymore » of manufacturing a press and sinter titanium component for a vehicle application. The project objective is two-fold, to develop the technology for manufacturing press and sinter titanium components, and to demonstrate the feasibility of producing a titanium component for a vehicle application. The lowest cost method for converting metal powder into a net shape part is the Powder Metallurgy Press and Sinter Process. The method involves compaction of the metal powder in a tool (usually a die and punches, upper and lower) at a high pressure (up to 60 TSI or 827 MPa) to form a green compact with the net shape of the final component. The powder in the green compact is held together by the compression bonds between the powder particles. The sinter process then converts the green compact to a metallurgically bonded net shape part through the process of solid state diffusion. The goal of this project is to expand the understanding and application of press and sinter technology to Titanium Powder applications, developing techniques to manufacture net shape Titanium components via the press and sinter process. In addition, working with a vehicle manufacturer, demonstrate the feasibility of producing a titanium component for a vehicle. This is not a research program, but rather a project to develop a process for press and sinter of net shape Titanium components. All of these project objectives have been successfully completed.« less

Fluorine lubricated bearing technology

NASA Technical Reports Server (NTRS)

Mallaire, F. R.

1973-01-01

An experimental program was conducted to evaluate and select materials for ball bearings intended for use in liquid fluorine and/or FLOX. The ability of three different ball-separator materials, each containing nickel, to form and transfer a nickel fluoride film to provide effective lubrication at the required areas of a ball bearing operating in liquid fluorine was evaluated. In addition, solid lubrication of a ball bearing operating in liquid fluorine by either a fused fluoride coating applied to all surfaces of the ball separator or by a fluoride impregnation of porous sintered material ball separators was evaluated. Less bearing wear occurred when tests were conducted in the less reactive FLOX. Bearings fabricated from any of the materials tested would have relatively short wear lives and would require frequent replacement in a reusable engine.

The Development of a Ti-6Al-4V Alloy via Oxygen Solid Solution Strengthening for Aerospace and Defense Applications

DTIC Science & Technology

2013-03-01

latter strategy. Mixtures of titanium powders and TiO2 particles were employed as starting materials and consolidated by spark - plasma sintering and...were consolidated in a carbon container installed in the spark - plasma sintering (SPS) equipment under vacuum condition (ɞ Pa) at a temperature of...evaluation of tensile properties of the wrought pure titanium materials consolidated by sintering and hot extrusion process, a theoretical approach using

Solid-state structure of a Li/F carbenoid: pentafluoroethyllithium.

PubMed

Waerder, Benedikt; Steinhauer, Simon; Neumann, Beate; Stammler, Hans-Georg; Mix, Andreas; Vishnevskiy, Yury V; Hoge, Berthold; Mitzel, Norbert W

2014-10-20

Lithium carbenoids are versatile compounds for synthesis owing to their intriguing ambiphilic behavior. Although this class of compounds has been known for several years, few solid-state structures exist because of their high reactivity and often low thermal stability. Using cryo X-ray techniques, we were now able to elucidate the first solid-state structure of a Li/F alkyl carbenoid, pentafluoroethyllithium (LiC2F5), finally yielding a prototype for investigating structure-reactivity relationships for this class of molecules. The compound forms a diethyl ether-solvated dimer bridged by a rare C-F-Li link. Complementary NMR spectroscopy studies in solution show dynamic processes and indicate rapid exchange of starting material and product. Theoretical investigations help to understand the formation of the observed unusual structural motif. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Aluminum powder metallurgy processing

NASA Astrophysics Data System (ADS)

Flumerfelt, Joel Fredrick

In recent years, the aluminum powder industry has expanded into non-aerospace applications. However, the alumina and aluminum hydroxide in the surface oxide film on aluminum powder require high cost powder processing routes. A driving force for this research is to broaden the knowledge base about aluminum powder metallurgy to provide ideas for fabricating low cost aluminum powder components. The objective of this dissertation is to explore the hypothesis that there is a strong linkage between gas atomization processing conditions, as-atomized aluminum powder characteristics, and the consolidation methodology required to make components from aluminum powder. The hypothesis was tested with pure aluminum powders produced by commercial air atomization commercial inert gas atomization and gas atomization reaction synthesis (GARS). The commercial atomization methods are bench marks of current aluminum powder technology. The GARS process is a laboratory scale inert gas atomization facility. A benefit of using pure aluminum powders is an unambiguous interpretation of the results without considering the effects of alloy elements. A comparison of the GARS aluminum powders with the commercial aluminum powders showed the former to exhibit superior powder characteristics. The powders were compared in terms of size and shape, bulk chemistry, surface oxide chemistry and structure, and oxide film thickness. Minimum explosive concentration measurements assessed the dependence of explosibility hazard on surface area, oxide film thickness, and gas atomization processing conditions. The GARS aluminum powders were exposed to different relative humidity levels, demonstrating the effect of atmospheric conditions on post-atomization oxidation of aluminum powder. An Al-Ti-Y GARS alloy exposed in ambient air at different temperatures revealed the effect of reactive alloy elements on post-atomization powder oxidation. The pure aluminum powders were consolidated by two different routes, a conventional consolidation process for fabricating aerospace components with aluminum powder and a proposed alternative. The consolidation procedures were compared by evaluating the consolidated microstructures and the corresponding mechanical properties. A low temperature solid state sintering experiment demonstrated that tap densified GARS aluminum powders can form sintering necks between contacting powder particles, unlike the total resistance to sintering of commercial air atomization aluminum powder.

Analysis of the compressive behaviour of the three-dimensional printed porous titanium for dental implants using a modified cellular solid model.

PubMed

Gagg, Graham; Ghassemieh, Elaheh; Wiria, Florencia E

2013-09-01

A set of cylindrical porous titanium test samples were produced using the three-dimensional printing and sintering method with samples sintered at 900 °C, 1000 °C, 1100 °C, 1200 °C or 1300 °C. Following compression testing, it was apparent that the stress-strain curves were similar in shape to the curves that represent cellular solids. This is despite a relative density twice as high as what is considered the threshold for defining a cellular solid. As final sintering temperature increased, the compressive behaviour developed from being elastic-brittle to elastic-plastic and while Young's modulus remained fairly constant in the region of 1.5 GPa, there was a corresponding increase in 0.2% proof stress of approximately 40-80 MPa. The cellular solid model consists of two equations that predict Young's modulus and yield or proof stress. By fitting to experimental data and consideration of porous morphology, appropriate changes to the geometry constants allow modification of the current models to predict with better accuracy the behaviour of porous materials with higher relative densities (lower porosity).

Method of making an air electrode material having controlled sinterability

DOEpatents

Vasilow, Theodore R.; Kuo, Lewis J. H.; Ruka, Roswell J.

1994-01-01

A tubular, porous ceramic electrode structure (3) is made from the sintered admixture of doped lanthanum manganite and an additive containing cerium where a solid electrolyte (4), substantially surrounds the air electrode, and a porous outer fuel electrode (7) substantially surrounds the electrolyte, to form a fuel cell (1).

Method of making an air electrode material having controlled sinterability

DOEpatents

Vasilow, T.R.; Kuo, L.J.H.; Ruka, R.J.

1994-08-30

A tubular, porous ceramic electrode structure is made from the sintered admixture of doped lanthanum manganite and an additive containing cerium where a solid electrolyte, substantially surrounds the air electrode, and a porous outer fuel electrode substantially surrounds the electrolyte, to form a fuel cell. 2 figs.

High temperature resistant cermet and ceramic compositions. [for thermal resistant insulators and refractory coatings

NASA Technical Reports Server (NTRS)

Phillips, W. M. (Inventor)

1978-01-01

High temperature oxidation resistance, high hardness and high abrasion and wear resistance are properties of cermet compositions particularly to provide high temperature resistant refractory coatings on metal substrates, for use as electrical insulation seals for thermionic converters. The compositions comprise a sintered body of particles of a high temperature resistant metal or metal alloy, preferably molybdenum or tungsten particles, dispersed in and bonded to a solid solution formed of aluminum oxide and silicon nitride, and particularly a ternary solid solution formed of a mixture of aluminum oxide, silicon nitride and aluminum nitride. Ceramic compositions comprising a sintered solid solution of aluminum oxide, silicon nitride and aluminum nitride are also described.

Development of a sintering process for recycling oil shale fly ash and municipal solid waste incineration bottom ash into glass ceramic composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Zhikun; Zhang, Lei; Li, Aimin, E-mail: leeam@dlut.edu.cn

Highlights: • Glass ceramic composite is prepared from oil shale fly ash and MSWI bottom ash. • A novel method for the production of glass ceramic composite is presented. • It provides simple route and lower energy consumption in terms of recycling waste. • The vitrified slag can promote the sintering densification process of glass ceramic. • The performances of products decrease with the increase of oil shale fly ash content. - Abstract: Oil shale fly ash and municipal solid waste incineration bottom ash are industrial and municipal by-products that require further treatment before disposal to avoid polluting the environment.more » In the study, they were mixed and vitrified into the slag by the melt-quench process. The obtained vitrified slag was then mixed with various percentages of oil shale fly ash and converted into glass ceramic composites by the subsequent sintering process. Differential thermal analysis was used to study the thermal characteristics and determine the sintering temperatures. X-ray diffraction analysis was used to analyze the crystalline phase compositions. Sintering shrinkage, weight loss on ignition, density and compressive strength were tested to determine the optimum preparation condition and study the co-sintering mechanism of vitrified amorphous slag and oil shale fly ash. The results showed the product performances increased with the increase of sintering temperatures and the proportion of vitrified slag to oil shale fly ash. Glass ceramic composite (vitrified slag content of 80%, oil shale fly ash content of 20%, sintering temperature of 1000 °C and sintering time of 2 h) showed the properties of density of 1.92 ± 0.05 g/cm{sup 3}, weight loss on ignition of 6.14 ± 0.18%, sintering shrinkage of 22.06 ± 0.6% and compressive strength of 67 ± 14 MPa. The results indicated that it was a comparable waste-based material compared to previous researches. In particular, the energy consumption in the production process was reduced compared to conventional vitrification and sintering method. Chemical resistance and heavy metals leaching results of glass ceramic composites further confirmed the possibility of its engineering applications.« less

Silicon carbide sintered products and a method for their manufacturing

NASA Technical Reports Server (NTRS)

Suzuki, K.

1986-01-01

SiC based sinters are produced by pressureless sintering from a SiC-AlN solid solution containing Al2 to 20, N 0.2 to 10, O 0.2 to 5, a Group IIIB element 0 to 15 percent, the remainder being Si and C. Thus, a 90:10 mixture of SiC and AlN powders were cold pressed at 2000 kg/sq cm and sintered for 5 hours at 2100 C in a nitrogen atmosphere. The resulting product had density of 3.11 g/cu cm and bending strength at ambient and 1400 C at 68.5 and 66.3 kg/sq mm.

Study of Diffusion Bonding of 45 Steel through the Compacted Nickel Powder Layer

NASA Astrophysics Data System (ADS)

Zeer, G. M.; Zelenkova, E. G.; Temnykh, V. I.; Tokmin, A. M.; Shubin, A. A.; Koroleva, Yu. P.; Mikheev, A. A.

2018-02-01

The microstructure of the transition zone and powder spacer, the concentration distribution of chemical elements over the width of the diffusion-bonded joint, and microhardness of 45 steel-compacted Ni powder spacer-45 steel layered composites formed by diffusion bonding have been investigated. It has been shown that the relative spacer thickness χ < 0.06 is optimal for obtaining a high-quality joint has been formed under a compacting pressure of 500 MPa. The solid-state diffusion bonding is accompanied by sintering the nickel powder spacer and the formation of the transition zone between the spacer and steel. The transition zone consists of solid solution of nickel in the α-Fe phase and ordered solid solution of iron in nickel (FeNi3).

Influence of high-temperature steam on the reactivity of CaO sorbent for CO₂ capture.

PubMed

Donat, Felix; Florin, Nicholas H; Anthony, Edward J; Fennell, Paul S

2012-01-17

Calcium looping is a high-temperature CO(2) capture technology applicable to the postcombustion capture of CO(2) from power station flue gas, or integrated with fuel conversion in precombustion CO(2) capture schemes. The capture technology uses solid CaO sorbent derived from natural limestone and takes advantage of the reversible reaction between CaO and CO(2) to form CaCO(3); that is, to achieve the separation of CO(2) from flue or fuel gas, and produce a pure stream of CO(2) suitable for geological storage. An important characteristic of the sorbent, affecting the cost-efficiency of this technology, is the decay in reactivity of the sorbent over multiple CO(2) capture-and-release cycles. This work reports on the influence of high-temperature steam, which will be present in flue (about 5-10%) and fuel (∼20%) gases, on the reactivity of CaO sorbent derived from four natural limestones. A significant increase in the reactivity of these sorbents was found for 30 cycles in the presence of steam (from 1-20%). Steam influences the sorbent reactivity in two ways. Steam present during calcination promotes sintering that produces a sorbent morphology with most of the pore volume associated with larger pores of ∼50 nm in diameter, and which appears to be relatively more stable than the pore structure that evolves when no steam is present. The presence of steam during carbonation reduces the diffusion resistance during carbonation. We observed a synergistic effect, i.e., the highest reactivity was observed when steam was present for both calcination and carbonation.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kassen, Aaron G.; White, Emma M. H.; Tang, Wei

We present economic uncertainty in the rare earth (RE) permanent magnet marketplace, as well as in an expanding electric drive vehicle market that favors permanent magnet alternating current synchronous drive motors, motivated renewed research in RE-free permanent magnets like “alnico,” an Al-Ni-Co-Fe alloy. Thus, high-pressure, gas-atomized isotropic type-8H pre-alloyed alnico powder was compression molded with a clean burn-out binder to near-final shape and sintered to density >99% of cast alnico 8 (full density of 7.3 g/cm 3). To produce aligned sintered alnico magnets for improved energy product and magnetic remanence, uniaxial stress was attempted to promote controlled grain growth, avoidingmore » directional solidification that provides alignment in alnico 9. Lastly, successful development of solid-state powder processing may enable anisotropically aligned alnico magnets with enhanced energy density to be mass-produced.« less

Feasibility study of the welding of SiC

NASA Technical Reports Server (NTRS)

Moore, T. J.

1985-01-01

In a brief study of the feasibility of welding sintered alpha-SiC, solid-state welding and brazing were investigated. Joint quality was determined solely by microstructural examination. Hot-pressure welding was shown to be feasible at 1950 C. Diffusion welding and brazing were also successful under hot isostatic pressure at 1950 C when boride, carbide, and silicide interlayers were used. Furnace brazing was accomplished at 1750 C when a TiSi2 interlayer was introduced.

Leachability of Heavy Metals from Lightweight Aggregates Made with Sewage Sludge and Municipal Solid Waste Incineration Fly Ash

PubMed Central

Wei, Na

2015-01-01

Lightweight aggregate (LWA) production with sewage sludge and municipal solid waste incineration (MSWI) fly ash is an effective approach for waste disposal. This study investigated the stability of heavy metals in LWA made from sewage sludge and MSWI fly ash. Leaching tests were conducted to find out the effects of MSWI fly ash/sewage sludge (MSWI FA/SS) ratio, sintering temperature and sintering time. It was found that with the increase of MSWI FA/SS ratio, leaching rates of all heavy metals firstly decreased and then increased, indicating the optimal ratio of MSWI fly ash/sewage sludge was 2:8. With the increase of sintering temperature and sintering time, the heavy metal solidifying efficiencies were strongly enhanced by crystallization and chemical incorporations within the aluminosilicate or silicate frameworks during the sintering process. However, taking cost-savings and lower energy consumption into account, 1100 °C and 8 min were selected as the optimal parameters for LWA sample- containing sludge production. Furthermore, heavy metal leaching concentrations under these optimal LWA production parameters were found to be in the range of China’s regulatory requirements. It is concluded that heavy metals can be properly stabilized in LWA samples containing sludge and cannot be easily released into the environment again to cause secondary pollution. PMID:25961800

Leachability of heavy metals from lightweight aggregates made with sewage sludge and municipal solid waste incineration fly ash.

PubMed

Wei, Na

2015-05-07

Lightweight aggregate (LWA) production with sewage sludge and municipal solid waste incineration (MSWI) fly ash is an effective approach for waste disposal. This study investigated the stability of heavy metals in LWA made from sewage sludge and MSWI fly ash. Leaching tests were conducted to find out the effects of MSWI fly ash/sewage sludge (MSWI FA/SS) ratio, sintering temperature and sintering time. It was found that with the increase of MSWI FA/SS ratio, leaching rates of all heavy metals firstly decreased and then increased, indicating the optimal ratio of MSWI fly ash/sewage sludge was 2:8. With the increase of sintering temperature and sintering time, the heavy metal solidifying efficiencies were strongly enhanced by crystallization and chemical incorporations within the aluminosilicate or silicate frameworks during the sintering process. However, taking cost-savings and lower energy consumption into account, 1100 °C and 8 min were selected as the optimal parameters for LWA sample- containing sludge production. Furthermore, heavy metal leaching concentrations under these optimal LWA production parameters were found to be in the range of China's regulatory requirements. It is concluded that heavy metals can be properly stabilized in LWA samples containing sludge and cannot be easily released into the environment again to cause secondary pollution.

Liquid phase sintered compacts in space

NASA Technical Reports Server (NTRS)

Mookherji, T. K.; Mcanelly, W. B.

1974-01-01

A model that will explain the effect of gravity on liquid phase sintering was developed. Wetting characteristics and density segregation which are the two important phenomena in liquid phase sintering are considered in the model development. Experiments were conducted on some selected material combinations to study the gravity effects on liquid phase sintering, and to verify the validity of the model. It is concluded that: (1) The surface tension forces acting on solid particles in a one-g environment are not appreciably different from those anticipated in a 0.00001g/g sub 0 (or lower) environment. (2) The capillary forces are dependent on the contact angle, the quantity of the liquid phase, and the distance between solid particles. (3) The pores (i.e., bubbles) do not appear to be driven to the surface by gravity-produced buoyancy forces. (4) The length of time to produce the same degree of settling in a low-gravity environment will be increased significantly. (5) A low gravity environment would appear to offer a unique means of satisfactorily infiltrating a larger and/or complex shaped compact.

Study on the mechanism of liquid phase sintering (M-12)

NASA Technical Reports Server (NTRS)

Kohara, S.

1993-01-01

The objectives were to (1) obtain the data representing the growth rate of solid particles in a liquid matrix without the effect of gravity; and (2) reveal the growth behavior of solid particles during liquid phase sintering using the data obtained. Nickel and tungsten are used as the constituent materials in liquid phase sintering. The properties of the constituent metals are given. When a compact of the mixture of tungsten and nickel powders is heated and kept at 1550 C, nickel melts down but tungsten stays solid. As the density of tungsten is much greater than that of nickel, the sedimentation of tungsten particles occurs in the experiment on Earth. The difference between the experiments on Earth and in space is illustrated. The tungsten particles sink to the bottom and are brought into contact with each other. The resulting pressure at the contact point causes the accelerated dissolution of tungsten. Consequently, flat surfaces are formed at the contact sites. As a result of dissolution and reprecipitation of tungsten, the shape of particles changes to a polygon. This phenomenon is called 'flattening.' An example of flattening of tungsten particles is shown. Thus, the data obtained by the experiment on Earth may not represent the exact growth behavior of the solid particles in a liquid matrix. If the experiments were done in a microgravity environment, the data corresponding to the theoretical growth behavior of solid particles could be achieved.

High strength porous support tubes for high temperature solid electrolyte electrochemical cells

DOEpatents

Rossing, Barry R.; Zymboly, Gregory E.

1986-01-01

A high temperature, solid electrolyte electrochemical cell is made, having an electrode and a solid electrolyte disposed on a porous, sintered support material containing thermally stabilized zirconia powder particles and from about 3 wt. % to about 45 wt. % of thermally stable oxide fibers.

A promising red-emitting phosphor for white-light-emitting diodes prepared by a modified solid-state reaction

NASA Astrophysics Data System (ADS)

Ren, Fuqiang; Chen, Donghua

2010-02-01

Using urea, boric acid and polyethylene glycol (PEG) as auxiliary reagents, the novel red-emitting phosphors Ca 19Zn 2 (PO 4) 14:Eu 3+ have been successfully synthesized by a modified solid-state reaction. Thermogravimetric (TG) analysis, X-ray diffraction (XRD), transmission electron microscopy (TEM) and photoluminescence (PL) spectra were used to characterize the resulting phosphors. The dependence of the photoluminescence properties of Ca 19Zn 2 (PO 4) 14:Eu 3+ phosphors upon urea, boric acid and PEG concentration and the quadric-sintered temperature were investigated. Luminescent measurements showed that the phosphors can be efficiently excited by ultraviolet (UV) to visible region, emitting a red light with a peak wavelength of 616 nm. The material has potential application as a fluorescent material for ultraviolet light-emitting diodes (UV-LEDs).

Mn1.4Co1.4Cu0.2O4 spinel protective coating on ferritic stainless steels for solid oxide fuel cell interconnect applications

NASA Astrophysics Data System (ADS)

Chen, Guoyi; Xin, Xianshuang; Luo, Ting; Liu, Leimin; Zhou, Yuchun; Yuan, Chun; Lin, Chucheng; Zhan, Zhongliang; Wang, Shaorong

2015-03-01

In an attempt to reduce the oxidation and Cr evaporation rates of solid oxide fuel cells (SOFCs), Mn1.4Co1.4Cu0.2O4 spinel coating is developed on the Crofer22 APU ferritic stainless steel substrate by a powder reduction technique. Doping of Cu into Mn-Co spinels improves electrical conductivity as well as thermal expansion match with the Crofer22 APU interconnect. Good adhesion between the coating and the alloy substrate is achieved by the reactive sintering process using the reduced powders. Long-term isothermal oxidation experiment and area specific resistance (ASR) measurement are investigated. The ASR is less than 4 mΩ cm2 even though the coated alloy undergoes oxidation at 800 °C for 530 h and four thermal cycles from 800 °C to room temperature. The Mn1.4Co1.4Cu0.2O4 spinel coatings demonstrate excellent anti-oxidation performance and long-term stability. It exhibits a promising prospect for the practical application of SOFC alloy interconnect.

Performance of laser sintered Ti-6Al-4V implants with bone-inspired porosity and micro/nanoscale surface roughness in the rabbit femur

PubMed Central

Cohen, David J.; Cheng, Alice; Sahingur, Kaan; Clohessy, Ryan M.; Hopkins, Louis B.; Boyan, Barbara D.; Schwartz, Zvi

2018-01-01

Long term success of bone-interfacing implants remains a challenge in compromised patients and in areas of low bone quality. While surface roughness at the micro/nanoscale can promote osteogenesis, macro-scale porosity is important for promoting mechanical stability of the implant over time. Currently, machining techniques permit pores to be placed throughout the implant, but the pores are generally uniform in dimension. The advent of laser sintering provides a way to design and manufacture implants with specific porosity and variable dimensions at high resolution. This approach enables production of metal implants that mimic complex geometries found in biology. In this study, we used a rabbit femur model to compare osseointegration of laser sintered solid and porous implants. Ti-6Al-4V implants were laser sintered in a clinically relevant size and shape. One set of implants had a novel porosity based on human trabecular bone; both sets had grit-blasted/acid-etched surfaces. After characterization, implants were inserted transaxially into rabbit femora; mechanical testing, microCT and histomorphometry were conducted 10 weeks postoperatively. There were no differences in pull-out strength or bone-to-implant contact. However, both microCT and histomorphometry showed significantly higher new bone volume for porous compared to solid implants. Bone growth was observed into porous implant pores, especially near apical portions of the implant interfacing with cortical bone. These results show that laser sintered Ti-6Al-4V implants with micro/nanoscale surface roughness and trabecular bone-inspired porosity promote bone growth and may be used as a superior alternative to solid implants for bone-interfacing implants. PMID:28452335

Performance of laser sintered Ti-6Al-4V implants with bone-inspired porosity and micro/nanoscale surface roughness in the rabbit femur.

PubMed

Cohen, David J; Cheng, Alice; Sahingur, Kaan; Clohessy, Ryan M; Hopkins, Louis B; Boyan, Barbara D; Schwartz, Zvi

2017-04-28

Long term success of bone-interfacing implants remains a challenge in compromised patients and in areas of low bone quality. While surface roughness at the micro/nanoscale can promote osteogenesis, macro-scale porosity is important for promoting mechanical stability of the implant over time. Currently, machining techniques permit pores to be placed throughout the implant, but the pores are generally uniform in dimension. The advent of laser sintering provides a way to design and manufacture implants with specific porosity and variable dimensions at high resolution. This approach enables production of metal implants that mimic complex geometries found in biology. In this study, we used a rabbit femur model to compare osseointegration of laser sintered solid and porous implants. Ti-6Al-4V implants were laser sintered in a clinically relevant size and shape. One set of implants had a novel porosity based on human trabecular bone; both sets had grit-blasted/acid-etched surfaces. After characterization, implants were inserted transaxially into rabbit femora; mechanical testing, micro-computed tomography (microCT) and histomorphometry were conducted 10 weeks post-operatively. There were no differences in pull-out strength or bone-to-implant contact. However, both microCT and histomorphometry showed significantly higher new bone volume for porous compared to solid implants. Bone growth was observed into porous implant pores, especially near apical portions of the implant interfacing with cortical bone. These results show that laser sintered Ti-6Al-4V implants with micro/nanoscale surface roughness and trabecular bone-inspired porosity promote bone growth and may be used as a superior alternative to solid implants for bone-interfacing implants.

Al{sub 2}O{sub 3} - TiO{sub 2}-A simple sol-gel strategy to the synthesis of low temperature sintered alumina-aluminium titanate composites through a core-shell approach

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jayasankar, M.; Ananthakumar, S.; Mukundan, P.

A simple sol-gel based core-shell approach for the synthesis of alumina-aluminium titanate composite is reported. Alumina is the core and titania is the shell. The coating of titania has been performed in aqueous medium on alumina particle by means of heterocoagulation of titanyl chloride. Further heat treatment results in low temperature formation of aluminium titanate as well as low temperature sintering of alumina-aluminium titanate composites. The lowering of the reaction temperature can be attributed to the maximisation of the contact surface between the reactants due to the core-shell approach involving nanoparticles. The mechanism of formation of aluminium titanate and themore » observations on densification features in the present process are compared with that of mixture of oxides under identical conditions. The sintered alumina-aluminium titanate composite has an average grain size of 2 {mu}m. - Graphical abstract: The article presents a simple sol-gel process through core-shell approach to the synthesis of low temperature sintered alumina-aluminium titanate. The lowering of the reaction temperature can be attributed to the maximisation of the contact surface between the reactant due to the core-shell approach. This material showed the better microstructure control compared to the standard solid-state mixing route.« less

Sintering of MSW fly ash for reuse as a concrete aggregate.

PubMed

Mangialardi, T

2001-10-12

The sintering process of municipal solid waste (MSW) fly ash was investigated in order to manufacture sintered products for reuse as concrete aggregates. Four types of fly ash resulting from different Italian MSW incineration plants were tested in this study. A modification of the chemical composition of MSW fly ash--through a preliminary four-stage washing treatment of this material with water--was attempted to improve the chemical and mechanical characteristics of sintered products.The sintering treatment of untreated or washed fly ash was performed on cylindrical compact specimens (15 mm in diameter and 20mm in height) at different compact pressures, sintering temperatures and times.The sintering process of untreated MSW fly ashes proved to be ineffective for manufacturing sintered products for reuse as a construction material, because of the adverse chemical characteristics of these fly ashes in terms of sulfate, chloride, and vitrifying oxide contents.A preliminary washing treatment of MSW fly ash with water greatly improved the chemical and mechanical characteristics of sintered products and, for all the types of fly ash tested, the sintered products satisfied the Italian requirements for normal weight aggregates for use in concretes having a specified strength not greater than 12 and 15N/mm(2), when measured on cylindrical and cubic specimens, respectively.A compact pressure of 28 N/mm(2), a sintering temperature of 1140 degrees C, and a sintering time of 60 min were the best operating conditions for manufacturing sintered products of washed MSW fly ash.

Apparatus and process for controlling fluidized beds

DOEpatents

Rehmat, Amirali G.; Patel, Jitendra G.

1985-10-01

An apparatus and process for control and maintenance of fluidized beds under non-steady state conditions. An ash removal conduit is provided for removing solid particulates from a fluidized bed separate from an ash discharge conduit in the lower portion of the grate supporting such a bed. The apparatus and process of this invention is particularly suitable for use in ash agglomerating fluidized beds and provides control of the fluidized bed before ash agglomeration is initiated and during upset conditions resulting in stable, sinter-free fluidized bed maintenance.

Apparatus for controlling fluidized beds

DOEpatents

Rehmat, Amirali G.; Patel, Jitendra G.

1987-05-12

An apparatus and process for control and maintenance of fluidized beds under non-steady state conditions. An ash removal conduit is provided for removing solid particulates from a fluidized bed separate from an ash discharge conduit in the lower portion of the grate supporting such a bed. The apparatus and process of this invention is particularly suitable for use in ash agglomerating fluidized beds and provides control of the fluidized bed before ash agglomeration is initiated and during upset conditions resulting in stable, sinter-free fluidized bed maintenance.

Influence of Hydrogen on Atomized Titanium Powders Sintering

NASA Astrophysics Data System (ADS)

Senkevich, K. S.

2018-07-01

The aim of this work is to study the effect of hydrogen reversible alloying (thermohydrogen processing, THP) on low-temperature sintering of atomized titanium powders. It is stated that alloying with 0.2 to 0.8 wt pct of hydrogen beneficially affects titanium powders sintering. The effect is caused by phase transformations occurring upon hydrogen saturation of powders and dehydrogenation, which substantially intensifies sintering at temperatures from 800 °C to 900 °C. The role of certain THP stages (sintering in hydrogenated state and upon dehydrogenation) on formation of sintered contacts in porous materials is shown.

Influence of Hydrogen on Atomized Titanium Powders Sintering

NASA Astrophysics Data System (ADS)

Senkevich, K. S.

2018-05-01

The aim of this work is to study the effect of hydrogen reversible alloying (thermohydrogen processing, THP) on low-temperature sintering of atomized titanium powders. It is stated that alloying with 0.2 to 0.8 wt pct of hydrogen beneficially affects titanium powders sintering. The effect is caused by phase transformations occurring upon hydrogen saturation of powders and dehydrogenation, which substantially intensifies sintering at temperatures from 800 °C to 900 °C. The role of certain THP stages (sintering in hydrogenated state and upon dehydrogenation) on formation of sintered contacts in porous materials is shown.

PHASE EVOLUTION AND MICROWAVE DIELECTRIC PROPERTIES OF (Li0.5Bi0.5)(W1-xMox)O4(0.0 ≤ x ≤ 1.0) CERAMICS WITH ULTRA-LOW SINTERING TEMPERATURES

NASA Astrophysics Data System (ADS)

Zhou, Di; Guo, Jing; Yao, Xi; Pang, Li-Xia; Qi, Ze-Ming; Shao, Tao

2012-11-01

The (Li0.5Bi0.5)(W1-xMox)O4(0.0 ≤ x ≤ 1.0) ceramics were prepared via the solid state reaction method. The sintering temperature decreased almost linearly from 755°C for (Li0.5Bi0.5)WO4 to 560°C for (Li0.5Bi0.5)MoO4. When the x≤0.3, a wolframite solid solution can be formed. For x = 0.4 and x = 0.6 compositions, both the wolframite and scheelite phases can be formed from the X-ray diffraction analysis, while two different kinds of grains can be revealed from the scanning electron microscopy and energy-dispersive X-ray spectrometer results. High performance of microwave dielectric properties were obtained in the (Li0.5Bi0.5)(W0.6Mo0.4)O4 ceramic sintered at 620°C with a relative permittivity of 31.5, a Qf value of 8500 GHz (at 8.2 GHz), and a temperature coefficient value of +20 ppm/°C. Complex dielectric spectra of pure (Li0.5Bi0.5)WO4 ceramic gained from the infrared spectra were extrapolated down to microwave range, and they were in good agreement with the measured values. The (Li0.5Bi0.5)(W1-xMox)O4(0.0 ≤ x ≤ 1.0) ceramics might be promising for low temperature co-fired ceramic technology.

High-Pressure Spark Plasma Sintering (HP SPS): A Promising and Reliable Method for Preparing Ti-Al-Si Alloys.

PubMed

Knaislová, Anna; Novák, Pavel; Cygan, Sławomir; Jaworska, Lucyna; Cabibbo, Marcello

2017-04-27

Ti-Al-Si alloys are prospective material for high-temperature applications. Due to low density, good mechanical properties, and oxidation resistance, these intermetallic alloys can be used in the aerospace and automobile industries. Ti-Al-Si alloys were prepared by powder metallurgy using reactive sintering, milling, and spark plasma sintering. One of the novel SPS techniques is high-pressure spark plasma sintering (HP SPS), which was tested in this work and applied to a Ti-10Al-20Si intermetallic alloy using a pressure of 6 GPa and temperatures ranging from 1318 K (1045 °C) to 1597 K (1324 °C). The low-porosity consolidated samples consist of Ti₅Si₃ silicides in an aluminide (TiAl) matrix. The hardness varied between 720 and 892 HV 5.

High-Pressure Spark Plasma Sintering (HP SPS): A Promising and Reliable Method for Preparing Ti–Al–Si Alloys

PubMed Central

Knaislová, Anna; Novák, Pavel; Cygan, Sławomir; Jaworska, Lucyna; Cabibbo, Marcello

2017-01-01

Ti–Al–Si alloys are prospective material for high-temperature applications. Due to low density, good mechanical properties, and oxidation resistance, these intermetallic alloys can be used in the aerospace and automobile industries. Ti–Al–Si alloys were prepared by powder metallurgy using reactive sintering, milling, and spark plasma sintering. One of the novel SPS techniques is high-pressure spark plasma sintering (HP SPS), which was tested in this work and applied to a Ti–10Al–20Si intermetallic alloy using a pressure of 6 GPa and temperatures ranging from 1318 K (1045 °C) to 1597 K (1324 °C). The low-porosity consolidated samples consist of Ti5Si3 silicides in an aluminide (TiAl) matrix. The hardness varied between 720 and 892 HV 5. PMID:28772824

Monolithic All-Phosphate Solid-State Lithium-Ion Battery with Improved Interfacial Compatibility.

PubMed

Yu, Shicheng; Mertens, Andreas; Tempel, Hermann; Schierholz, Roland; Kungl, Hans; Eichel, Rüdiger-A

2018-06-22

High interfacial resistance between solid electrolyte and electrode of ceramic all-solid-state batteries is a major reason for the reduced performance of these batteries. A solid-state battery using a monolithic all-phosphate concept based on screen printed thick LiTi 2 (PO 4 ) 3 anode and Li 3 V 2 (PO 4 ) 3 cathode composite layers on a densely sintered Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 solid electrolyte has been realized with competitive cycling performance. The choice of materials was primarily based on the (electro-)chemical and mechanical matching of the components instead of solely focusing on high-performance of individual components. Thus, the battery utilized a phosphate backbone in combination with tailored morphology of the electrode materials to ensure good interfacial matching for a durable mechanical stability. Moreover, the operating voltage range of the active materials matches with the intrinsic electrochemical window of the electrolyte which resulted in high electrochemical stability. A highly competitive discharge capacity of 63.5 mAh g -1 at 0.39 C after 500 cycles, corresponding to 84% of the initial discharge capacity, was achieved. The analysis of interfacial charge transfer kinetics confirmed the structural and electrical properties of the electrodes and their interfaces with the electrolyte, as evidenced by the excellent cycling performance of the all-phosphate solid-state battery. These interfaces have been studied via impedance analysis with subsequent distribution of relaxation times analysis. Moreover, the prepared solid-state battery could be processed and operated in air atmosphere owing to the low oxygen sensitivity of the phosphate materials. The analysis of electrolyte/electrode interfaces after cycling demonstrates that the interfaces remained stable during cycling.

Electrodes for solid state gas sensor

DOEpatents

Mukundan, Rangachary [Santa Fe, NM; Brosha, Eric L [Los Alamos, NM; Garzon, Fernando [Santa Fe, NM

2007-05-08

A mixed potential electrochemical sensor for the detection of gases has a ceria-based electrolyte with a surface for exposing to the gases to be detected, and with a reference wire electrode and a sensing wire electrode extending through the surface and fixed within the electrolyte as the electrolyte is compressed and sintered. The electrochemical sensor is formed by placing a wire reference electrode and a wire sensing electrode in a die, where each electrode has a first compressed planar section and a second section depending from the first section with the second section of each electrode extending axially within the die. The die is filled with an oxide-electrolyte powder and the powder is pressed within the die with the wire electrodes. The wire-electrodes and the pressed oxide-electrolyte powder are sintered to form a ceramic electrolyte base with a reference wire electrode and a sensing wire electrode depending therefrom.

Electrodes for solid state gas sensor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mukundan, Rangachary; Brosha, Eric L; Garzon, Fernando

2007-05-08

A mixed potential electrochemical sensor for the detection of gases has a ceria-based electrolyte with a surface for exposing to the gases to be detected, and with a reference wire electrode and a sensing wire electrode extending through the surface and fixed within the electrolyte as the electrolyte is compressed and sintered. The electrochemical sensor is formed by placing a wire reference electrode and a wire sensing electrode in a die, where each electrode has a first compressed planar section and a second section depending from the first section with the second section of each electrode extending axially within themore » die. The die is filled with an oxide-electrolyte powder and the powder is pressed within the die with the wire electrodes. The wire-electrodes and the pressed oxide-electrolyte powder are sintered to form a ceramic electrolyte base with a reference wire electrode and a sensing wire electrode depending therefrom.« less

Electrodes for solid state gas sensor

DOEpatents

Mukundan, Rangachary; Brosha, Eric L.; Garzon, Fernando

2003-08-12

A mixed potential electrochemical sensor for the detection of gases has a ceria-based electrolyte with a surface for exposing to the gases to be detected, and with a reference wire electrode and a sensing wire electrode extending through the surface and fixed within the electrolyte as the electrolyte is compressed and sintered. The electrochemical sensor is formed by placing a wire reference electrode and a wire sensing electrode in a die, where each electrode has a first compressed planar section and a second section depending from the first section with the second section of each electrode extending axially within the die. The die is filled with an oxide-electrolyte powder and the powder is pressed within the die with the wire electrodes. The wire-electrodes and the pressed oxide-electrolyte powder are sintered to form a ceramic electrolyte base with a reference wire electrode and a sensing wire electrode depending therefrom.

Porous Titanium Parts Fabricated by Sintering of TiH2 and Ti Powder Mixtures

NASA Astrophysics Data System (ADS)

Peng, Qin; Yang, Bin; Friedrich, Bernd

2018-01-01

A new simple powder metallurgy process by sintering TiH2 powders was used to manufacture porous Ti components. The effects of the processing parameters (pressure of cold isostatic pressing and sintering temperature) and the TiH2/Ti ratio in the powder mixtures on the impurities, the linear shrinkage and the pore properties (including overall and open porosities) were comprehensively determined. The addition of TiH2 as a reactant has been found beneficial for the synthesis of porous Ti components. The formation mechanisms of pores were demonstrated based on the dehydrogenation process of TiH2 during sintering, resulting in highest reactivity due to the "in statu nascendi" generation of the metal. In addition, the hardness and corrosion resistance of all the sintered samples were evaluated, related to the overall and open porosities. As a result, an optimal composition of Ti-40 wt.% TiH2 was defined, as its maximum open porosity was about 23%.

Constrained Sintering in Fabrication of Solid Oxide Fuel Cells

PubMed Central

Lee, Hae-Weon; Park, Mansoo; Hong, Jongsup; Kim, Hyoungchul; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook

2016-01-01

Solid oxide fuel cells (SOFCs) are inevitably affected by the tensile stress field imposed by the rigid substrate during constrained sintering, which strongly affects microstructural evolution and flaw generation in the fabrication process and subsequent operation. In the case of sintering a composite cathode, one component acts as a continuous matrix phase while the other acts as a dispersed phase depending upon the initial composition and packing structure. The clustering of dispersed particles in the matrix has significant effects on the final microstructure, and strong rigidity of the clusters covering the entire cathode volume is desirable to obtain stable pore structure. The local constraints developed around the dispersed particles and their clusters effectively suppress generation of major process flaws, and microstructural features such as triple phase boundary and porosity could be readily controlled by adjusting the content and size of the dispersed particles. However, in the fabrication of the dense electrolyte layer via the chemical solution deposition route using slow-sintering nanoparticles dispersed in a sol matrix, the rigidity of the cluster should be minimized for the fine matrix to continuously densify, and special care should be taken in selecting the size of the dispersed particles to optimize the thermodynamic stability criteria of the grain size and film thickness. The principles of constrained sintering presented in this paper could be used as basic guidelines for realizing the ideal microstructure of SOFCs. PMID:28773795

The Preparation and Characterization of Materials.

ERIC Educational Resources Information Center

Wold, Aaron

1980-01-01

Presents several examples illustrating different aspects of materials problems, including problems associated with solid-solid reactions, sintering and crystal growth, characterization of materials, preparation and characterization of stoichiometric ferrites and chromites, copper-sulfur systems, growth of single crystals by chemical vapor…

The effect of B{sub 2}O{sub 3} flux on growth NLBCO superconductor by solid state reaction and wet-mixing methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Suharta, W. G., E-mail: wgsuharta@gmail.com; Wendri, N.; Ratini, N.

The synthesis of B{sub 2}O{sub 3} flux substituted NLBCO superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} has been done using solid state reaction and wet-mixing methods in order to obtain homogeneous crystals and single phase. From DTA/TGA characteritations showed the synthesis process by wet-mixing requires a lower temperature than the solid state reaction in growing the superconductor NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂}. Therefore, in this research NdBa{sub 1.75}La{sub 0.25}Cu{sub 3}O{sub 7-∂} sample calcinated at 650°C for wet-mixing method and 820°C for solid state reaction methods. The all samples was sintered at 950°C for ten hours. Crystallinity of the sample was confirmedmore » using X-ray techniques and generally obtained sharp peaks that indicates the sample already well crystallized. Search match analyses for diffraction data gave weight fractions of impurity phase of the solid state reaction method higher than wet-mixing method. In this research showed decreasing the price of the lattice parameter about 1% with the addition of B{sub 2}O{sub 3} flux for the both synthesis process and 2% of wet mixing process for all samples. Characterization using scanning electron microscopy (SEM) showed the distribution of crystal zise for wet-mixing method more homogeneous than solid state reaction method, with he grain size of samples is around 150–250 nm. The results of vibrating sample magnetometer (VSM) showed the paramagnetic properties for all samples.« less

A Study of Photoluminiscence and UV-Vis in Enhanced GaN Nanofibers

NASA Astrophysics Data System (ADS)

Robles-Garcia, Joshua; Melendez-Zambrana, Anamaris; Ramos, Idalia

2014-03-01

The photoluminiscence (PL) and UV-Vis properties of Gallium Nitride (GaN) nanofibers were investigated for samples fabricated with a precursor solution containing Gallium Nitrate Hydrate, Cellulose Acetate, and Urea in the solvents Dimethylacetamide (DMA) and Acetone. GaN is a wide bandgap (3.4 eV) semiconductor that can be used in a variety of applications including solid-state lighting, high power, and high frequency devices. In previous work, we produced polycrystalline GaN nanofibers with wurtzite structure, using the electrospinning method and a thermal treatment in nitrogen and ammonia at 1000C. In this research we study the addition of urea to the precursor solution to enhance the crystallinity of the fibers at lower sintering temperatures. The molar ratios of urea added to the precursor range from 0 to 1.7 M. After electrospinning the fibers were sintered in Nitrogen at 450C for 3 hours and then, under ammonia gas flow at 900C for 5 hours. X-Ray Diffraction (XRD), UV-Vis spectroscopy, and PL measurements at room temperature were used to study the structural and optical properties of the fibers during the sintering process. This work was sponsored by UPRH PREM (NSF-DMR-0934195).

Production of superconductor/carbon bicomponent fibers

NASA Technical Reports Server (NTRS)

Wise, S. A.; Fain, C. C.; Leigh, H. D.; Sherrill, M.

1990-01-01

Certain materials are unable to be drawn or spun into fiber form due to their improper melting characteristics or brittleness. However, fibrous samples of such materials are often necessary for the fabrication of intricate shapes and composites. In response to this problem, a unique process, referred to as the piggyback process, was developed to prepare fibrous samples of a variety of nonspinnable ceramics. In this technique, specially produced C-shaped carbon fibers serve as micromolds to hold the desired materials prior to sintering. Depending on the sintering atmosphere used, bicomponent or single component fibers result. While much has been demonstrated worldwide concerning the YBa2Cu3O(7-x) superconductor, fabrication into unique forms has proven quite difficult. However, a variety of intricate shapes are necessary for rapid commercialization of the superconducting materials. The potential for producing fibrous samples of the YBa2Cu3O(7-x) compound by the piggyback process is being investigated. Various organic and acrylic materials were investigated to determine suspending ability, reactivity with the YBa2Cu3O(7-x) compound during long term storage, and burn out characteristics. While many questions were answered with respect to the interfacial reactions between YBa2Cu3O(7-x) and carbon, much work is still necessary to improve the quality of the sintered material if the fibers produced are to be incorporated into useful composites or cables. Additional research is necessary to evaluate quality of the barrier layer during long soakings at the peak temperature; adjust the firing schedule to avoid microcracking and improve densification; and increase the solids loading in the superconductive suspension to decrease porosity.

Parallel Large-Scale Molecular Dynamics Simulation Opens New Perspective to Clarify the Effect of a Porous Structure on the Sintering Process of Ni/YSZ Multiparticles.

PubMed

Xu, Jingxiang; Higuchi, Yuji; Ozawa, Nobuki; Sato, Kazuhisa; Hashida, Toshiyuki; Kubo, Momoji

2017-09-20

Ni sintering in the Ni/YSZ porous anode of a solid oxide fuel cell changes the porous structure, leading to degradation. Preventing sintering and degradation during operation is a great challenge. Usually, a sintering molecular dynamics (MD) simulation model consisting of two particles on a substrate is used; however, the model cannot reflect the porous structure effect on sintering. In our previous study, a multi-nanoparticle sintering modeling method with tens of thousands of atoms revealed the effect of the particle framework and porosity on sintering. However, the method cannot reveal the effect of the particle size on sintering and the effect of sintering on the change in the porous structure. In the present study, we report a strategy to reveal them in the porous structure by using our multi-nanoparticle modeling method and a parallel large-scale multimillion-atom MD simulator. We used this method to investigate the effect of YSZ particle size and tortuosity on sintering and degradation in the Ni/YSZ anodes. Our parallel large-scale MD simulation showed that the sintering degree decreased as the YSZ particle size decreased. The gas fuel diffusion path, which reflects the overpotential, was blocked by pore coalescence during sintering. The degradation of gas diffusion performance increased as the YSZ particle size increased. Furthermore, the gas diffusion performance was quantified by a tortuosity parameter and an optimal YSZ particle size, which is equal to that of Ni, was found for good diffusion after sintering. These findings cannot be obtained by previous MD sintering studies with tens of thousands of atoms. The present parallel large-scale multimillion-atom MD simulation makes it possible to clarify the effects of the particle size and tortuosity on sintering and degradation.

Sandblasting nozzle

NASA Technical Reports Server (NTRS)

Perkins, G. S.; Pawlik, E. V.; Phillips, W. M. (Inventor)

1981-01-01

A nozzle for use with abrasive and/or corrosive materials is formed of sintered ceramic compositions having high temperature oxidation resistance, high hardness and high abrasion and corrosion resistance. The ceramic may be a binary solid solution of a ceramic oxide and silicon nitride, and preferably a ternary solid solution of a ceramic oxide, silicon nitride and aluminum nitride. The ceramic oxide is selected from a group consisting of Al2O3, Y2O3 and Cr2O3, or mixtures of those compounds. Titanium carbide particles are dispersed in the ceramic mixture before sintering. The nozzles are encased for protection from external forces while in use by a metal or plastic casing.

Performance of planar single cell lanthanum gallate based solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Maffei, N.; Kuriakose, A. K.

A novel synthesis of high purity, single phase strontium-magnesium doped lanthanum gallate through a nitrate route is described. The prepared powder is formed into planar monolithic elements by uniaxial pressing followed by isostatic pressing and sintering. XRD analysis of the sintered elements reveal no detectable secondary phases. The performance of the electrolyte in solid oxide fuel cells (SOFC) with three different anode/cathode combinations tested at 700°C with respect to the J- V and power density is reported. The data show that the characteristics of this SOFC are strongly dependent on the particular anode/cathode system chosen.

High temperature strain gages

NASA Technical Reports Server (NTRS)

Gregory, Otto J. (Inventor); You, Tao (Inventor)

2011-01-01

A ceramic strain gage based on reactively sputtered indium-tin-oxide (ITO) thin films is used to monitor the structural integrity of components employed in aerospace propulsion systems operating at temperatures in excess of 1500.degree. C. A scanning electron microscopy (SEM) of the thick ITO sensors reveals a partially sintered microstructure comprising a contiguous network of submicron ITO particles with well defined necks and isolated nanoporosity. Densification of the ITO particles was retarded during high temperature exposure with nitrogen thus stabilizing the nanoporosity. ITO strain sensors were prepared by reactive sputtering in various nitrogen/oxygen/argon partial pressures to incorporate more nitrogen into the films. Under these conditions, sintering and densification of the ITO particles containing these nitrogen rich grain boundaries was retarded and a contiguous network of nano-sized ITO particles was established.

Growth of single crystals of BaFe12O19 by solid state crystal growth

NASA Astrophysics Data System (ADS)

Fisher, John G.; Sun, Hengyang; Kook, Young-Geun; Kim, Joon-Seong; Le, Phan Gia

2016-10-01

Single crystals of BaFe12O19 are grown for the first time by solid state crystal growth. Seed crystals of BaFe12O19 are buried in BaFe12O19+1 wt% BaCO3 powder, which are then pressed into pellets containing the seed crystals. During sintering, single crystals of BaFe12O19 up to ∼130 μm thick in the c-axis direction grow on the seed crystals by consuming grains from the surrounding polycrystalline matrix. Scanning electron microscopy-energy dispersive spectroscopy analysis shows that the single crystal and the surrounding polycrystalline matrix have the same chemical composition. Micro-Raman scattering shows the single crystal to have the BaFe12O19 structure. The optimum growth temperature is found to be 1200 °C. The single crystal growth behavior is explained using the mixed control theory of grain growth.

Sintering activation energy MoSi2-WSi2-Si3N4 ceramic

NASA Astrophysics Data System (ADS)

Titov, D. D.; Lysenkov, A. S.; Kargin, Yu F.; Frolova, M. G.; Gorshkov, V. A.; Perevislov, S. N.

2018-04-01

The activation energy of sintering process was calculated based on dilatometric studies of shrinkage processes (Mo,W)Si2 + Si3N4 composite ceramic. (Mo,W)Si2 powders was obtained by solid-phase solutions of 70 wt% MoSi2 and 30 wt% WSi2 by SHS in the ISMAN RAS. The concentration rate Si3N4 was from 1 to 15 wt.%. The sintering was carried out to 1850°C in Ar atmosphere the heating rate of 5, 10, 12 and 15°C/min by the way of dilatometer tests. Based on the differential kinetic analysis method (Friedman’s method), the sintering process activation energy of (Mo,W)Si2 + Si3N4 were calculated. The two-stage sintering process and the dependence of the activation energy on the Si3N4 content was shown. Average value of 370 kJ/mol for Q was obtained.

Ionic and Covalent Stabilization of Intermediates and Transition States in Catalysis by Solid Acids

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deshlahra, Prashant; Carr, Robert T.; Iglesia, Enrique

Reactivity descriptors describe catalyst properties that determine the stability of kinetically relevant transition states and adsorbed intermediates. Theoretical descriptors, such as deprotonation energies (DPE), rigorously account for Brønsted acid strength for catalytic solids with known structure. Here, mechanistic interpretations of methanol dehydration turnover rates are used to assess how charge reorganization (covalency) and electrostatic interactions determine DPE and how such interactions are recovered when intermediates and transition states interact with the conjugate anion in W and Mo polyoxometalate (POM) clusters and gaseous mineral acids. Turnover rates are lower and kinetically relevant species are less stable on Mo than W POMmore » clusters with similar acid strength, and such species are more stable on mineral acids than that predicted from W-POM DPE–reactivity trends, indicating that DPE and acid strength are essential but incomplete reactivity descriptors. Born–Haber thermochemical cycles indicate that these differences reflect more effective charge reorganization upon deprotonation of Mo than W POM clusters and the much weaker reorganization in mineral acids. Such covalency is disrupted upon deprotonation but cannot be recovered fully upon formation of ion pairs at transition states. Predictive descriptors of reactivity for general classes of acids thus require separate assessments of the covalent and ionic DPE components. Here, we describe methods to estimate electrostatic interactions, which, taken together with energies derived from density functional theory, give the covalent and ionic energy components of protons, intermediates, and transition states. In doing so, we provide a framework to predict the reactive properties of protons for chemical reactions mediated by ion-pair transition states.« less

Computational and Experimental Investigations of Na-Ion Conduction in Cubic Na 3PSe 4

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bo, Shou -Hang; Wang, Yan; Kim, Jae Chul

All-solid-state Na-ion batteries that operate at or close to room temperature are a promising next-generation battery technology with enhanced safety and reduced manufacturing cost. An indispensable component of this technology is the solid-state electrolyte that allows rapid shuttling of the mobile cation (i.e., Na +) between the cathode and anode. However, there are very few fast Na-ion conductors with ionic conductivity approaching that of the liquid counterparts (i.e., 1 mS cm –1). In this work, we present the synthesis and characterization of a fast Na-ion conductor, cubic Na 3PSe 4. This material possesses a room-temperature ionic conductivity exceeding 0.1 mSmore » cm –1 and does not require high-temperature sintering to minimize grain boundary resistance, making it a promising solid-state electrolyte candidate for all-solid-state Na-ion battery applications. On the basis of density functional theory, nudged elastic band, and molecular dynamics investigations, we demonstrate that the framework of cubic Na 3PSe 4 only permits rapid Na + diffusion with the presence of defects, and that the formation of the Na vacancy (charge-balanced by slight Se 2– oxidation) is more energetically favorable among the various defects considered. This finding provides important guidelines to further improve Na-ion conductivity in this class of materials.« less

Computational and Experimental Investigations of Na-Ion Conduction in Cubic Na 3PSe 4

DOE PAGES

Bo, Shou -Hang; Wang, Yan; Kim, Jae Chul; ...

2015-11-17

All-solid-state Na-ion batteries that operate at or close to room temperature are a promising next-generation battery technology with enhanced safety and reduced manufacturing cost. An indispensable component of this technology is the solid-state electrolyte that allows rapid shuttling of the mobile cation (i.e., Na +) between the cathode and anode. However, there are very few fast Na-ion conductors with ionic conductivity approaching that of the liquid counterparts (i.e., 1 mS cm –1). In this work, we present the synthesis and characterization of a fast Na-ion conductor, cubic Na 3PSe 4. This material possesses a room-temperature ionic conductivity exceeding 0.1 mSmore » cm –1 and does not require high-temperature sintering to minimize grain boundary resistance, making it a promising solid-state electrolyte candidate for all-solid-state Na-ion battery applications. On the basis of density functional theory, nudged elastic band, and molecular dynamics investigations, we demonstrate that the framework of cubic Na 3PSe 4 only permits rapid Na + diffusion with the presence of defects, and that the formation of the Na vacancy (charge-balanced by slight Se 2– oxidation) is more energetically favorable among the various defects considered. This finding provides important guidelines to further improve Na-ion conductivity in this class of materials.« less

Critical considerations for the qualitative and quantitative determination of process-induced disorder in crystalline solids.

PubMed

Newman, Ann; Zografi, George

2014-09-01

Solid-state instabilities in crystalline solids arise during processing primarily because a certain level of structural disorder has been introduced into the crystal. Many physical instabilities appear to be associated with the recrystallization of molecules from these disordered regions, while chemical instabilities arise from sufficient molecular mobility to allow solid-state chemical reactivity. In this Commentary we discuss the various forms of structural disorder, processing which can produce disorder, the quantitative analysis of process-induced order, and strategies to limit disorder and its effects. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

The study of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites

NASA Astrophysics Data System (ADS)

Yu, Peng

Aluminum-based metal matrix composites (MMCs) have been widely used as structural materials in the automobile and aerospace industry due to their specific properties. In this thesis, we report the fabrication of in-situ formed alumina and aluminide intermetallic reinforced aluminum-based metal matrix composites by the displacement reactions between Al and selected metal oxides (NiO, CuO and ZnO). These MMCs were produced when the Al-20wt% NiO, Al-20wt% CuO and Al-10wt% ZnO green compacts were reaction sintered in the tube furnaces. In this work, differential thermal analysis (DTA) was performed on the green samples. The green samples were then sintered separately in different tube furnaces for 30 minutes. In order to study the reaction mechanisms, the x-ray diffractometry (XRD) was used to obtain diffraction patterns of these sintered samples, the scanning electron microscope (SEM) and transmission electron microscope (TEM) were used to study the microstructures of these samples. The elemental quantitative compositions of samples were determined by the energy dispersive x-ray spectrometry (EDX). In order to study the effect of cooling rate on the samples, the green samples were further sintered to 1000°C and cooled down to room temperature in different conditions: by furnace-cooling, air-quenching, oil-quenching or NaCl-solution-quenching. The SEM, TEM and atomic force microscopy (AFM) were conducted to investigate their microstructures. A microhardness tester was used to measure the hardness values of these samples. It was found that during sintering of the Al-20wt% NiO green sample, displacement reaction between Al and NiO initially occurred in solid-solid form and was soon halted by its products that separated the NiO particles from the Al matrix. The reaction then resumed in solid-liquid form as the temperature increased to the eutectic temperature of Al3Ni-Al when liquid (Al, Ni) phase appeared in the sample. After cooling, Al2O 3 particles, Al3Ni proeutectic phase and fiber-like Al 3Ni-Al eutectic were found in the sintered Al-MMC sample. (Abstract shortened by UMI.)

Mechanical Testing of Ultra-High Temperature Ceramics at 1500 C in Air - Development of an Experimental Facility and Test Method

DTIC Science & Technology

2015-03-26

SiC. TEM micrograph courtesy of R. S . Hay (AFRL/RXCC). ...................33 Fig. 5. Schematic of HfB2-based UHTC test specimen...the early work performed by the U. S . Air force and NASA was the identification of hafnium diboride (HfB2) and zirconium diboride (ZrB2) as good high...sintering, reactive routes, and spark plasma sintering. ~ 14 ~ Because diborides exhibit strong covalent bonding and low self-diffusion, high

Towards Development of a Super Ceramic Composite - Initial Investigation into Improvement of Strength and Toughness of Polycrystalline Ceramics

DTIC Science & Technology

2012-08-01

sintering of SiC. James Lill (2010) evaluated the Reactive Empirical Bond Order potentials of Brenner (Brenner 1990); the Adaptive Intermolecular Reactive...Protection mechanisms of the iron-plated armor of a deep-sea hydrothermal vent gastropod . PNAS 107(3):987-997. Yu, J., S. B. Sinnott, and S. R. Phillpot

Alloying Behavior and Properties of FeSiBAlNiCo x High Entropy Alloys Fabricated by Mechanical Alloying and Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Wang, Wen; Li, Boyu; Zhai, Sicheng; Xu, Juan; Niu, Zuozhe; Xu, Jing; Wang, Yan

2018-02-01

In this paper, FeSiBAlNiCo x (x = 0.2, 0.8) high-entropy alloy (HEA) powders were fabricated by mechanical alloying process, and the powders milled for 140 h were sintered by spark plasma sintering (SPS) technique. The microstructures and properties of as-milled powders and as-sintered samples were investigated. The results reveal that the final milling products (140 h) of both sample powders present the fully amorphous structure. The increased Co contents obviously enhance the glass forming ability and thermal stability of amorphous HEA powders, which are reflected by the shorter formation time of fully amorphous phase and the higher onset crystallization temperature, respectively. According to coercivity, the as-milled FeSiBAlNiCo x (x = 0.2, 0.8) powders (140 h) are the semi-hard magnetic materials. FeSiBAlNiCo0.8 HEA powders possess the highest saturation magnetization and largest remanence ratio. The SPS-ed products of both bulk HEAs are composed of body-centered cubic solid solution, and FeSi and FeB intermetallic phases. They possess the high relative density above 97% and excellent microhardness exceeding 1150 HV. The as-sintered bulks undergo the remarkable increase in saturation magnetization compared with the as-milled state. The SPS-ed FeSiBAlNiCo0.8 HEA exhibits the soft magnetic properties. The electrochemical corrosion test is carried out in 3.5% NaCl solution. The SPS-ed FeSiBAlNiCo0.2 HEA reveals the better passivity with low passive current density, and the higher pitting resistance with wide passive region.

Surface structure and electrochemical characteristics of Ti-V-Cr bcc-type solid solution alloys sintered with Ni

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsuji, Yoichiro; Yamamoto, Osamu; Matsuda, Hiromu

2000-07-01

Ti-V-Cr bcc-type solid solution alloys can absorb a large amount of hydrogen and be applied to active materials of the negative electrode in Ni-MH batteries. However, because of the insolubility of Ni into these alloys, the electrochemical characteristics like discharge capacity and cycle life were poor. In order to increase the discharge capacity of hydrogen absorbing alloy electrodes, Ti-V-Cr bcc-type alloy powders were sintered with Ni in order to form Ni contained surface layer on the alloy surface. As sintering temperature rose up, the surface composition changed from TiNi to Ti{sub 2}Ni. TiNi surface layer showed better electrochemical characteristics. Formore » the Ni adding method, Ni electroless plating was preferred because of good adhesion. As a result of optimized conditions, a discharge capacity of 570 mAh/g and an improvement of cycle life were achieved.« less

Processing and fabrication of mixed uranium/refractory metal carbide fuels with liquid-phase sintering

NASA Astrophysics Data System (ADS)

Knight, Travis W.; Anghaie, Samim

2002-11-01

Optimization of powder processing techniques were sought for the fabrication of single-phase, solid-solution mixed uranium/refractory metal carbide nuclear fuels - namely (U, Zr, Nb)C. These advanced, ultra-high temperature nuclear fuels have great potential for improved performance over graphite matrix, dispersed fuels tested in the Rover/NERVA program of the 1960s and early 1970s. Hypostoichiometric fuel samples with carbon-to-metal ratios of 0.98, uranium metal mole fractions of 5% and 10%, and porosities less than 5% were fabricated. These qualities should provide for the longest life and highest performance capability for these fuels. Study and optimization of processing methods were necessary to provide the quality assurance of samples for meaningful testing and assessment of performance for nuclear thermal propulsion applications. The processing parameters and benefits of enhanced sintering by uranium carbide liquid-phase sintering were established for the rapid and effective consolidation and formation of a solid-solution mixed carbide nuclear fuel.

Synthesis of One-Dimensional and Hyperbranched Nanomaterials for Lithium-Ion Battery Solid Electrolytes

NASA Astrophysics Data System (ADS)

Yang, Ting

Lithium-ion batteries can fail and catch fire when overcharged, exposed to high temperatures or short-circuited due to the highly flammable organic liquid used in the electrolyte. Using inorganic solid electrolyte materials can potentially improve the safety factor. Additionally, nanostructured electrolyte materials may further enhanced performance by taking advantage of their large aspect ratio. In this work, the synthesis of two promising nanostructured solid electrolyte materials was explored. Amorphous lithium niobate nanowires were synthesized through the decomposition of a niobium-containing complex in a structure-directing solvent using a reflux method. Lithium lanthanum titanate was obtained via solid state reaction with titanium oxide nanowires as the titanium precursor, but the nanowire morphology could not be preserved due to high temperature sintering. Hyperbranched potassium lanthanum titanate was synthesized through hydrothermal route. This was the first time that hyperbranched nanowires with perovskite structure were made without any catalyst or substrate. This result has the potential to be applied to other perovskite materials.

The Effects of Bismuth Oxide on Microstructures and Magnetic Properties of Mn-Mg-Al Ferrites

NASA Astrophysics Data System (ADS)

Nekouee, Kh. A.; Rahimi, A. H.; Haghighi, M. Alineghad; Ehsani, N.

2018-04-01

In the present paper, the effects of bismuth oxide as an additive on microstructure and magnetic properties of Mg0.9Mn0.1Al0.4Fe1.6O4 were investigated. Mg-Mn-Al ferrite powders were prepared by the conventional solid state synthesis method. Two different amounts of bismuth oxide (2.5 wt.% and 5 wt.%) were utilized as the sintering aid and their microstructure and physical properties were compared to those of the sample without additives. X-ray diffraction (XRD) analysis indicated that crystal lattice distortion due to the microstructural constraints as the result from incorporation of bismuth oxide into the microstructure was developed by adding bismuth oxide. XRD Rietveld refinement was used to define the cation distribution and to refine the lattice parameter and oxygen parameter for the sample without bismuth oxide as (Mg0.16Mn0.02Al0.15Fe0.77)A(Mg0.74Mn0.08Al0.25Fe0.83)BO4 and 8.3308 Å and 0.2542, respectively. Microstructure studies show that a bismuth rich liquid phase forms during the sintering at 1250°C, which enhances the densification of sintered bodies up to 13% (a relative density of 93%). Magnetization of sintered samples were increased from 21.1 emu/g to 26.2 emu/g upon addition of 2.5 wt.% bismuth oxide and then decreased to 24.9 emu/g when 5 wt.% bismuth oxide was added.

Heterotopic bone formation around sintered porous-surfaced Ti-6Al-4V implants coated with native bone morphogenetic proteins.

PubMed

Simon, Ziv; Deporter, Douglas A; Pilliar, Robert M; Clokie, Cameron M

2006-09-01

Coating endosseous dental implants with growth factors such as bone morphogenetic proteins (BMPs) may be one way to accelerate and/or enhance the quality of osseointegration. The purpose of this study was to investigate in the murine muscle pouch model whether sintered porous-surfaced titanium alloy implants coated with BMPs would lead to heterotopic bone formation around and within the implant surface geometry. Porous-surfaced dental implants were coated with partially purified native human BMPs, with or without a carrier of Poloxamer 407 (BASF Corp., Parsippany, NJ), placed in gelatin capsules and implanted into the hindquarter muscles of mice. Mice were euthanized after 28 days. Sections of retrieved specimens were subsequently prepared for morphometric analysis of bone formation using backscatter electron microscopic images. Human BMPs, either with or without the carrier of Poloxamer 407, led to bone formation within and outside of the sintered porous implant surface. When the sintered implant surface region was subdivided into inner and outer halves, similar levels of bone ingrowth and contact were seen in the 2 halves. Evidence of bone formation to the depth of the solid implant core (i.e., the deepest level possible) also was seen. Sintered porous-surfaced dental implants can be used as substrate for partially purified BMPs in the murine muscle pouch model. With the addition of these osteoinductive factors, the porous implant surface supported bone formation within the surface porosity provided, in some instances, all the way to the solid implant core. The addition of growth factors to a sintered porous surface may be an efficient method for altering locally the healing sequence and quality of bone associated with osseointegration of bone-interfacing implants.

Preparation and Properties of (YCa)(TiMn)O3−δ Ceramics Interconnect of Solid Oxide Fuel Cells

PubMed Central

Liou, Yi-Cheng; Tsai, Wen-Chou; Yen, Hao-Hsuan; Chang, Yung-Chia

2015-01-01

(YCa)(TiMn)O3–δ ceramics prepared using a reaction-sintering process were investigated. Without any calcination involved, the mixture of raw materials was pressed and sintered directly. Y2Ti2O7 instead of YTiO3 formed when a mixture of Y2O3 and TiO2 with Y/Ti ratio 1/1 were sintered in air. Y2Ti2O7, YTiO2.085 and some unknown phases were detected in Y0.6Ca0.4Ti0.6Mn0.4O3–δ. Monophasic Y0.6Ca0.4Ti0.4Mn0.6O3–δ ceramics were obtained after 1400–1500 °C sintering. Dense Y0.6Ca0.4Ti0.4Mn0.6O3–δ with a density 4.69 g/cm3 was observed after 1500 °C/4 h sintering. Log σ for Y0.6Ca0.4Ti0.6Mn0.4O3–δ increased from –3.73 Scm–1 at 350 °C to –2.14 Scm–1 at 700 °C. Log σ for Y0.6Ca0.4Ti0.4Mn0.6O3–δ increased from –2.1 Scm–1 at 350 °C to –1.36 Scm–1 at 700 °C. Increasing Mn content decreased activation energy Ea and increased electrical conductivity. Reaction-sintering process is proved to be a simple and effective method to obtain (YCa)(TiMn)O3–δ ceramics for interconnects in solid oxide fuel cells. PMID:28793436

Selective Laser Sintering of Nano Al2O3 Infused Polyamide

PubMed Central

Warnakula, Anthony; Singamneni, Sarat

2017-01-01

Nano Al2O3 polyamide composites are evaluated for processing by selective laser sintering. A thermal characterization of the polymer composite powders allowed us to establish the possible initial settings. Initial experiments are conducted to identify the most suitable combinations of process parameters. Based on the results of the initial trials, more promising ranges of different process parameters could be identified. The post sintering characterization showed evidence of sufficient inter-particle sintering and intra-layer coalescence. While the inter-particle coalescence gradually improved, the porosity levels slightly decreased with increasing laser power. The nano-filler particles tend to agglomerate around the beads along the solid tracks, possibly due to Van der Walls forces. The tensile stress results showed an almost linear increase with increasing nano-filler content. PMID:28773220

Evaluation of Chemically-Sensitive Field-Effect Transistors for Detection of Organophosphorus Compounds

DTIC Science & Technology

1989-12-05

during past decade. In order to understand the basic operation of these sensors, especially of the CHEMFET, the appropriate background information will...during the past decade for detecting organophosphorus compounds, the chemically- sensitive thin films investigated in this thesis, and finally, the...reactivate the phosphorylated cholinesterase enzyme. Solid State Chemical Sensors During the past decade, a number of solid state chemical sensors have been

Optically triggered high voltage switch network and method for switching a high voltage

DOEpatents

El-Sharkawi, Mohamed A.; Andexler, George; Silberkleit, Lee I.

1993-01-19

An optically triggered solid state switch and method for switching a high voltage electrical current. A plurality of solid state switches (350) are connected in series for controlling electrical current flow between a compensation capacitor (112) and ground in a reactive power compensator (50, 50') that monitors the voltage and current flowing through each of three distribution lines (52a, 52b and 52c), which are supplying three-phase power to one or more inductive loads. An optical transmitter (100) controlled by the reactive power compensation system produces light pulses that are conveyed over optical fibers (102) to a switch driver (110') that includes a plurality of series connected optical triger circuits (288). Each of the optical trigger circuits controls a pair of the solid state switches and includes a plurality of series connected resistors (294, 326, 330, and 334) that equalize or balance the potential across the plurality of trigger circuits. The trigger circuits are connected to one of the distribution lines through a trigger capacitor (340). In each switch driver, the light signals activate a phototransistor (300) so that an electrical current flows from one of the energy reservoir capacitors through a pulse transformer (306) in the trigger circuit, producing gate signals that turn on the pair of serially connected solid state switches (350).

A new insight into high-strength Ti62Nb12.2Fe13.6Co6.4Al5.8 alloys with bimodal microstructure fabricated by semi-solid sintering

PubMed Central

Liu, L. H.; Yang, C.; Kang, L. M.; Qu, S. G.; Li, X. Q.; Zhang, W. W.; Chen, W. P.; Li, Y. Y.; Li, P. J.; Zhang, L. C.

2016-01-01

It is well known that semi-solid forming could only obtain coarse-grained microstructure in a few alloy systems with a low melting point, such as aluminum and magnesium alloys. This work presents that semi-solid forming could also produce novel bimodal microstructure composed of nanostructured matrix and micro-sized (CoFe)Ti2 twins in a titanium alloy, Ti62Nb12.2Fe13.6Co6.4Al5.8. The semi-solid sintering induced by eutectic transformation to form a bimodal microstructure in Ti62Nb12.2Fe13.6Co6.4Al5.8 alloy is a fundamentally different approach from other known methods. The fabricated alloy exhibits high yield strength of 1790 MPa and plastic strain of 15.5%. The novel idea provides a new insight into obtaining nano-grain or bimodal microstructure in alloy systems with high melting point by semi-solid forming and into fabricating high-performance metallic alloys in structural applications. PMID:27029858

Average current per vacuum-arc cathode spot and spot velocity in a magnetic field on a CuCr50/50 nanocomposite

NASA Astrophysics Data System (ADS)

Zabello, K. K.; Poluyanova, I. N.; Yakovlev, V. V.; Shkol'nik, S. M.

2017-11-01

It has been shown that such cathode spot characteristics as the average current per spot and its dependence on tangential magnetic-field induction B t and the spot velocity and its dependence on B t for two CuCr50/50 specimens with very different structures (nanocomposite and "solid-state sintered" composite) almost coincide if the surface of contacts has been totally remelted before measurements with the use of moderate arc currents in the process of conditioning.

Apparatus for controlling fluidized beds

DOEpatents

Rehmat, A.G.; Patel, J.G.

1987-05-12

An apparatus and process are disclosed for control and maintenance of fluidized beds under non-steady state conditions. An ash removal conduit is provided for removing solid particulates from a fluidized bed separate from an ash discharge conduit in the lower portion of the grate supporting such a bed. The apparatus and process of this invention is particularly suitable for use in ash agglomerating fluidized beds and provides control of the fluidized bed before ash agglomeration is initiated and during upset conditions resulting in stable, sinter-free fluidized bed maintenance. 2 figs.

Impact of densification on microstructure and transport properties of CaFe5O7

NASA Astrophysics Data System (ADS)

Delacotte, C.; Hébert, S.; Hardy, V.; Bréard, Y.; Maki, R.; Mori, T.; Pelloquin, D.

2016-04-01

Monophasic CaFe5O7 ceramic has been synthesized by solid state route. Its microstructural features have been studied by diffraction techniques and electron microscopy images before and after Spark Plasma Sintering (SPS) annealings. This work is completed by measurements of electrical and thermal properties. Especially, attention is focused around the structural and electronic transition at 360 K for which specific heat measurements have revealed a sharp peak. Densification by SPS techniques led to a significant improvement of electrical conductivity above 360 K.

The properties of LaSrМnO3 powders synthesized at various regimes

NASA Astrophysics Data System (ADS)

Mikhailov, M.; Sokolovskiy, A.; Vlasov, V.; Smolin, A.

2017-09-01

For the first time the concentration of ferromagnetic and paramagnetic phases in LaSrMnO3 compounds has been defined using diffuse reflection and absorption spectra in the visible and near-infrared regions. The compounds as powders were synthesized by heating La2O3/SrCO3/МnСO3 mixtures at 1200 °C which is less than their sintering temperature. The possibility to obtain LaSrMnO3 powders by solid state synthesis for smart coatings was shown.

Toward garnet electrolyte–based Li metal batteries: An ultrathin, highly effective, artificial solid-state electrolyte/metallic Li interface

PubMed Central

Fu, Kun (Kelvin); Gong, Yunhui; Liu, Boyang; Zhu, Yizhou; Xu, Shaomao; Yao, Yonggang; Luo, Wei; Wang, Chengwei; Lacey, Steven D.; Dai, Jiaqi; Chen, Yanan; Mo, Yifei; Wachsman, Eric; Hu, Liangbing

2017-01-01

Solid-state batteries are a promising option toward high energy and power densities due to the use of lithium (Li) metal as an anode. Among all solid electrolyte materials ranging from sulfides to oxides and oxynitrides, cubic garnet–type Li7La3Zr2O12 (LLZO) ceramic electrolytes are superior candidates because of their high ionic conductivity (10−3 to 10−4 S/cm) and good stability against Li metal. However, garnet solid electrolytes generally have poor contact with Li metal, which causes high resistance and uneven current distribution at the interface. To address this challenge, we demonstrate a strategy to engineer the garnet solid electrolyte and the Li metal interface by forming an intermediary Li-metal alloy, which changes the wettability of the garnet surface (lithiophobic to lithiophilic) and reduces the interface resistance by more than an order of magnitude: 950 ohm·cm2 for the pristine garnet/Li and 75 ohm·cm2 for the surface-engineered garnet/Li. Li7La2.75Ca0.25Zr1.75Nb0.25O12 (LLCZN) was selected as the solid-state electrolyte (SSE) in this work because of its low sintering temperature, stabilized cubic garnet phase, and high ionic conductivity. This low area-specific resistance enables a solid-state garnet SSE/Li metal configuration and promotes the development of a hybrid electrolyte system. The hybrid system uses the improved solid-state garnet SSE Li metal anode and a thin liquid electrolyte cathode interfacial layer. This work provides new ways to address the garnet SSE wetting issue against Li and get more stable cell performances based on the hybrid electrolyte system for Li-ion, Li-sulfur, and Li-oxygen batteries toward the next generation of Li metal batteries. PMID:28435874

Toward garnet electrolyte–based Li metal batteries: An ultrathin, highly effective, artificial solid-state electrolyte/metallic Li interface

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fu, Kun; Gong, Yunhui; Liu, Boyang

Solid-state batteries are a promising option toward high energy and power densities due to the use of lithium (Li) metal as an anode. Among all solid electrolyte materials ranging from sulfides to oxides and oxynitrides, cubic garnet–type Li 7La 3Zr 2O 12 (LLZO) ceramic electrolytes are superior candidates because of their high ionic conductivity (10 -3 to 10 -4 S/cm) and good stability against Li metal. However, garnet solid electrolytes generally have poor contact with Li metal, which causes high resistance and uneven current distribution at the interface. To address this challenge, we demonstrate a strategy to engineer the garnetmore » solid electrolyte and the Li metal interface by forming an intermediary Li-metal alloy, which changes the wettability of the garnet surface (lithiophobic to lithiophilic) and reduces the interface resistance by more than an order of magnitude: 950 ohm·cm2 for the pristine garnet/Li and 75 ohm·cm 2 for the surface-engineered garnet/Li. Li 7La 2.75Ca 0.25Zr 1.75Nb 0.25O 12 (LLCZN) was selected as the solid-state electrolyte (SSE) in this work because of its low sintering temperature, stabilized cubic garnet phase, and high ionic conductivity. This low area-specific resistance enables a solid-state garnet SSE/Li metal configuration and promotes the development of a hybrid electrolyte system. The hybrid system uses the improved solid-state garnet SSE Li metal anode and a thin liquid electrolyte cathode interfacial layer. This work provides new ways to address the garnet SSE wetting issue against Li and get more stable cell performances based on the hybrid electrolyte system for Li-ion, Li-sulfur, and Li-oxygen batteries toward the next generation of Li metal batteries.« less

Toward garnet electrolyte–based Li metal batteries: An ultrathin, highly effective, artificial solid-state electrolyte/metallic Li interface

DOE PAGES

Fu, Kun; Gong, Yunhui; Liu, Boyang; ...

2017-04-07

Solid-state batteries are a promising option toward high energy and power densities due to the use of lithium (Li) metal as an anode. Among all solid electrolyte materials ranging from sulfides to oxides and oxynitrides, cubic garnet–type Li 7La 3Zr 2O 12 (LLZO) ceramic electrolytes are superior candidates because of their high ionic conductivity (10 -3 to 10 -4 S/cm) and good stability against Li metal. However, garnet solid electrolytes generally have poor contact with Li metal, which causes high resistance and uneven current distribution at the interface. To address this challenge, we demonstrate a strategy to engineer the garnetmore » solid electrolyte and the Li metal interface by forming an intermediary Li-metal alloy, which changes the wettability of the garnet surface (lithiophobic to lithiophilic) and reduces the interface resistance by more than an order of magnitude: 950 ohm·cm2 for the pristine garnet/Li and 75 ohm·cm 2 for the surface-engineered garnet/Li. Li 7La 2.75Ca 0.25Zr 1.75Nb 0.25O 12 (LLCZN) was selected as the solid-state electrolyte (SSE) in this work because of its low sintering temperature, stabilized cubic garnet phase, and high ionic conductivity. This low area-specific resistance enables a solid-state garnet SSE/Li metal configuration and promotes the development of a hybrid electrolyte system. The hybrid system uses the improved solid-state garnet SSE Li metal anode and a thin liquid electrolyte cathode interfacial layer. This work provides new ways to address the garnet SSE wetting issue against Li and get more stable cell performances based on the hybrid electrolyte system for Li-ion, Li-sulfur, and Li-oxygen batteries toward the next generation of Li metal batteries.« less

Visible light photoreactivity from hybridization states between carbon nitride bandgap states and valence states in Nb and Ti oxides

NASA Astrophysics Data System (ADS)

Lee, Hosik; Ohno, Takahisa

2013-03-01

For better efficiency as photocatalysts, N-doping for visible light reactivity has been intensively studied in Lamellar niobic and titanic solid acids (HNb3O8, H2Ti4O9), and its microscopic structures have been debated in this decade. We calculate the layered solid acids' structures and bandgaps. Bandgap reduction by carbon nitride adsorption in interlayer space is observed computationally. It originates from localized nitrogen states which form delocalized top-valence states by hybridizing with the host oxygen states and can contribute to photo-current.

Low sintering temperature glass waste forms for sequestering radioactive iodine

DOEpatents

Nenoff, Tina M.; Krumhansl, James L.; Garino, Terry J.; Ockwig, Nathan W.

2012-09-11

Materials and methods of making low-sintering-temperature glass waste forms that sequester radioactive iodine in a strong and durable structure. First, the iodine is captured by an adsorbant, which forms an iodine-loaded material, e.g., AgI, AgI-zeolite, AgI-mordenite, Ag-silica aerogel, ZnI.sub.2, CuI, or Bi.sub.5O.sub.7I. Next, particles of the iodine-loaded material are mixed with powdered frits of low-sintering-temperature glasses (comprising various oxides of Si, B, Bi, Pb, and Zn), and then sintered at a relatively low temperature, ranging from 425.degree. C. to 550.degree. C. The sintering converts the mixed powders into a solid block of a glassy waste form, having low iodine leaching rates. The vitrified glassy waste form can contain as much as 60 wt % AgI. A preferred glass, having a sintering temperature of 500.degree. C. (below the silver iodide sublimation temperature of 500.degree. C.) was identified that contains oxides of boron, bismuth, and zinc, while containing essentially no lead or silicon.

Densification of Zirconia with Borates.

DTIC Science & Technology

1980-01-24

solid electrolytes for fuel cell and oxygen sensor applications.1 ’ 2 The sintering temperatures for commercial quality stabilized zirconia powders are...in the temperature range 1450-1500C). A few studies were also made using a much coarser particle size (- 1-2 pm ave.) cubic stabilized zirconia ... powder , "Zircoa B" [Zirconia Corp. of America]. The additives used as sintering aids were reagent grade horic anhydride, calcium metaborate and calcium

Effect of coating density on oxidation resistance and Cr vaporization from solid oxide fuel cell interconnects

NASA Astrophysics Data System (ADS)

Talic, Belma; Falk-Windisch, Hannes; Venkatachalam, Vinothini; Hendriksen, Peter Vang; Wiik, Kjell; Lein, Hilde Lea

2017-06-01

Manganese cobalt spinel oxides are promising materials for protective coatings for solid oxide fuel cell (SOFC) interconnects. To achieve high density such coatings are often sintered in a two-step procedure, involving heat treatment first in reducing and then in oxidizing atmospheres. Sintering the coating inside the SOFC stack during heating would reduce production costs, but may result in a lower coating density. The importance of coating density is here assessed by characterization of the oxidation kinetics and Cr evaporation of Crofer 22 APU with MnCo1.7Fe0.3O4 spinel coatings of different density. The coating density is shown to have minor influence on the long-term oxidation behavior in air at 800 °C, evaluated over 5000 h. Sintering the spinel coating in air at 900 °C, equivalent to an in-situ heat treatment, leads to an 88% reduction of the Cr evaporation rate of Crofer 22 APU in air-3% H2O at 800 °C. The air sintered spinel coating is initially highly porous, however, densifies with time in interaction with the alloy. A two-step reduction and re-oxidation heat treatment results in a denser coating, which reduces Cr evaporation by 97%.

Sintering in Ceramics and Solid Oxide Fuel Cells

NASA Astrophysics Data System (ADS)

Hunt, Clay Dale

Nature's propensity to minimize energy, and the change in energy with respect to position, drives diffusion. Diffusion is a means by which mass transport resulting in the bonding of the particles of a powder compact can be achieved without melting. This phenomenon occurs in powdered materials near their melting temperature, and is referred to as "sintering". Because of the extreme melting temperature of some materials, sintering might be the only practical means of processing. The complexity and subtlety of sintering ceramics motivated the evaluation of empirical data and existing sintering models. This project examined polycrystalline cubic-zirconia sintering with and without transition-metal oxide additions that change sintering behavior. This study was undertaken to determine how sintering aids affect the driving force, and activation energy, the energy barrier that must be overcome in order for an atom or ion to diffuse, of the densification occurring during sintering. Examination of commercially-available cubic-zirconia powder sintering behavior was undertaken with dilatometry, which allows monitoring of the length change a material undergoes as it sinters, and with scanning electron microscopy, which facilitates the study of sintered-sample microstructure. MATLAB algorithms quantifying sintering results were developed. Results from this work include proposed definitions of a 26-year-old undefined function of density factor in a well-accepted mathematical model of sintering. These findings suggest activation energy is not changing with density, as is suggested by recent published results. The first numerical integration of the studied sintering model has been performed. With these tools, a measure of the activation energy of densification of cubic-zirconia with and without the addition of cobalt-oxide as a sintering aid has been performed. The resulting MATLAB algorithms can be used in future sintering studies. It is concluded that sintering enhancement achieved with cobalt-oxide addition comes from reduction in activation energy of densification of cubic-zirconia. Further, it is suggested that the activation energy of densification does not change with material density. This conclusion is supported by the sensitivity of the numerical integration of the aforementioned sintering model to changes in activation energy.

Techno-Economic Assessment of Recycling BOF Offgas Cleaning System Solid Wastes by Using Zinc-Free Scrap

NASA Astrophysics Data System (ADS)

Ma, Naiyang

High zinc concentration in basic oxygen furnace (BOF) steelmaking offgas (OG) cleaning system solid wastes is one of the main barriers for recycling of the solid wastes in sintering — blast furnace ironmaking process. One of the possible solutions is to utilize zinc-free scrap in BOF steelmaking so that the BOF OG solid wastes will not be contaminated with zinc and can be recycled through sintering — blast furnace ironmaking. This paper describes a model for helping to decide whether to use zinc-free scrap in a BOF process. A model computing marginal price increment of zinc-free scrap is developed. The marginal price increment is proportional to value change of the BOF OG solid wastes after and before using zinc-free scrap, to ratio of BOF solid waste rate to purchased galvanized scrap rate, and to price of galvanized scrap. Due to the variations of consumption rate of purchased galvanized scrap and home galvanized scrap, iron ore price, landfill cost, and price of purchased galvanized scrap, using zinc-free scrap in a BOF process might be economically feasible for some ironmaking and steelmaking plants or in some particular market circumstances.

Reactive power compensator

DOEpatents

El-Sharkawi, Mohamed A.; Venkata, Subrahmanyam S.; Chen, Mingliang; Andexler, George; Huang, Tony

1992-01-01

A system and method for determining and providing reactive power compensation for an inductive load. A reactive power compensator (50,50') monitors the voltage and current flowing through each of three distribution lines (52a, 52b, 52c), which are supplying three-phase power to one or more inductive loads. Using signals indicative of the current on each of these lines when the voltage waveform on the line crosses zero, the reactive power compensator determines a reactive power compensator capacitance that must be connected to the lines to maintain a desired VAR level, power factor, or line voltage. Alternatively, an operator can manually select a specific capacitance for connection to each line, or the capacitance can be selected based on a time schedule. The reactive power compensator produces control signals, which are coupled through optical fibers (102/106) to a switch driver (110, 110') to select specific compensation capacitors (112) for connections to each line. The switch driver develops triggering signals that are supplied to a plurality of series-connected solid state switches (350), which control charge current in one direction in respect to ground for each compensation capacitor. During each cycle, current flows from ground to charge the capacitors as the voltage on the line begins to go negative from its positive peak value. The triggering signals are applied to gate the solid state switches into a conducting state when the potential on the lines and on the capacitors reaches a negative peak value, thereby minimizing both the potential difference and across the charge current through the switches when they begin to conduct. Any harmonic distortion on the potential and current carried by the lines is filtered out from the current and potential signals used by the reactive power compensator so that it does not affect the determination of the required reactive compensation.

Reactive Power Compensator.

DOEpatents

El-Sharkawi, M.A.; Venkata, S.S.; Chen, M.; Andexler, G.; Huang, T.

1992-07-28

A system and method for determining and providing reactive power compensation for an inductive load. A reactive power compensator (50,50') monitors the voltage and current flowing through each of three distribution lines (52a, 52b, 52c), which are supplying three-phase power to one or more inductive loads. Using signals indicative of the current on each of these lines when the voltage waveform on the line crosses zero, the reactive power compensator determines a reactive power compensator capacitance that must be connected to the lines to maintain a desired VAR level, power factor, or line voltage. Alternatively, an operator can manually select a specific capacitance for connection to each line, or the capacitance can be selected based on a time schedule. The reactive power compensator produces control signals, which are coupled through optical fibers (102/106) to a switch driver (110, 110') to select specific compensation capacitors (112) for connections to each line. The switch driver develops triggering signals that are supplied to a plurality of series-connected solid state switches (350), which control charge current in one direction in respect to ground for each compensation capacitor. During each cycle, current flows from ground to charge the capacitors as the voltage on the line begins to go negative from its positive peak value. The triggering signals are applied to gate the solid state switches into a conducting state when the potential on the lines and on the capacitors reaches a negative peak value, thereby minimizing both the potential difference and across the charge current through the switches when they begin to conduct. Any harmonic distortion on the potential and current carried by the lines is filtered out from the current and potential signals used by the reactive power compensator so that it does not affect the determination of the required reactive compensation. 26 figs.

Solid oxide fuel cell with multi-unit construction and prismatic design

DOEpatents

McPheeters, Charles C.; Dees, Dennis W.; Myles, Kevin M.

1999-01-01

A single cell unit of a solid oxide fuel cell that is individually fabricated and sintered prior to being connected to adjacent cells to form a solid oxide fuel cell. The single cell unit is comprised of a shaped anode sheet positioned between a flat anode sheet and an anode-electrolyte-cathode (A/E/C) sheet, and a shaped cathode sheet positioned between the A/E/C sheet and a cathode-interconnect-anode (C/I/A) sheet. An alternate embodiment comprises a shaped cathode sheet positioned between an A/E/C sheet and a C/I/A sheet. The shaped sheets form channels for conducting reactant gases. Each single cell unit is individually sintered to form a finished sub-assembly. The finished sub-assemblies are connected in electrical series by interposing connective material between the end surfaces of adjacent cells, whereby individual cells may be inspected for defects and interchanged with non-defective single cell units.

Flash sintering of ceramic materials

NASA Astrophysics Data System (ADS)

Dancer, C. E. J.

2016-10-01

During flash sintering, ceramic materials can sinter to high density in a matter of seconds while subjected to electric field and elevated temperature. This process, which occurs at lower furnace temperatures and in shorter times than both conventional ceramic sintering and field-assisted methods such as spark plasma sintering, has the potential to radically reduce the power consumption required for the densification of ceramic materials. This paper reviews the experimental work on flash sintering methods carried out to date, and compares the properties of the materials obtained to those produced by conventional sintering. The flash sintering process is described for oxides of zirconium, yttrium, aluminium, tin, zinc, and titanium; silicon and boron carbide, zirconium diboride, materials for solid oxide fuel applications, ferroelectric materials, and composite materials. While experimental observations have been made on a wide range of materials, understanding of the underlying mechanisms responsible for the onset and latter stages of flash sintering is still elusive. Elements of the proposed theories to explain the observed behaviour include extensive Joule heating throughout the material causing thermal runaway, arrested by the current limitation in the power supply, and the formation of defect avalanches which rapidly and dramatically increase the sample conductivity. Undoubtedly, the flash sintering process is affected by the electric field strength, furnace temperature and current density limit, but also by microstructural features such as the presence of second phase particles or dopants and the particle size in the starting material. While further experimental work and modelling is still required to attain a full understanding capable of predicting the success of the flash sintering process in different materials, the technique non-etheless holds great potential for exceptional control of the ceramic sintering process.

Production technology of an electrolyte for Na/S batteries

NASA Astrophysics Data System (ADS)

Heimke, G.; Mayer, H.; Reckziegel, A.

1982-05-01

The trend to develop a cheap electrochemical electric battery and the development of the Na/S system are discussed. The main element in this type of battery is the beta Al2O3 solid electrolyte. Characteristics for this material of first importance are: specific surface, density of green and of sintered material, absence of cracks, gas permeability, resistance to flexion, purity, electrical conductivity, crystal structure and dimensions. Influence of production method on all these characteristics were investigated, e.g., method of compacting powder, tunnel kiln sintering versus static chamber furnace sintering, sintering inside a container or not, and type of kiln material when sintering in a container. In the stationary chamber furnace, beta alumina ceramics were produced with a density of 3.2 g/cm3, a mechanical strength higher than 160 MPa, and an electrical conductivity of about 0.125 Ohm-1cm-1 at 300 C. The best kiln material proved to be MgO and MgAl2O3.MgO ceramics.

Luminescence Characteristics of ZnGa2O4 Thick Film Doped with Mn2+ and Cr3+ at Various Sintering Temperatures

NASA Astrophysics Data System (ADS)

Cha, Jae Hyeok; Kim, Kyung Hwan; Park, Yong Seo; Kwon, Sang Jik; Choi, Hyung Wook

2007-10-01

ZnGa2O4 phosphor separately doped with Mn2+ and Cr3+ was synthesized by solid-state reaction, and thick films were deposited by screen printing. The X-ray diffraction (XRD) patterns of ZnGa2O4 phosphor thick films show a (311) main peak and a spinal phase. Uniform distribution and filled morphology of the doped ZnGa2O4 phosphor thick films were formed at the sintering temperature of 1100 °C. The CL spectrum of Mn2+-doped ZnGa2O4 shows the main peak of 512 nm green emission with the 4T1→6A1 transition of Mn2+ ions and the CL spectrum of Cr3+-doped ZnGa2O4 shows the main peak of 716 nm red emission with the 2E→4A2 transition of Cr3+ ions.

Effects of Sintering Holding Time on the Structural, Electrical and Magnetic Properties of Zn0.95Ni0.05O

NASA Astrophysics Data System (ADS)

Ginting, M.; Aryanto, D.; Kurniawan, C.; Sari, A. Y.; Subhan, A.; Sudiro, T.; Sebayang, P.; Tarigan, E. R.; Nasruddin, M. N.; Sebayang, K.

2017-05-01

Zn0.95Ni0.05O has been synthesized by mixing 5% mol of NiO into ZnO using solid state reaction and high-speed shaker mill method. The samples were sintered at 900 °C with holding time for 2, 4 and 8 hours. Crystal structure, electrical and magnetic properties of Zn0.95Ni0.05O were characterized by using XRD, I-V, C-V and VSM. XRD results showed that variation of holding time does not change the structure of ZnO and no other secondary phase observed. The value of lattice parameters (a and c) tends to decrease proportionally to the holding time. The Intensity value changes and the peak shifted to a higher 2θ angle due to holding time variation. In general, the conductance of Zn0.95Ni0.05O decreases and the magnetic properties decrease also as the holding time is increased.

Cu3Mo2O9: An Ultralow-Firing Microwave Dielectric Ceramic with Good Temperature Stability and Chemical Compatibility with Aluminum

NASA Astrophysics Data System (ADS)

Wen, Wangxi; Li, Chunchun; Sun, Yihua; Tang, Ying; Fang, Liang

2018-02-01

An ultralow-firing microwave dielectric ceramic Cu3Mo2O9 with orthorhombic structure has been fabricated via a solid-state reaction method. X-ray diffraction analysis, Rietveld refinement, Raman spectroscopy, energy-dispersive spectrometry, and scanning electron microscopy were employed to explore the phase purity, crystal structure, and microstructure. Pure and dense Cu3Mo2O9 ceramics could be obtained in the sintering temperature range from 580°C to 680°C. The sample sintered at 660°C for 4 h exhibited the highest relative density (˜ 97.2%) and best microwave dielectric properties with ɛ r = 7.2, Q × f = 19,300 GHz, and τ f = - 7.8 ppm/°C. Chemical compatibility with aluminum electrodes was also confirmed. All the results suggest that Cu3Mo2O9 ceramic is a promising candidate for use in ultralow-temperature cofired ceramic applications.

Transport Properties of La- doped SrTiO3 Ceramics Prepared Using Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Mehdizadeh Dehkordi, Arash; Bhattacharya, Sriparna; Tritt, Terry M.; Alshareef, Husam N.

2012-02-01

In this work, thermoelectric transport properties of La-doped SrTiO3 ceramics prepared using conventional solid state reaction and spark plasma sintering have been investigated. Room temperature power factor of single crystal strontium titanate (SrTiO3), comparable to that of Bi2Te3, has brought new attention to this perovskite-type transition metal-oxide as a potential n-type thermoelectric for high temperature applications. Electronic properties of this model complex oxide, SrTiO3 (ABO3), can be tuned in a wide range through different doping mechanisms. In addition to A site (La-doped) or B site (Nb-doped) substitutional doping, introducing oxygen vacancies plays an important role in electrical and thermal properties of these structures. Having multiple doping mechanisms makes the transport properties of these perovskites more dependent on preparation parameters. The effect of these synthesis parameters and consolidation conditions on the transport properties of these materials has been studied.

Effect of structural phase transformation in FeGaO{sub 3} on its magnetic and ferroelectric properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lone, A. G., E-mail: agl221986@gmail.com; Bhowmik, R. N.

2015-06-24

We investigate the structural phase transformation from orthorhombic to rhombohedral structure in FeGaO{sub 3} by adopting a combined effect of mechanical alloying/milling and solid state sintering techniques. The structural phase formation of the FeGaO{sub 3} compound has been characterized by X-ray diffraction pattern. Mechanical milling played a significant role on the stabilization of rhombohedral phase in FeGaO{sub 3}, where as high temperature sintering stabilized the system in orthorhombic phase. A considerable difference has been observed in magnetic and ferroelectric properties of the system in two phases. The system in rhombohedral (R-3c) phase exhibited better ferromagnetic and of ferroelectric properties atmore » room temperature in comparison to orthorhombic (Pc2{sub 1}n) phase. The rhombohedral phase appears to be good for developing metal doped hematite system for spintronics applications and in that process mechanical milling played an important role.« less

Relationship between fabrication method and chemical stability of Ni-BaZr0.8Y0.2O3-δ membrane

NASA Astrophysics Data System (ADS)

Fang, Shumin; Wang, Siwei; Brinkman, Kyle S.; Su, Qing; Wang, Haiyan; Chen, Fanglin

2015-03-01

NiO effectively promotes the sintering of highly refractory Y-doped BaZrO3 (BZY) through the formation of BaY2NiO5, providing a simple and cost-effective method for the fabrication of dense BZY electrolyte and Ni-BZY hydrogen separation membrane at ∼1400 °C. Unfortunately, insulating BaCO3 and Y2O3 phases formed on the surface of BZY and Ni-BZY prepared by solid state reaction method with NiO after annealing in wet CO2. Ni-BZY membranes prepared from different methods suffered different degree of performance loss in wet H2 at 900 °C. The chemical instability of Ni-BZY is attributed to the formation of a secondary phase (BaY2O4) generated from the reduction of BaY2NiO5 in H2 during the sintering process. Both BaY2O4 and BaY2NiO5 react with H2O, and CO2 at elevated temperatures, generating insulating Ba(OH)2 and BaCO3 phases, respectively. The less BaY2O4 is formed in the fabrication process, the better chemical stability the Ni-BZY membranes possess. Therefore, a new Ni-BZY membrane is prepared through a judicial combination of BZY powders prepared from combined EDTA-citric and solid state reaction methods, and demonstrates exceptional chemical stability in H2O and CO2, enabling stable and even improved hydrogen flux in wet 50% CO2 at 900 °C.

Effect of the MgO on microstructure and optical properties of TAG (Tb3Al5O12) transparent ceramics using hot isostatic pressing

NASA Astrophysics Data System (ADS)

Zhang, Shouyi; Liu, Peng; Xu, Xiaodong; Zhang, Jian

2018-06-01

In this work, the TAG transparent ceramics doped with 0.4 wt.% TEOS and different concentration of MgO were fabricated by a reactive sintering process under vacuum sintering combined with hot isostatic pressing (HIP) treatment. The effect of MgO on the microstructure evolution and optical properties of delivered ceramics were investigated. The results showed that the TAG ceramics doped with 0.4 wt.% TEOS and 0.1 wt.% MgO exhibited the optimum optical transmittance, which can reach about 81% in the visible and near-infrared (NIR) regions. The addition of MgO inhibited the grain growth and accelerated the densification of TAG ceramic at the sintering temperature reached about 1600 °C.

Processing and properties of SiC whisker reinforced Si sub 3 N sub 4 ceramic matrix composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nunn, S.D.

1991-01-01

Silicon carbide whiskers reinforced silicon nitride ceramic matrix composites were pressureless sintered to high density by liquid phase sintering. Important processing parameters included: whisker dispersion by ultrasonic shear homogenization, particle refinement by attrition milling, pressure slip casting to obtain high greed densities, and sintering in a protective powder bed to limit decomposition. Composites with a {beta}20-Si{sub 3}N{sub 4} solid solution matrix containing 20 vol.% SiC whiskers were sintered to 98-100% theoretical density; composites having a Si{sub 3}N{sub 4} matrix containing YAG sintering aid were sintered to 98% of the theoretical density with 20 vol.% SiC whiskers, and 94% density withmore » 30 vol.% SiC whiskers. Analysis of the pressureless sintered composites revealed orientation of the SiC whiskers and the Si{sub 3}N{sub 4} matrix grains. The mechanical properties of hot pressed Si{sub 3}N{sub 4} composites reinforced with 20 vol.% SiC whiskers were shown to depend on the characteristics of the intergranular phase. Variations in the properties of the composites were analyzed in terms of the amount and morphology of the secondary phase, and the development of internal residual stresses due to the thermal expansion mismatch between the sintering aid phase at the grain boundaries.« less

Putting Cocrystal Stoichiometry to Work: A Reactive Hydrogen-Bonded "Superassembly" Enables Nanoscale Enlargement of a Metal-Organic Rhomboid via a Solid-State Photocycloaddition.

PubMed

Chu, Qianli; Duncan, Andrew J E; Papaefstathiou, Giannis S; Hamilton, Tamara D; Atkinson, Manza B J; Mariappan, S V Santhana; MacGillivray, Leonard R

2018-04-11

Enlargement of a self-assembled metal-organic rhomboid is achieved via the organic solid state. The solid-state synthesis of an elongated organic ligand was achieved by a template directed [2 + 2] photodimerization in a cocrystal. Initial cocrystals obtained of resorcinol template and reactant alkene afforded a 1:2 cocrystal with the alkene in a stacked yet photostable geometry. Cocrystallization performed in the presence of excess template resulted in a 3:2 cocrystal composed of novel discrete 10-component hydrogen-bonded "superassemblies" wherein the alkenes undergo a head-to-head [2 + 2] photodimerization. Isolation and reaction of elongated photoproduct with Cu(II) ions afforded a metal-organic rhomboid of nanoscale dimensions that hosts small molecules in the solid state as guests.

Physical, mechanical and electrochemical characterization of all-perovskite intermediate temperature solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Mohammadi, Alidad

Strontium- and magnesium-doped lanthanum gallate (LSGM) has been considered as a promising electrolyte for solid oxide fuel cell (SOFC) systems in recent years due to its high ionic conductivity and chemical stability over a wide range of oxygen partial pressures and temperatures. This research describes synthesis, physical and mechanical behavior, electrochemical properties, phase evolution, and microstructure of components of an all-perovskite anode-supported intermediate temperature solid oxide fuel cell (ITSOFC), based on porous La 0.75Sr0.25Cr0.5Mn0.5O3 (LSCM) anode, La0.8Sr0.2Ga0.8Mg0.2O 2.8 (LSGM) electrolyte, and porous La0.6Sr0.4Fe 0.8Co0.2O3 (LSCF) cathode. The phase evolution of synthesized LSGM and LSCM powders has been investigated, and it has been confirmed that there is no reaction between LSGM and LSCM at sintering temperature. Using different amounts of poreformers and binders as well as controlling firing temperature, porosity of the anode was optimized while still retaining good mechanical integrity. The effect of cell operation conditions under dry hydrogen fuel on the SOFC open circuit voltage (OCV) and cell performance were also investigated. Characterization study of the synthesized LSGM indicates that sintering at 1500°C obtains higher electrical conductivity compared to the currently published results, while conductivity of pellets sintered at 1400°C and 1450°C would be slightly lower. The effect of sintering temperature on bulk and grain boundary resistivities was also discussed. The mechanical properties, such as hardness, Young's modulus, fracture toughness and modulus of rupture of the electrolyte were determined and correlated with scanning electron microscopy (SEM) morphological characterization. Linear thermal expansion and thermal expansion coefficient of LSGM were also measured.

Sol-gel synthesis of lithium metatitanate as tritium breeding material under different sintering conditions

NASA Astrophysics Data System (ADS)

Lu, Wei; Wang, Jing; Pu, Wenjing; Li, Kaiping; Ma, Shubing; Wang, Weihua

2018-04-01

Lithium metatitanate (Li2TiO3) is a promising tritium breeding material candidate for solid blanket of D-T fusion reactors, due to its high mechanical strength, chemical stability, and tritium release rate. In this paper, Li2TiO3 powder with homogeneous crystal structure is synthesized by sol-gel method. The chemical reactions in gel thermal cracking and sintering process are studied by thermo gravimetric/differential scanning calorimetry (TG-DSC). The relationship between the sintering condition and the particle/grain size is characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Results show that below 673 K the gel precursor is completely decomposed and Li2TiO3 phase initially forms. The LiTiO2 by-product formed under the reductive atmosphere in muffle furnace, could be oxidized continually to Li2TiO3 at higher sintering temperature (≥1273 K) for longer sintering time (≥10 h). Both grain and particle sizes rely on a linear growth with the increase of sintering time at 1273 K. Over 1473 K, significant agglomerations exist among particles. The optimal sintering condition is selected as 1273 K for 10 h, for the purer Li2TiO3 phase (>99%), smaller grain and particle size.

77 FR 51046 - Certain Sintered Rare Earth Magnets, Methods of Making Same and Products Containing Same; Notice...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-08-23

... INTERNATIONAL TRADE COMMISSION [Docket No. 2908] Certain Sintered Rare Earth Magnets, Methods of... Certain Sintered Rare Earth Magnets, Methods of Making Same and Products Containing Same, DN 2908; the... importation, and the sale within the United States after importation of certain sintered rare earth magnets...

Rapid Sintering of Li₂O-Nb₂O₅-TiO₂ Solid Solution by Air Pressure Control and Clarification of Its Mechanism.

PubMed

Nakano, Hiromi; Kamimoto, Konatsu; Yamamoto, Takahisa; Furuta, Yoshio

2018-06-11

We first successfully synthesized Li 1+ x − y Nb 1− x −3 y Ti x +4 y O₃ (LNT) solid solutions (0.13 ≤ x ≤ 0.18, 0 ≤ y ≤ 0.06) rapidly at 1373 K for one hour under 0.35 MPa by the controlling of air pressure using an air-pressure control atmosphere furnace. The composition is a formation area of a superstructure for LNT, in which the periodical intergrowth layer was formed in the matrix, and where it can be controlled by Ti content. Therefore, the sintering time depended on Ti content, and annealing was repeated for over 24 h until a homogeneous structure was formed using a conventional electric furnace. We clarified the mechanism of the rapid sintering using various microscale to nanoscale characterization techniques: X-ray diffraction, a scanning electron microscope, a transmission electron microscope (TEM), a Cs-corrected scanning TEM equipped with electron energy-loss spectroscopy, and X-ray absorption fine structure spectroscopy.

Processing strategies for smart electroconductive carbon nanotube-based bioceramic bone grafts

NASA Astrophysics Data System (ADS)

Mata, D.; Oliveira, F. J.; Ferreira, N. M.; Araújo, R. F.; Fernandes, A. J. S.; Lopes, M. A.; Gomes, P. S.; Fernandes, M. H.; Silva, R. F.

2014-04-01

Electroconductive bone grafts have been designed to control bone regeneration. Contrary to polymeric matrices, the translation of the carbon nanotube (CNT) electroconductivity into oxide ceramics is challenging due to the CNT oxidation during sintering. Sintering strategies involving reactive-bed pressureless sintering (RB + P) and hot-pressing (HP) were optimized towards prevention of CNT oxidation in glass/hydroxyapatite (HA) matrices. Both showed CNT retentions up to 80%, even at 1300 °C, yielding an increase of the electroconductivity in ten orders of magnitude relative to the matrix. The RB + P CNT compacts showed higher electroconductivity by ˜170% than the HP ones due to the lower damage to CNTs of the former route. Even so, highly reproducible conductivities with statistical variation below 5% and dense compacts up to 96% were only obtained by HP. The hot-pressed CNT compacts possessed no acute toxicity in a human osteoblastic cell line. A normal cellular adhesion and a marked orientation of the cell growth were observed over the CNT composites, with a proliferation/differentiation relationship favouring osteoblastic functional activity. These sintering strategies offer new insights into the sintering of electroconductive CNT containing bioactive ceramics with unlimited geometries for electrotherapy of the bone tissue.

Application of the Zero-Order Reaction Rate Model and Transition State Theory to predict porous Ti6Al4V bending strength.

PubMed

Reig, L; Amigó, V; Busquets, D; Calero, J A; Ortiz, J L

2012-08-01

Porous Ti6Al4V samples were produced by microsphere sintering. The Zero-Order Reaction Rate Model and Transition State Theory were used to model the sintering process and to estimate the bending strength of the porous samples developed. The evolution of the surface area during the sintering process was used to obtain sintering parameters (sintering constant, activation energy, frequency factor, constant of activation and Gibbs energy of activation). These were then correlated with the bending strength in order to obtain a simple model with which to estimate the evolution of the bending strength of the samples when the sintering temperature and time are modified: σY=P+B·[lnT·t-ΔGa/R·T]. Although the sintering parameters were obtained only for the microsphere sizes analysed here, the strength of intermediate sizes could easily be estimated following this model. Copyright © 2012 Elsevier B.V. All rights reserved.

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

DOE PAGES

Xiong, Chunyan; Taillon, Joshua A.; Pellegrinelli, Christopher; ...

2016-07-19

Here, the impact of sintering temperature on Cr-poisoning of solid oxide fuel cell (SOFC) cathodes was systematically studied. La 0.6Sr 0.4Fe 0.8Co 0.2O 3-δ - Ce 0.9Gd 0.1O 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 increasesmore » 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.« less

Low-temperature sintering and electrical properties of strontium- and magnesium-doped lanthanum gallate with V2O5 additive

NASA Astrophysics Data System (ADS)

Ha, Sang Bu; Cho, Yoon Ho; Ji, Ho-Il; Lee, Jong-Ho; Kang, Yun Chan; Lee, Jong-Heun

2011-03-01

The effects of a V2O5 additive on the low-temperature sintering and ionic conductivity of strontium- and magnesium-doped lanthanum gallate (LSGM: La0.8Sr0.2Ga0.8Mg0.2O2.8) are studied. The LSGM powders prepared by the glycine nitrate method are mixed with 0.5-2 at.% of VO5/2 and then sintered at 1100-1400 °C in air for 4 h. The apparent density and phase purity of the LSGM specimens are increased with increasing sintering temperature and VO5/2 concentration due to the enhanced sintering and mass transfer via the intergranular liquid phase. The 1 at.% VO5/2-doped LSGM specimen sintered at 1300 °C exhibits a high oxide ion conductivity of ∼0.027 S cm-1 at 700 °C over a wide range of oxygen partial pressure (PO2 =10-27 - 1 atm), thereby demonstrating its potential as a useful electrolyte for anode-supported solid oxide fuel cells (SOFCs) without the requirement for any buffer layer between the electrolyte and anode.

Porous Ni-Fe alloys as anode support for intermediate temperature solid oxide fuel cells: I. Fabrication, redox and thermal behaviors

NASA Astrophysics Data System (ADS)

Wang, Xin; Li, Kai; Jia, Lichao; Zhang, Qian; Jiang, San Ping; Chi, Bo; Pu, Jian; Jian, Li; Yan, Dong

2015-03-01

Porous Ni-Fe anode supports for intermediate solid oxide fuel cells are prepared by reducing the sintered NiO-(0-50 wt. %) Fe2O3 composites in H2, their microstructure, redox and thermal expansion/cycling characteristics are systematically investigated. The sintered NiO-Fe2O3 composites are consisted of NiO and NiFe2O4, and are fully reducible to porous metallic Ni-Fe alloys in H2 at temperatures between 600 and 750 °C. The porous structure contains pores in bimodal distribution with larger pores between the sintered particles and smaller ones inside the particles. The oxidation resistance of the Ni-Fe alloy anode supports at 600 and 750 °C is increased by the addition of Fe, their oxidation kinetics obeys a multistage parabolic law in the form of (Percentageweightgain /Specificsurfacearea) 2 =kp · t , where kp is the rate constant and t the oxidation time. The dimension of the Ni-Fe anode supports is slightly changed without disintegrating their structure, and Fe addition is beneficial to the redox stability. The TEC of the Ni-Fe alloy anode supports decreases with the increase of Fe content. The anode supports containing Fe is less stable in dimension during thermal cycles due to the continuous sintering, but the dimension change after thermal cycles is within 1%.

Porous-electrode preparation method

DOEpatents

Arons, R.M.; Dusek, J.T.

1981-09-17

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity.

Porous electrode preparation method

DOEpatents

Arons, Richard M.; Dusek, Joseph T.

1983-01-01

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder of such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity.

Porous electrode preparation method

DOEpatents

Arons, R.M.; Dusek, J.T.

1983-10-18

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder of such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity. 2 figs.

Thermoelectric properties of a doped LaNiO3 perovskite system prepared using a spark-plasma sintering process

NASA Astrophysics Data System (ADS)

Tak, Jang-Yeul; Choi, Soon-Mok; Seo, Won-Seon; Cho, Hyung Koun

2013-07-01

Both perovskites LaNiO3 and LaCuO3 have a limitation associated with phase transitions for high-temperature thermoelectric applications. The optimized conditions were investigated to obtain the LaNi1- x Cu x O3- δ perovskite single phase showing a Cu-doping effect into Ni sites against unintended deoxidized phases. Three advantages of synergetic effects due to the simultaneous presence of nickel and copper were investigated: a low melting temperature of CuO as compared to that of NiO, the absence of intermediated deoxidized phases in the LaCuO3 system, and the Cu doping effect, which suppresses the formation of intermediate secondary phases. A solid solution was also fabricated using a spark-plasma sintering (SPS) process for the purpose of sintering LaNi1- x Cu x O3- δ compositions at a low sintering temperature.

Phase transformation in the alumina-titania system during flash sintering experiments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jha, S. K.; Lebrun, J. M.; Raj, R.

2016-02-01

We show that phase transformation in the alumina–titania system, which produces aluminum-titanate, follows an unusual trajectory during flash sintering. The experiments begin with mixed powders of alumina–titania and end in dense microstructures that are transformed into aluminum-titanate. The sintering and the phase transformation are separated in time, with the sintering occurs during Stage II, and phase transformation during Stage III of the flash sintering experiment. Stage III is the steady-state condition of flash activated state that is established under current control, while Stage II is the period of transition from voltage to current control. The extent of phase transformation increasesmore » with the current density and the hold time in Stage III.« less

Solid state neutron detector and method for use

DOEpatents

Doty, F. Patrick; Zwieback, Ilya; Ruderman, Warren

2002-01-01

Crystals of lithium tetraborate or alpha-barium borate had been found to be neutron detecting materials. The crystals are prepared using known crystal growing techniques, wherein the process does not include the common practice of using a fluxing agent, such as sodium oxide or sodium fluoride, to reduce the melting temperature of the crystalline compound. Crystals prepared by this method can be sliced into thin single or polycrystalline wafers, or ground to a powder and prepared as a sintered compact or a print paste, and then configured with appropriate electronic hardware, in order to function as neutron detectors.

Method of making a functionally graded material

DOEpatents

Lauf, Robert J.; Menchhofer, Paul A.; Walls, Claudia A.

2001-01-01

A gelcasting method of making an internally graded article includes the steps of: preparing at least two slurries, each of the slurries including a different gelcastable powder suspended in a gelcasting solution, the slurries characterized by having comparable shrinkage upon drying and sintering thereof; casting the slurries into a mold having a selected shape, wherein relative proportions of the slurries is varied in at least one direction within the selected shape; gelling the slurries to form a solid gel while preserving the variation in relative proportions of the slurries; drying the gel to form a dried green body; and sintering the dry green body to form a solid object, at least one property thereof varying because of the variation in relative proportions of the starting slurries. A gelcasting method of making an internally graded article alternatively includes the steps of: preparing a slurry including a least two different phases suspended in a gelcasting solution, the phases characterized by having different settling characteristics; casting the slurry into a mold having a selected shape; allowing the slurry to stand for a sufficient period of time to permit desired gravitational fractionation in order to achieve a vertical compositional gradient in the molded slurry; gelling the slurry to form a solid gel while preserving the vertical compositional gradient in the molded slurry; drying the gel to form a dried green body; and sintering the dry green body to form a solid object, at least one property thereof varying along the vertical direction because of the compositional gradient in the molded slurry.

Hole mobility enhancement of Cu-deficient Cu{sub 1.75}Zn(Sn{sub 1−x}Al{sub x})Se{sub 4} bulks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kuo, Dong-Hau, E-mail: dhkuo@mail.ntust.edu.tw; Tsega, Moges

2013-10-15

Cu-deficient Cu{sub 1.75}ZnSn{sub 1−x}Al{sub x}Se{sub 4} (x=0–0.6) bulks were prepared by a liquid-phase reactive sintering method at 600 {sup °}C with soluble sintering aids of Sb{sub 2}S{sub 3} and Te. Defect chemistry was studied by measuring electrical properties of Al-doped CZTSe as a function of dopant concentration. Al-CZTSe pellets at x=0.4 with electrical conductivity of 57.2 S cm{sup −1} showed the highest hole mobility of 32.5 cm{sup 2} V{sup −1} s{sup −1}. The high mobility is mainly contributed from the low atomic scattering factor of Al. The high carrier concentration and slightly changed lattice parameter of Al-CZTSe are related tomore » the types of its defects. - Graphical abstract: The controls in electrical properties and the changes in lattice parameters of Cu-deficient Cu{sub 2}ZnSnSe{sub 4} by doping Al{sup 3+} on the Sn{sup 4+} site. Display Omitted - Highlights: • Cu-deficient Cu{sub 1.75}Zn(Sn{sub 1−x}Al{sub x})Se{sub 4} was prepared by liquid-phase sintering at 600 °C. • Sintering aids of Sb{sub 2}S{sub 3} and Te were used for reactive sintering. • Al-CZTSe at x=0.4 showed the extremely high mobility of 32.5 cm{sup 2} V{sup −1} s{sup −1}. • Al-CZTSe reached large grains of 2−3 μm, while it was <1.0 μm for the undoped. • Electrical properties of Al-CZTSe pellets changed with the Al content.« less

Bioinspired ion-transport properties of solid-state single nanochannels and their applications in sensing.

PubMed

Tian, Ye; Wen, Liping; Hou, Xu; Hou, Guanglei; Jiang, Lei

2012-07-16

Biological ion channels are able to control ion-transport processes precisely because of their intriguing properties, such as selectivity, rectification, and gating. Learning from nature, scientists have developed a promising system--solid-state single nanochannels--to mimic biological ion-transport properties. These nanochannels have many impressive properties, such as excess surface charge, making them selective; the ability to be produced or modified asymmetrically, endowing them with rectification; and chemical reactivity of the inner surface, imparting them with desired gating properties. Based on these unique characteristics, solid-state single nanochannels have been explored in various applications, such as sensing. In this context, we summarize recent developments of bioinspired solid-state single nanochannels with ion-transport properties that resemble their biological counterparts, including selectivity, rectification, and gating; their applications in sensing are also introduced briefly. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The reactivity of Fe(II) associated with goethite formed during short redox cycles toward Cr(VI) reduction under oxic conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tomaszewski, Elizabeth J.; Lee, Seungyeol; Rudolph, Jared

Chromium (Cr) is a toxic metal that causes a myriad of health problems and enters the environment as a result of anthropogenic activities and/or natural processes. The toxicity and solubility of chromium is linked to its oxidation state; Cr(III) is poorly soluble and relatively nontoxic, while Cr(VI) is soluble and a known carcinogen. Solid Fe(II) in iron-bearing minerals, such as pyrite, magnetite, and green rusts, reduce the oxidation state of chromium, reducing its toxicity and mobility. However, these minerals are not the only potential sources of solid-associated Fe(II) available for Cr(VI) reduction. For example, ferric (Fe(III)) (hydr)oxides, such as goethitemore » or hematite, can have Fe(II) in the solid without phase transformation; however, the reactivity of Fe(II) within Fe(III) (hydr)oxides with contaminants, has not been previously investigated. Here, we cyclically react goethite with dissolved Fe(II) followed by dissolved O2, leading to the formation of reactive Fe(II) associated with goethite. In separate reactors, the reactivity of this Fe(II) is probed under oxic conditions, by exposure to chromate (CrO42 -) after either one, two, three or four redox cycles. Cr is not present during redox cycling; rather, it is introduced to a subset of the solid after each oxidation half-cycle. Analysis of X-ray absorption near edge structure (XANES) spectra reveals that the extent of Cr(VI) reduction to Cr(III) depends not only on solid Fe(II) content but also surface area and mean size of ordered crystalline domains, determined by BET surface area analysis and X-ray diffraction (XRD), respectively. Shell-by-shell fitting of the extended X-ray absorption fine structure (EXAFS) spectra demonstrates chromium forms both single and double corner sharing complexes on the surface of goethite, in addition to sorbed Cr(III) species. Finally, transmission electron microscope (TEM) imaging and X-ray energy-dispersive spectroscopy (EDS) illustrate that Cr preferentially localizes on the (100) face of goethite, independent of the number of redox cycles goethite undergoes. This work demonstrates that under oxic conditions, solid Fe(II) associated with goethite resulting from rapid redox cycling is reactive and available for electron transfer to Cr(VI), suggesting Fe(III) (hydr)oxides may act as reservoirs of reactive electron density, even in oxygen saturated environments.« less

Quantum State-Resolved Reactive and Inelastic Scattering at Gas-Liquid and Gas-Solid Interfaces

NASA Astrophysics Data System (ADS)

Grütter, Monika; Nelson, Daniel J.; Nesbitt, David J.

2012-06-01

Quantum state-resolved reactive and inelastic scattering at gas-liquid and gas-solid interfaces has become a research field of considerable interest in recent years. The collision and reaction dynamics of internally cold gas beams from liquid or solid surfaces is governed by two main processes, impulsive scattering (IS), where the incident particles scatter in a few-collisions environment from the surface, and trapping-desorption (TD), where full equilibration to the surface temperature (T{TD}≈ T{s}) occurs prior to the particles' return to the gas phase. Impulsive scattering events, on the other hand, result in significant rotational, and to a lesser extent vibrational, excitation of the scattered molecules, which can be well-described by a Boltzmann-distribution at a temperature (T{IS}>>T{s}). The quantum-state resolved detection used here allows the disentanglement of the rotational, vibrational, and translational degrees of freedom of the scattered molecules. The two examples discussed are (i) reactive scattering of monoatomic fluorine from room-temperature ionic liquids (RTILs) and (ii) inelastic scattering of benzene from a heated (˜500 K) gold surface. In the former experiment, rovibrational states of the nascent HF beam are detected using direct infrared absorption spectroscopy, and in the latter, a resonace-enhanced multi-photon-ionization (REMPI) scheme is employed in combination with a velocity-map imaging (VMI) device, which allows the detection of different vibrational states of benzene excited during the scattering process. M. E. Saecker, S. T. Govoni, D. V. Kowalski, M. E. King and G. M. Nathanson Science 252, 1421, 1991. A. M. Zolot, W. W. Harper, B. G. Perkins, P. J. Dagdigian and D. J. Nesbitt J. Chem. Phys 125, 021101, 2006. J. R. Roscioli and D. J. Nesbitt Faraday Disc. 150, 471, 2011.

Novel sintered ceramic materials incorporated with EAF carbon steel slag

NASA Astrophysics Data System (ADS)

Karayannis, V.; Ntampegliotis, K.; Lamprakopoulos, S.; Papapolymerou, G.; Spiliotis, X.

2017-01-01

In the present research, novel sintered clay-based ceramic materials containing electric arc furnace carbon steel slag (EAFC) as a useful admixture were developed and characterized. The environmentally safe management of steel industry waste by-products and their valorization as secondary resources into value-added materials towards circular economy have attracted much attention in the last years. EAF Carbon steel slag in particular, is generated during the manufacture of carbon steel. It is a solid residue mainly composed of rich-in- Fe, Ca and Si compounds. The experimental results show that the beneficial incorporation of lower percentages of EAFC up to 6%wt. into ceramics sintered at 950 °C is attained without significant variations in sintering behavior and physico-mechanical properties. Further heating up to 1100 °C strongly enhances the densification of the ceramic microstructures, thus reducing the porosity and strengthening their mechanical performance. On the other side, in terms of thermal insulation behavior as well as energy consumption savings and production cost alleviation, the optimum sintering temperature appears to be 950 °C.

Solid oxide fuel cell with multi-unit construction and prismatic design

DOEpatents

McPheeters, C.C.; Dees, D.W.; Myles, K.M.

1999-03-16

A single cell unit of a solid oxide fuel cell is described that is individually fabricated and sintered prior to being connected to adjacent cells to form a solid oxide fuel cell. The single cell unit is comprised of a shaped anode sheet positioned between a flat anode sheet and an anode-electrolyte-cathode (A/E/C) sheet, and a shaped cathode sheet positioned between the A/E/C sheet and a cathode-interconnect-anode (C/I/A) sheet. An alternate embodiment comprises a shaped cathode sheet positioned between an A/E/C sheet and a C/I/A sheet. The shaped sheets form channels for conducting reactant gases. Each single cell unit is individually sintered to form a finished sub-assembly. The finished sub-assemblies are connected in electrical series by interposing connective material between the end surfaces of adjacent cells, whereby individual cells may be inspected for defects and interchanged with non-defective single cell units. 7 figs.

Copper Chloride Cathode For Liquid-Sodium Cell

NASA Technical Reports Server (NTRS)

Bugga, Ratnakumar V.; Distefano, Salvador; Nagasubramanian, Ganesan; Bankston, Clyde P.

1990-01-01

Rechargeable liquid-sodium cell with copper chloride cathode offers substantial increase in energy density over cells made with other cathode materials. Unit has theoretical maximum energy density of 1135 W.h/kg. Generates electricity by electrochemical reaction of molten sodium and solid copper chloride immersed in molten electrolyte, sodium tetrachloroaluminate at temperature of equal to or greater than 200 degrees C. Wall of alumina tube separates molten electrolyte from molten sodium anode. Copper chloride cathode embedded in pores of sintered nickel cylinder or directly sintered.

Gordon Research Conferences, 1991

DTIC Science & Technology

1993-04-01

Chemistry Title of Conference Brewster Academy. Wolfeboro, NH Richard D. Adams, Chairman Suzanne Harris, Vice Chairman July 29. 1991 Date Monday. 8:45...am Materials and the Solid State Richard D. Adams Discussion Leader Robert Haushalter Hydrothermal Synthesis of Microporous 1. Speaker Molybdenum...Rouxel Design and Chemical Reactivity in 3. Speaker Low Dimensional Solids Title of Presentation Monday 7:30 om Catalysis Richard D. Adams Discussion

Segregation Phenomena in Size-Selected Bimetallic CuNi Nanoparticle Catalysts

DOE PAGES

Pielsticker, Lukas; Zegkinoglou, Ioannis; Divins, Nuria J.; ...

2017-10-25

Surface segregation, restructuring, and sintering phenomena in size-selected copper–nickel nanoparticles (NPs) supported on silicon dioxide substrates were systematically investigated as a function of temperature, chemical state, and reactive gas environment. Using near-ambient pressure (NAP-XPS) and ultrahigh vacuum X-ray photoelectron spectroscopy (XPS), we showed that nickel tends to segregate to the surface of the NPs at elevated temperatures in oxygen- or hydrogen-containing atmospheres. It was found that the NP pretreatment, gaseous environment, and oxide formation free energy are the main driving forces of the restructuring and segregation trends observed, overshadowing the role of the surface free energy. The depth profile ofmore » the elemental composition of the particles was determined under operando CO 2 hydrogenation conditions by varying the energy of the X-ray beam. The temperature dependence of the chemical state of the two metals was systematically studied, revealing the high stability of nickel oxides on the NPs and the important role of high valence oxidation states in the segregation behavior. Atomic force microscopy (AFM) studies revealed a remarkable stability of the NPs against sintering at temperatures as high as 700 °C. The results provide new insights into the complex interplay of the various factors which affect alloy formation and segregation phenomena in bimetallic NP systems, often in ways different from those previously known for their bulk counterparts. In conclusion, this leads to new routes for tuning the surface composition of nanocatalysts, for example, through plasma and annealing pretreatments.« less

Generation of White Light from Dysprosium-Doped Strontium Aluminate Phosphor by a Solid-State Reaction Method

NASA Astrophysics Data System (ADS)

Sahu, Ishwar Prasad; Bisen, D. P.; Brahme, N.; Tamrakar, Raunak Kumar

2016-04-01

A single-host lattice, white light-emitting SrAl2O4:Dy3+ phosphor was synthesized by a solid-state reaction method. The crystal structure of prepared SrAl2O4:Dy3+ phosphor was in a monoclinic phase with space group P21. The chemical composition of the sintered SrAl2O4:Dy3+ phosphor was confirmed by the energy dispersive x-ray spectroscopy technique. Under ultra-violet excitation, the characteristic emissions of Dy3+ are peaking at 475 nm, 573 nm and 660 nm, originating from the transitions of 4F9/2 → 6H15/2, 4F9/2 →&!nbsp; 6H13/2 and 4F9/2 → 6H11/2 in the 4f9 configuration of Dy3+ ions. Commission International de I'Eclairage color coordinates of SrAl2O4:Dy3+ are suitable for white light-emitting phosphor. In order to investigate the suitability of the samples as white color light sources for industrial uses, correlated color temperature (CCT) and color rendering index (CRI) values were calculated. Values of CCT and CRI were found well within the defined acceptable range. Mechanoluminescence (ML) intensity of SrAl2O4:Dy3+ phosphor increased linearly with increasing impact velocity of the moving piston. Thus, the present investigation indicates piezo-electricity was responsible for producing ML in sintered SrAl2O4:Dy3+ phosphor. Decay rates of the exponential decaying period of the ML curves do not change significantly with impact velocity. The photoluminescence and ML results suggest that the synthesized SrAl2O4:Dy3+ phosphor was useful for the white light-emitting diodes and stress sensor respectively.

Fast synthesis and consolidation of porous FeAl by pressureless Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Dudina, D. V.; Brester, A. E.; Anisimov, A. G.; Bokhonov, B. B.; Legan, M. A.; Novoselov, A. N.; Skovorodin, I. N.; Uvarov, N. F.

2017-07-01

We report one-step fast synthesis and consolidation of iron aluminide FeAl of high open porosity by pressureless reactive Spark Plasma Sintering (SPS). The starting material of the Fe-40at.%Al composition was a mixture of an iron powder with an average particle diameter of 4 μm and an aluminum powder with an average particle diameter of 6 μm. The rationale behind the choice of the SPS as a processing technique and fine and comparable sizes of the two reactants for the synthesis of high-open porosity FeAl was realization of fast full chemical conversion of Fe and Al into single-phase FeAl reducing the time available for the compact shrinkage. According to the XRD phase analysis, single-phase FeAl compacts formed after SPS at 800 and 900°C. These compacts had open porosities of 41 and 46%, respectively. The transverse rupture strength of the compacts sintered at 700-900°C was found to change little with the sintering temperature in the selected range.

Probing the molecular-level control of aluminosilicate dissolution: A sensitive solid-state NMR proxy for reactive surface area

NASA Astrophysics Data System (ADS)

Washton, Nancy M.; Brantley, Susan L.; Mueller, Karl T.

2008-12-01

For two suites of volcanic aluminosilicate glasses, the accessible and reactive sites for covalent attachment of the fluorine-containing (3,3,3-trifluoropropyl)dimethylchlorosilane (TFS) probe molecule were measured by quantitative 19F nuclear magnetic resonance (NMR) spectroscopy. The first set of samples consists of six rhyolitic and dacitic glasses originating from volcanic activity in Iceland and one rhyolitic glass from the Bishop Tuff, CA. Due to differences in the reactive species present on the surfaces of these glasses, variations in the rate of acid-mediated dissolution (pH 4) for samples in this suite cannot be explained by variations in geometric or BET-measured surface area. In contrast, the rates scale directly with the surface density of TFS-reactive sites as measured by solid-state NMR. These data are consistent with the inference that the TFS-reactive M-OH species on the glass surface, which are known to be non-hydrogen-bonded Q 3 groups, represent loci accessible to and affected by proton-mediated dissolution. The second suite of samples, originating from a chronosequence in Kozushima, Japan, is comprised of four rhyolites that have been weathered for 1.1, 1.8, 26, and 52 ka. The number of TFS-reactive sites per gram increases with duration of weathering in the laboratory for the "Icelandic" samples and with duration of field weathering for both "Icelandic" and Japanese samples. One hypothesis is consistent with these and published modeling, laboratory, and field observations: over short timescales, dissolution is controlled by fast-dissolving sites, but over long timescales, dissolution is controlled by slower-dissolving sites, the surface density of which is proportional to the number of TFS-reactive Q 3 sites. These latter sites are not part of a hydrogen-bonded network on the surface of the glasses, and measurement of their surface site density allows predictions of trends in reactive surface area. The TFS treatment method, which is easily monitored by quantitative 19F solid-state NMR, therefore provides a chemically specific and quantifiable proxy to understand the nature of how sites on dissolving silicates control dissolution. Furthermore, 27Al NMR techniques are shown here to be useful in identifying clays on the glass surfaces, and these methods are therefore effective for quantifying concentrations of weathering impurities. Our interpretations offer a testable hypothesis for the mechanism of proton-promoted dissolution for low-iron aluminosilicate minerals and glasses and suggest that future investigations of reactive surfaces with high-sensitivity NMR techniques are warranted.

Effect of Dopants and Sintering Method on the Properties of Ceria-Based Electrolytes for IT-SOFCs Applications

NASA Astrophysics Data System (ADS)

Sharma, Payal; Sharma, Chetan; Singh, Kanchan L.; Singh, Anirudh P.

2018-05-01

Doped and co-doped ceria ceramics are used as electrolyte materials in solid oxide fuel cells. In this work, ceria-based oxides, Ce0.90Gd0.06Y0.02M0.02O2-δ (M = Ca, Fe, La, and Sr) were prepared by conventional as well as microwave processing from the precursors prepared by the mixed oxide method. The consolidated calcined powders in pellet form were sintered in microwave energy at 1400°C for 20 min and in an electric furnace of IR radiation at 1400°C for 6 h. The x-ray diffraction analysis confirmed that all the compositions were crystallized into a cubic fluorite structure. Surface morphology of the sintered products was studied using scanning electron microscopy and the microhardness was investigated using the Vickers hardness test. The comparative results analysis shows that the microwave-sintered samples have uniform grain growth, higher density and higher microhardness than the corresponding conventionally sintered products. The microwave-sintered sample of composition Ce0.90Gd0.06Y0.02Sr0.02O2-δ was found to have the highest microhardness among the four compositions due to its high density and smallest grain size.

Microstructure evolution and electrical characterization of Lanthanum doped Barium Titanate (BaTiO{sub 3}) ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Billah, Masum, E-mail: masum.buet09@gmail.com; Ahmed, A., E-mail: jhinukbuetmme@gmail.com; Rahman, Md. Miftaur, E-mail: miftaurrahman@mme.buet.ac.bd

2016-07-12

In the current work, we investigated the structural and dielectric properties of Lanthanum oxide (La{sub 2}O{sub 3}) doped Barium Titanate (BaTiO{sub 3}) ceramics and established a correlation between them. Solid state sintering method was used to dope BaTiO{sub 3} with 0.3, 0.5 and 0.7 mole% La{sub 2}O{sub 3} under different sintering parameters. The raw materials used were La{sub 2}O{sub 3} nano powder of ~80 nm grain size and 99.995% purity and BaTiO{sub 3} nano powder of 100 nm grain size and 99.99% purity. Grain size distribution and morphology of fracture surface of sintered pellets were examined by Field Emission Scanningmore » Electron Microscope and X-Ray Diffraction analysis was conducted to confirm the formation of desired crystal structure. The research result reveal that grain size and electrical properties of BaTiO{sub 3} ceramic significantly enhanced for small amount of doping (up to 0.5 mole% La{sub 2}O{sub 3}) and then decreased with increasing doping concentration. Desired grain growth (0.80-1.3 µm) and high densification (<90% theoretical density) were found by proper combination of temperature, sintering parameters and doping concentration. We found the resultant stable value of dielectric constant was 10000-12000 at 100-300 Hz in the temperature range of 30°-50° C for 0.5 mole% La{sub 2}O{sub 3} with corresponding shift of curie temperature around 30° C. So overall this research showed that proper La{sup 3+} concentration can control the grain size, increase density, lower curie temperature and hence significantly improve the electrical properties of BaTiO{sub 3} ceramics.« less

Dielectric, Piezoelectric, and Vibration Properties of the LiF-Doped (Ba0.95Ca0.05)(Ti0.93Sn0.07)O₃ Lead-Free Piezoceramic Sheets.

PubMed

Cheng, Chien-Min; Chen, Kai-Huang; Lee, Da-Huei; Jong, Fuh-Cheng; Chen, Mei-Li; Chang, Jhih-Kai

2018-01-24

By the conventional solid state reaction method, a small amount of lithium fluoride (LiF) was used as the sintering promoter to improve the sintering and piezoelectric characteristics of (Ba 0.95 Ca 0.05 )(Ti 0.93 Sn 0.07 )O₃ (BCTS) lead-free piezoceramic sheets. Using X-ray diffraction (XRD) and a scanning electron microscope (SEM), the inferences of the crystalline and surface microstructures were obtained and analyzed. Then, the impedance analyzer and d 33 -meter were used to measure the dielectric and piezoelectric characteristics. In this study, the optimum sintering temperature of the BCTS sheets decreased from 1450 °C to 1390 °C due to LiF doping. For the 0.07 wt % LiF-doped BCTS sheets sintered at 1390 °C, the piezoelectric constant (d 33 ) is 413 pC/N, the electric-mechanical coupling coefficient (k p ) is 47.5%, the dielectric loss (tan δ) is 3.9%, and the dielectric constant (ε r ) is 8100, which are all close to or even better than that of the pure undoped BCTS ceramics. The Curie temperature also improved, from 85 °C for pure BCTS to 140 °C for BCTS-0.07 LiF sheets. Furthermore, by using the vibration system and fixing 1.5 g tip mass at the end of the sheets, as the vibration frequency is 20 Hz, the proposed piezoelectric ceramic sheets also reveal a good energy harvesting performance at the maximum output peak voltage of 4.6 V, which is large enough and can be applied in modern low-power electronic products.

Effect of heating parameters on sintering behaviors and properties of mullite whisker frameworks

NASA Astrophysics Data System (ADS)

Zhang, Y. M.; Zeng, D. J.; Wang, B.; Yang, J. F.

2018-04-01

Mullite whisker frameworks were fabricated by vapor-solid reaction with SiO2, Al2O3 and AlF3 powders as the whisker forming agent at high temperatures. The effects of heating temperature and soaking time on the weight loss, liner shrinkage, porosity, microstructure and compressive strength were investigated. The results showed that with the increasing of the sintering temperature and soaking time, the weight loss and liner shrinkage of the samples increased and the porosities decreased due to the accelerated vapor-solid reaction, resulting in strong bonding and grain growth of the mullite frameworks. The compressive strength of the samples increased with increasing the sintering temperature from 1500 to 1650 °C, and decreased with the soaking time extended to more than 5 h for 1500 °C and 2 h for 1650 °C. A maximum compressive strength of 142 MPa at a porosity of 62.3% was obtained for the mullite whisker framework heated at 1500 °C for 5 h. The enhanced strength was attributed to the strong bonding strength and fine mullite grains resulting from a relative lower heating temperature and a modest soaking time.

Influence of Resin Composition on the Defect Formation in Alumina Manufactured by Stereolithography

PubMed Central

Johansson, Emil; Lidström, Oscar; Johansson, Jan; Lyckfeldt, Ola; Adolfsson, Erik

2017-01-01

Stereolithography (SL) is a technique allowing additive manufacturing of complex ceramic parts by selective photopolymerization of a photocurable suspension containing photocurable monomer, photoinitiator, and a ceramic powder. The manufactured three-dimensional object is cleaned and converted into a dense ceramic part by thermal debinding of the polymer network and subsequent sintering. The debinding is the most critical and time-consuming step, and often the source of cracks. In this study, photocurable alumina suspensions have been developed, and the influence of resin composition on defect formation has been investigated. The suspensions were characterized in terms of rheology and curing behaviour, and cross-sections of sintered specimens manufactured by SL were evaluated by SEM. It was found that the addition of a non-reactive component to the photocurable resin reduced polymerization shrinkage and altered the thermal decomposition of the polymer matrix, which led to a reduction in both delamination and intra-laminar cracks. Using a non-reactive component that decomposed rather than evaporated led to less residual porosity. PMID:28772496

Morphology and phase identification of micron to nanosized manganese oxide (MnO) with variations in sintering time

NASA Astrophysics Data System (ADS)

Sasongko, Muhammad Ilman Nur; Puspitasari, Poppy; Yazirin, Cepi; Tsamroh, Dewi Izzatus; Risdanareni, Puput

2017-09-01

Manganese oxide (MnO) occurs in many rock types and may take the form of minerals. MnO has its drawbacks, namely highly reactive oxidizing species classified as dangerous and explosive at temperatures above 55 °C. Despite this,MnO has excellent magnetic, electrochemical, and conductivity properties, which should be reduced to nano-size to maximize their use and improve the properties of MnO. Phase and morphology characterization of powder this research aims to reduce the grain size of the MnO from micro to nano using the sol-gel method with various sintering times. Sol-gel is a simple synthesis method that has been proven capable of synthesizing a wide variety of micro-sized oxide materials into nano. Sintering time is a technique performed in the synthesis process to dry the material to a temperature above the normal temperature. The temperature used for sintering starting from 600 °C to 1000 °C. Characterizations were done using XRD, SEM, EDX, and FTIR machines. The sintering processes in this study used a temperature of 600 °C with different sintering periods of 30, 60 and 90 minutes. The XRD characterization with a 30-minute sintering time resulted in the smallest MnO in the form crystalline powder of 47.3 nm. The highest intensity (degree of crystallinity) found in MnO sintered for 90 minutes. The results of the morphological characterization of SEM showed a morphological change in MnO from micro-sized triangular to nano-sized spherical shape. The EDX characterization results indicated that the 30-minute sintering caused the lowest change in Mn and the highest change in O. The results of FTIR characterization showed a shift in C-H and Mn-O followed by an increase in the group of N-H, C=O and Mn-O.

Organic Binder Developments for Solid Freeform Fabrication

NASA Technical Reports Server (NTRS)

Cooper, Ken; Mobasher, Amir A.

2003-01-01

A number of rapid prototyping techniques are under development at Marshall Space Flight Center's (MSFC) National Center for Advanced Manufacturing Rapid Prototyping Laboratory. Commercial binder developments in creating solid models for rapid prototyping include: 1) Fused Deposition Modeling; 2) Three Dimensional Printing; 3) Selective Laser Sintering (SLS). This document describes these techniques developed by the private sector, as well as SLS undertaken by MSFC.

The influence of petrography, mineralogy and chemistry on burnability and reactivity of quicklime produced in Twin Shaft Regenerative (TSR) kilns from Neoarchean limestone (Transvaal Supergroup, South Africa)

NASA Astrophysics Data System (ADS)

Vola, Gabriele; Sarandrea, Luca; Della Porta, Giovanna; Cavallo, Alessandro; Jadoul, Flavio; Cruciani, Giuseppe

2017-12-01

This study evaluates the influence of chemical, mineralogical and petrographic features of the Neoarchean limestone from the Ouplaas Mine (Griqualand West, South Africa) on its burnability and quicklime reactivity, considering the main use as raw material for high-grade lime production in twin shaft regenerative (TSR) kilns. This limestone consists of laminated clotted peloidal micrite and fenestrate microbial boundstone with herringbone calcite and organic carbon (kerogen) within stylolites. Diagenetic modifications include hypidiotopic dolomite, micrite to microsparite recrystallization, stylolites, poikilotopic calcite, chert and saddle dolomite replacements. Burning and technical tests widely attest that the Neoarchean limestone is sensitive to high temperature, showing an unusual and drastically pronounced sintering or overburning tendency. The slaking reactivity, according to EN 459-2 is high for lime burnt at 1050 °C, but rapidly decreases for lime burnt at 1150 °C. The predominant micritic microbial textures, coupled with the organic carbon, are key-factors influencing the low burnability and the high sintering tendency. The presence of burial cementation, especially poikilotopic calcite, seems to promote higher burnability, either in terms of starting calcination temperature, or in terms of higher carbonate dissociation rate. In fact, the highest calcination velocity determined by thermal analysis is consistent with the highest slaking reactivity of the lower stratum of the quarry, enriched in poikilotopic calcite. Secondly, locally concentered dolomitic marly limestones, and sporadic back shales negatively affects the quicklime reactivity, as well. This study confirms that a multidisciplinary analytical approach is essential for selecting the best raw mix for achieving the highest lime reactivity in TSR kilns.

Thermoelectric SnS and SnS-SnSe solid solutions prepared by mechanical alloying and spark plasma sintering: Anisotropic thermoelectric properties

PubMed Central

Asfandiyar; Wei, Tian-Ran; Li, Zhiliang; Sun, Fu-Hua; Pan, Yu; Wu, Chao-Feng; Farooq, Muhammad Umer; Tang, Huaichao; Li, Fu; Li, Bo; Li, Jing-Feng

2017-01-01

P–type SnS compound and SnS1−xSex solid solutions were prepared by mechanical alloying followed by spark plasma sintering (SPS) and their thermoelectric properties were then studied in different compositions (x = 0.0, 0.2, 0.5, 0.8) along the directions parallel (//) and perpendicular (⊥) to the SPS–pressurizing direction in the temperature range 323–823 Κ. SnS compound and SnS1−xSex solid solutions exhibited anisotropic thermoelectric performance and showed higher power factor and thermal conductivity along the direction ⊥ than the // one. The thermal conductivity decreased with increasing contents of Se and fell to 0.36 W m−1 K−1 at 823 K for the composition SnS0.5Se0.5. With increasing selenium content (x) the formation of solid solutions substantially improved the electrical conductivity due to the increased carrier concentration. Hence, the optimized power factor and reduced thermal conductivity resulted in a maximum ZT value of 0.64 at 823 K for SnS0.2Se0.8 along the parallel direction. PMID:28240324

Thermoelectric SnS and SnS-SnSe solid solutions prepared by mechanical alloying and spark plasma sintering: Anisotropic thermoelectric properties.

PubMed

Asfandiyar; Wei, Tian-Ran; Li, Zhiliang; Sun, Fu-Hua; Pan, Yu; Wu, Chao-Feng; Farooq, Muhammad Umer; Tang, Huaichao; Li, Fu; Li, Bo; Li, Jing-Feng

2017-02-27

P-type SnS compound and SnS 1-x Se x solid solutions were prepared by mechanical alloying followed by spark plasma sintering (SPS) and their thermoelectric properties were then studied in different compositions (x = 0.0, 0.2, 0.5, 0.8) along the directions parallel (//) and perpendicular (⊥) to the SPS-pressurizing direction in the temperature range 323-823 Κ. SnS compound and SnS 1-x Se x solid solutions exhibited anisotropic thermoelectric performance and showed higher power factor and thermal conductivity along the direction ⊥ than the // one. The thermal conductivity decreased with increasing contents of Se and fell to 0.36 W m -1  K -1 at 823 K for the composition SnS 0.5 Se 0.5 . With increasing selenium content (x) the formation of solid solutions substantially improved the electrical conductivity due to the increased carrier concentration. Hence, the optimized power factor and reduced thermal conductivity resulted in a maximum ZT value of 0.64 at 823 K for SnS 0.2 Se 0.8 along the parallel direction.

Compositional inhomogeneityand segregation in (K 0.5Na 0.5)NbO 3 ceramics

DOE PAGES

Chen, Kepi; Tang, Jing; Chen, Yan

2016-03-11

The effects of the calcination temperature of (K 0.5Na 0.5)NbO 3 (KNN) powder on the sintering and piezoelectric properties of KNN ceramics have been investigated in this report. KNN powders are synthesized via the solid-state approach. Scanning electron microscopy and X-ray diffraction characterizations indicate that the incomplete reaction at 700 °C and 750 °C calcination results in the compositional inhomogeneity of the K-rich and Na-rich phases while the orthorhombic single phase is obtained after calcination at 900 °C. During the sintering, the presence of the liquid K-rich phase due to the lower melting point has a significant impact on themore » densification, the abnormal grain growth and the deteriorated piezoelectric properties. From the standpoint of piezoelectric properties, the optimal calcination temperature obtained for KNN ceramics calcined at this temperature is determined to be 800 °C, with piezoelectric constant d 33=128.3 pC/N, planar electromechanical coupling coefficient k p=32.2%, mechanical quality factor Q m=88, and dielectric loss tan δ=2.1%.« less

Formation of nickel and copper ferrites in ceramics: a potential reaction in the reuse of iron-rich sludge incineration ash.

PubMed

Shih, Kaimin

2012-12-01

This study investigates potential solid-state reactions for the stabilization of hazardous metals when reusing the incineration ash from chemically enhanced primary treatment (CEPT) sludge to fabricate ceramic products. Nickel and copper were used as examples of hazardous metals, and the iron content in the reaction system was found to play a major role in incorporating these hazardous metals into their ferrite phases (NiFe2O4 and CuFe2O4). The results from three-hour sintering experiments on NiO + Fe2O3 and CuO + Fe2O3 systems clearly demonstrate the potential for initiating metal incorporation mechanisms using an iron-containing precursor at attainable ceramic sintering temperatures (above 750 degrees C). Both ferrite phases were examined using a prolonged leaching experiment modified from the widely used toxicity characteristic leaching procedure (TCLP) to evaluate their long-term metal leachability. The leaching results indicate that both the NiFe2O4 and the CuFe2O4 products were significantly superior to their oxide forms in immobilizing hazardous metals.

Effect of orthorhombic distortion on dielectric and piezoelectric properties of CaBi4Ti4O15 ceramics

NASA Astrophysics Data System (ADS)

Tanwar, Amit; Sreenivas, K.; Gupta, Vinay

2009-04-01

High temperature bismuth layered piezoelectric and ferroelectric ceramics of CaBi4Ti4O15 (CBT) have been prepared using the solid state route. The formation of single phase material with orthorhombic structure was verified from x-ray diffraction and Raman spectroscopy. The orthorhombic distortion present in the CBT ceramic sintered at 1200 °C was found to be maximum. A sharp phase transition from ferroelectric to paraelectric was observed in the temperature dependent dielectric studies of all CBT ceramics. The Curie's temperature (Tc=790 °C) was found to be independent of measured frequency. The behavior of ac conductivity as a function of frequency (100 Hz-1 MHz) at low temperatures (<500 °C) follows the power law and is attributed to hopping conduction. The presence of large orthorhombic distortion in the CBT ceramic sintered at 1200 °C results in high dielectric constant, low dielectric loss, and high piezoelectric coefficient (d33). The observed results indicate the important role of orthorhombic distortion in determining the improved property of multicomponent ferroelectric material.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Kepi; Tang, Jing; Chen, Yan

The effects of the calcination temperature of (K 0.5Na 0.5)NbO 3 (KNN) powder on the sintering and piezoelectric properties of KNN ceramics have been investigated in this report. KNN powders are synthesized via the solid-state approach. Scanning electron microscopy and X-ray diffraction characterizations indicate that the incomplete reaction at 700 °C and 750 °C calcination results in the compositional inhomogeneity of the K-rich and Na-rich phases while the orthorhombic single phase is obtained after calcination at 900 °C. During the sintering, the presence of the liquid K-rich phase due to the lower melting point has a significant impact on themore » densification, the abnormal grain growth and the deteriorated piezoelectric properties. From the standpoint of piezoelectric properties, the optimal calcination temperature obtained for KNN ceramics calcined at this temperature is determined to be 800 °C, with piezoelectric constant d 33=128.3 pC/N, planar electromechanical coupling coefficient k p=32.2%, mechanical quality factor Q m=88, and dielectric loss tan δ=2.1%.« less

Solid-state synthesis of nano-sized Ba(Ti1- x Sn x )O3 powders and dielectric properties of corresponding ceramics

NASA Astrophysics Data System (ADS)

Ansaree, Md. Jawed; Kumar, Upendra; Upadhyay, Shail

2017-06-01

Powders of a few compositions of solid solution BaTi1- x Sn x O3 ( x = 0.0, 0.1, 0.2, 0.3 and 0.40) have been synthesized at 800 °C for 8 h using Ba(NO3)2, TiO2 and SnCl4·5H2O as starting materials. The thermogravimetric (TG) and differential scanning calorimetric (DSC) analysis of mixture in the stoichiometric proportion for sample BaTi0.80Sn0.20O3 have been carried out to understand the formation of solid solutions. Single-phase pure compounds (except x = 0.40) of the samples have been obtained at a lower calcination temperature (800 °C) than that of those reported in the literature for traditional solid-state synthesis making use of oxides and or carbonates as starting material (≥1200 °C). Tetragonal symmetry for compositions x = 0.0 and 0.10, cubic for x = 0.2 and 0.30 were found by X-ray diffraction (XRD) analysis. The transmission electron microscopic (TEM) analysis confirmed that calcined powders have a particle size between 30 and 50 nm. Ceramics of these powders were prepared by sintering at 1350 °C for 4 h. Properties of ceramics obtained in this work have been compared with properties reported in the literature.

Microstructure and Mechanical Properties of Ti-6Al-4V Fabricated by Selective Laser Melting of Powder Produced by Granulation-Sintering-Deoxygenation Method

NASA Astrophysics Data System (ADS)

Sun, Pei; Fang, Z. Zak; Zhang, Ying; Xia, Yang

2017-12-01

Commercial spherical Ti powders for additive manufacturing applications are produced today by melt-atomization methods at relatively high costs. A meltless production method, called granulation-sintering-deoxygenation (GSD), was developed recently to produce spherical Ti alloy powder at a significantly reduced cost. In this new process, fine hydrogenated Ti particles are agglomerated to form spherical granules, which are then sintered to dense spherical particles. After sintering, the solid fully dense spherical Ti alloy particles are deoxygenated using novel low-temperature deoxygenation processes with either Mg or Ca. This technical communication presents results of 3D printing using GSD powder and the selective laser melting (SLM) technique. The results showed that tensile properties of parts fabricated from spherical GSD Ti-6Al-4V powder by SLM are comparable with typical mill-annealed Ti-6Al-4V. The characteristics of 3D printed Ti-6Al-4V from GSD powder are also compared with that of commercial materials.

Fabrication of Li2TiO3 pebbles using PVA-boric acid reaction for solid breeding materials

NASA Astrophysics Data System (ADS)

Park, Yi-Hyun; Cho, Seungyon; Ahn, Mu-Young

2014-12-01

Lithium metatitanate (Li2TiO3) is a candidate breeding material of the Helium Cooled Ceramic Reflector (HCCR) Test Blanket Module (TBM). The breeding material is used in pebble-bed form to reduce the uncertainty of the interface thermal conductance. In this study, Li2TiO3 pebbles were successfully fabricated by the slurry droplet wetting method using the cross-linking reaction between polyvinyl alcohol (PVA) and boric acid. The effects of fabrication parameters on the shaping of Li2TiO3 green body were investigated. In addition, the basic characteristics of the sintered pebble were also evaluated. The shape of Li2TiO3 green bodies was affected by slurry viscosity, PVA content and boric acid content. The grain size and average crush load of sintered Li2TiO3 pebble were controlled by the sintering time. The boron was completely removed during the final sintering process.

Geochemical characterization of slags, other mines wastes, and their leachates from the Elizabeth and Ely mines (Vermont), the Ducktown mining district (Tennessee), and the Clayton smelter site (Idaho)

USGS Publications Warehouse

Piatak, Nadine M.; Seal, Robert R.; Hammarstrom, Jane M.; Meier, Allen L.; Briggs, Paul H.

2003-01-01

Waste-rock material produced at historic metal mines contains elevated concentrations of potentially toxic trace elements. Two types of mine waste were examined in this study: sintered waste rock and slag. The samples were collected from the Elizabeth and Ely mines in the Vermont copper belt (Besshi-type massive sulfide deposits), from the Copper Basin mining district near Ducktown, Tennessee (Besshi-type massive sulfide deposits), and from the Clayton silver mine in the Bayhorse mining district, Idaho (polymetallic vein and replacement deposits). The data in this report are presented as a compilation with minimal interpretation or discussion. A detailed discussion and interpretation of the slag data are presented in a companion paper. Data collected from sintered waste rock and slag include: (1) bulk rock chemistry, (2) mineralogy, (3) and the distribution of trace elements among phases for the slag samples. In addition, the reactivity of the waste material under surficial conditions was assessed by examining secondary minerals formed on slag and by laboratory leaching tests using deionized water and a synthetic solution approximating precipitation in the eastern United States.

Monolithic translucent BaMgAl 10O 17:Eu 2+ phosphors for laser-driven solid state lighting

DOE PAGES

Cozzan, Clayton; Brady, Michael J.; O’Dea, Nicholas; ...

2016-10-11

With high power light emitting diodes and laser diodes being explored for white light generation and visible light communication, thermally robust encapsulation schemes for color-converting inorganic phosphors are essential. In the current work, the canonical blue-emitting phosphor, high purity Eu-doped BaMgAl 10O 17, has been prepared using microwave-assisted heating (25 min) and densified into translucent ceramic phosphor monoliths using spark plasma sintering (30 min). Lastly, the resulting translucent ceramic monoliths convert UV laser light to blue light with the same efficiency as the starting powder and provide superior thermal management in comparison with silicone encapsulation.

Method for preparing boron-carbide articles

DOEpatents

Benton, S.T.; Masters, D.R.

1975-10-21

The invention is directed to the preparation of boron carbide articles of various configurations. A stoichiometric mixture of particulate boron and carbon is confined in a suitable mold, heated to a temperature in the range of about 1250 to 1500$sup 0$C for effecting a solid state diffusion reaction between the boron and carbon for forming the boron carbide (B$sub 4$C), and thereafter the resulting boron-carbide particles are hot-pressed at a temperature in the range of about 1800 to 2200$sup 0$C and a pressure in the range of about 1000 to 4000 psi for densifying and sintering the boron carbide into the desired article.

Theoretical and computer models of detonation in solid explosives

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tarver, C.M.; Urtiew, P.A.

1997-10-01

Recent experimental and theoretical advances in understanding energy transfer and chemical kinetics have led to improved models of detonation waves in solid explosives. The Nonequilibrium Zeldovich - von Neumann - Doring (NEZND) model is supported by picosecond laser experiments and molecular dynamics simulations of the multiphonon up-pumping and internal vibrational energy redistribution (IVR) processes by which the unreacted explosive molecules are excited to the transition state(s) preceding reaction behind the leading shock front(s). High temperature, high density transition state theory calculates the induction times measured by laser interferometric techniques. Exothermic chain reactions form product gases in highly excited vibrational states,more » which have been demonstrated to rapidly equilibrate via supercollisions. Embedded gauge and Fabry-Perot techniques measure the rates of reaction product expansion as thermal and chemical equilibrium is approached. Detonation reaction zone lengths in carbon-rich condensed phase explosives depend on the relatively slow formation of solid graphite or diamond. The Ignition and Growth reactive flow model based on pressure dependent reaction rates and Jones-Wilkins-Lee (JWL) equations of state has reproduced this nanosecond time resolved experimental data and thus has yielded accurate average reaction zone descriptions in one-, two- and three- dimensional hydrodynamic code calculations. The next generation reactive flow model requires improved equations of state and temperature dependent chemical kinetics. Such a model is being developed for the ALE3D hydrodynamic code, in which heat transfer and Arrhenius kinetics are intimately linked to the hydrodynamics.« less

Synthesis of dense yttrium-stabilised hafnia pellets for nuclear applications by spark plasma sintering

NASA Astrophysics Data System (ADS)

Tyrpekl, Vaclav; Holzhäuser, Michael; Hein, Herwin; Vigier, Jean-Francois; Somers, Joseph; Svora, Petr

2014-11-01

Dense yttrium-stabilised hafnia pellets (91.35 wt.% HfO2 and 8.65 wt.% Y2O3) were prepared by spark plasma sintering consolidation of micro-beads synthesised by the "external gelation" sol-gel technique. This technique allows a preparation of HfO2-Y2O3 beads with homogenous yttria-hafnia solid solution. A sintering time of 5 min at 1600 °C was sufficient to produce high density pellets (over 90% of the theoretical density) with significant reproducibility. The pellets have been machined in a lathe to the correct dimensions for use as neutron absorbers in an experimental test irradiation in the High Flux Reactor (HFR) in Petten, Holland, in order to investigate the safety of americium based nuclear fuels.

Grain boundary premelting and activated sintering in binary refractory alloys

NASA Astrophysics Data System (ADS)

Shi, Xiaomeng

Quasi-liquid intergranular film (IGF) which has been widely observed in ceramic systems can persist into sub-solidus region whereby an analogy to Grain boundary (GB) premelting can be made. In this work, a grain boundary (GB) premelting/prewetting model in a metallic system was firstly built based on the Benedictus' model and computational thermodynamics, predicting that GB disordering can start at 60-85% of the bulk solidus temperatures in selected systems. This model quantitatively explains the long-standing mystery of subsolidus activated sintering in W-Pd, W-Ni, W-Co, W-Fe and W-Cu, and it has broad applications for understanding GB-controlled transport kinetics and physical properties. Furthermore, this study demonstrates the necessity of developing GB phase diagrams as a tool for materials design. Subsequently, Grain boundary (GB) wetting and prewetting in Ni-doped Mo are systematically evaluated via characterizing well-quenched specimens and thermodynamic modeling. In contrast to prior reports, the delta-NiMo phase does not wet Mo GBs in the solid state. In the solid-liquid two-phase region, the Ni-rich liquid wets Mo GBs completely. Furthermore, high-resolution transmission electron microscopy demonstrates that nanometer-thick quasi-liquid IGFs persist at GBs into the single-phase region where the bulk liquid phase is no longer stable; this is interpreted as a case of GB prewetting. An analytical thermodynamic model is developed and validated, and this model can be extended to other systems. Furthermore, the analytical model was refined based upon Beneditus' model with correction in determining interaction contribution of interfacial energy. A calculation-based GB phase diagram for Ni-Mo binary system was created and validated by comparing with GB diffusivities determined through a series of controlled sintering experiments. The dependence of GB diffusivity on doping level and temperature was examined and compared with model-predicted GB phase diagram. The consistency between GB phase diagram and GB diffusivity was evidently observed. This study revealed the existence of quasi-liquid IGF in Ni-Mo and re-confirmed our prior hypothesis proposed through work in Ni-W system. It also demonstrated further the necessity of a GB phase diagram as a new tool to guide the materials processing or design, such as selection of sintering aid and heat-treatment.

Surprising synthesis of nanodiamond from single-walled carbon nanotubes by the spark plasma sintering process

NASA Astrophysics Data System (ADS)

Mirzaei, Ali; Ham, Heon; Na, Han Gil; Kwon, Yong Jung; Kang, Sung Yong; Choi, Myung Sik; Bang, Jae Hoon; Park, No-Hyung; Kang, Inpil; Kim, Hyoun Woo

2016-10-01

Nanodiamond (ND) was successfully synthesized using single-walled carbon nanotubes (SWCNTs) as a pure solid carbon source by means of a spark plasma sintering process. Raman spectra and X-ray diffraction patterns revealed the generation of the cubic diamond phase by means of the SPS process. Lattice-resolved TEM images confirmed that diamond nanoparticles with a diameter of about ˜10 nm existed in the products. The NDs were generated mainly through the gas-phase nucleation of carbon atoms evaporated from the SWCNTs. [Figure not available: see fulltext.

Fabrication of lanthanum-doped thorium dioxide by high-energy ball milling and spark plasma sintering

NASA Astrophysics Data System (ADS)

Scott, Spencer M.; Yao, Tiankai; Lu, Fengyuan; Xin, Guoqing; Zhu, Weiguang; Lian, Jie

2017-03-01

High-energy ball milling was used to synthesize Th1-xLaxO2-0.5x (x = 0.09, 0.23) solid solutions, as well as improve the sinterability of ThO2 powders. Dense La-doped ThO2 pellets with theoretical density above 94% were consolidated by spark plasma sintering at temperatures above 1400 °C for 20 min, and the densification behavior and the non-equilibrium effects on phase and structure were investigated. A lattice contraction of the SPS-densified pellets occurred with increasing ball milling duration, and a secondary phase with increased La-content was observed in La-doped pellets. A dependence on the La-content and sintering duration for the onset of localized phase segregation has been proposed. The effects of high-energy ball milling, La-content, and phase formation on the thermal diffusivity were also studied for La-doped ThO2 pellets by laser flash measurement. Increasing La-content and high energy ball milling time decreases thermal diffusivity; while the sintering peak temperature and holding time beyond 1600 °C dramatically altered the temperature dependence of the thermal diffusivity beyond 600 °C.

Ceramic materials with low thermal conductivity and low coefficients of thermal expansion

DOEpatents

Brown, Jesse; Hirschfeld, Deidre; Liu, Dean-Mo; Yang, Yaping; Li, Tingkai; Swanson, Robert E.; Van Aken, Steven; Kim, Jin-Min

1992-01-01

Compositions having the general formula (Ca.sub.x Mg.sub.1-x)Zr.sub.4 (PO.sub.4).sub.6 where x is between 0.5 and 0.99 are produced by solid state and sol-gel processes. In a preferred embodiment, when x is between 0.5 and 0.8, the MgCZP materials have near-zero coefficients of thermal expansion. The MgCZPs of the present invention also show unusually low thermal conductivities, and are stable at high temperatures. Macrostructures formed from MgCZP are useful in a wide variety of high-temperature applications. In a preferred process, calcium, magnesium, and zirconium nitrate solutions have their pH adjusted to between 7 and 9 either before or after the addition of ammonium dihydrogen phosphate. After dehydration to a gel, and calcination at temperatures in excess of 850.degree. C. for approximately 16 hours, single phase crystalline MgCZP powders with particle sizes ranging from approximately 20 nm to 50 nm result. The MgCZP powders are then sintered at temperatures ranging from 1200.degree. C. to 1350.degree. C. to form solid macrostructures with near-zero bulk coefficients of thermal expansion and low thermal conductivities. Porous macrostructures of the MgCZP powders of the present invention are also formed by combination with a polymeric powder and a binding agent, and sintering at high temperatures. The porosity of the resulting macrostructures can be adjusted by varying the particle size of the polymeric powder used.

Ceramic materials with low thermal conductivity and low coefficients of thermal expansion

DOEpatents

Brown, J.; Hirschfeld, D.; Liu, D.M.; Yang, Y.; Li, T.; Swanson, R.E.; Van Aken, S.; Kim, J.M.

1992-04-07

Compositions, having the general formula (Ca[sub x]Mg[sub 1[minus]x])Zr[sub 4](PO[sub 4])[sub 6] where x is between 0.5 and 0.99, are produced by solid state and sol-gel processes. In a preferred embodiment, when x is between 0.5 and 0.8, the MgCZP materials have near-zero coefficients of thermal expansion. The MgCZPs of the present invention also show unusually low thermal conductivities, and are stable at high temperatures. Macrostructures formed from MgCZP are useful in a wide variety of high-temperature applications. In a preferred process, calcium, magnesium, and zirconium nitrate solutions have their pH adjusted to between 7 and 9 either before or after the addition of ammonium dihydrogen phosphate. After dehydration to a gel, and calcination at temperatures in excess of 850 C for approximately 16 hours, single phase crystalline MgCZP powders with particle sizes ranging from approximately 20 nm to 50 nm result. The MgCZP powders are then sintered at temperatures ranging from 1200 C to 1350 C to form solid macrostructures with near-zero bulk coefficients of thermal expansion and low thermal conductivities. Porous macrostructures of the MgCZP powders of the present invention are also formed by combination with a polymeric powder and a binding agent, and sintering at high temperatures. The porosity of the resulting macrostructures can be adjusted by varying the particle size of the polymeric powder used. 7 figs.

Phase behavior and reactive transport of partial melt in heterogeneous mantle model

NASA Astrophysics Data System (ADS)

Jordan, J.; Hesse, M. A.

2013-12-01

The reactive transport of partial melt is the key process that leads to the chemical and physical differentiation of terrestrial planets and smaller celestial bodies. The essential role of the lithological heterogeneities during partial melting of the mantle is increasingly recognized. How far can enriched melts propagate while interacting with the ambient mantle? Can the melt flow emanating from a fertile heterogeneity be localized through a reactive infiltration feedback in a model without exogenous factors or contrived initial conditions? A full understanding of the role of heterogeneities requires reactive melt transport models that account for the phase behavior of major elements. Previous work on reactive transport in the mantle focuses on trace element partitioning; we present the first nonlinear chromatographic analysis of reactive melt transport in systems with binary solid solution. Our analysis shows that reactive melt transport in systems with binary solid solution leads to the formation of two separate reaction fronts: a slow melting/freezing front along which enthalpy change is dominant and a fast dissolution/precipitation front along which compositional changes are dominated by an ion-exchange process over enthalpy change. An intermediate state forms between these two fronts with a bulk-rock composition and enthalpy that are not necessarily bounded by the bulk-rock composition and enthalpy of either the enriched heterogeneity or the depleted ambient mantle. The formation of this intermediate state makes it difficult to anticipate the porosity changes and hence the stability of reaction fronts. Therefore, we develop a graphical representation for the solution that allows identification of the intermediate state by inspection, for all possible bulk-rock compositions and enthalpies of the heterogeneity and the ambient mantle. We apply the analysis to the partial melting of an enriched heterogeneity. This leads to the formation of moving precipitation front that followes a stationary melting front which creates low porosity intermediate states. Therefore, localization of the melt flow is not observed because the precipitation front is stable and the melting front is always stationary under these conditions. This analysis illustrates the counterintuitive behavior that can arise when the phase behavior is taken into account and is a first step to understanding reactive melt transport and the reactive constraints on channelization in partial melts. ¬¬

Ice sintering timescales at the surface of Europa and implications for surface properties

NASA Astrophysics Data System (ADS)

Phillips, C. B.; Molaro, J.; Meirion-Griffith, G.

2017-12-01

The planned exploration of Europa by NASA's Europa Clipper Mission and the possibility of a future Europa lander have driven the need to characterize its surface strength, roughness, porosity, thermal conductivity, and regolith depth in order to accurately interpret remote sensing data and develop appropriate spacecraft landing systems. Many processes contribute to Europa's landscape evolution, such as sputtering, mass wasting, thermal segregation, and impact gardening, driving the creation and distribution of icy regolith across the surface. While the efficacy of these processes are not well constrained, any amount of regolith emplaced at the surface will undergo subsequent processing due to sintering. Ice sintering is a form of frost metamorphism whereby contacting ice grains experience the diffusion of material into their contact region, forming a "neck" between them and densifying over time. Over long enough timescales, ice aggregates will sinter into solid material, which may contribute to the incorporation of non-ice material into Europa's subsurface and help to drive subsurface chemistry. Sintering also interacts with other processes, adding to the complexity of icy surface evolution. For example, sputtering preferentially removes larger grains and may enhance sintering rates, and changes in ice porosity may affect the response of the surface to micrometeorite impacts. Quantifying the effects of ice sintering will allow us to predict the microstructural properties of Europa's surface at spacecraft scales. To this end, we have modeled pressure-less (no overburden) sintering of spherical water-ice grains and validated the results with a laboratory experiment. We also modeled ice at the surface of Europa to obtain a first-order approximation of the sintering timescale and surface properties. Preliminary results indicate that ice grains will experience neck growth but not significant densification over Europa's surface age, suggesting that loose surface ice forms a weak and porous crust. Furthermore, our results suggest that existing models do not accurately quantify all stages of the sintering process for ice, emphasizing the need for more laboratory studies on this topic.

Enhancement in superconducting properties of Bi2Sr2Ca1Cu2O8+θ (Bi-2212) by means of boron oxide additive

NASA Astrophysics Data System (ADS)

Fallah-Arani, Hesam; Baghshahi, Saeid; Sedghi, Arman; Stornaiuolo, Daniela; Tafuri, Francesco; Riahi-Noori, Nastaran

2018-05-01

By using a solid state method, Bi2Sr2Ca1Cu2O8+θ (Bi-2212) polycrystalline samples were synthesized with the addition of boron oxide additive, with the aim of improving the performance of this compound for large scale applications. As the first step, the parameters for the solid state method, in particular sintering temperature, were optimized in order to obtain pure Bi-2212 samples with an optimal microstructure. Then, based on this optimization, the properties of the Bi2Sr2Ca1Cu2BxOy samples with x = 0.05, 0.1, and 0.2 were studied using several characterization techniques. It was found that the sample having x = 0.05 showed a magnetic hysteresis loop larger than that of the pure Bi-2212 sample and a critical current density value of 3.71 × 105 A/cm2, comparable to the best results found in the literature for Bi-2212, while preserving well-stacked and oriented grains.

Separation of uranium from (U, Th)O 2 and (U, Pu)O 2 by solid state reactions route

NASA Astrophysics Data System (ADS)

Keskar, Meera; Mudher, K. D. Singh; Venugopal, V.

2005-01-01

Solid state reactions of UO 2, ThO 2, PuO 2 and their mixed oxides (U, Th)O 2 and (U, Pu)O 2 were carried out with sodium nitrate upto 900 °C, to study the formation of various phases at different temperatures, which are amenable for easy dissolution and separation of the actinide elements in dilute acid. Products formed by reacting unsintered as well as sintered UO 2 with NaNO 3 above 500 °C were readily soluble in 2 M HNO 3, whereas ThO 2 and PuO 2 did not react with NaNO 3 to form any soluble products. Thus reactions of mixed oxides (U, Th)O 2 and (U, Pu)O 2 with NaNO 3 were carried out to study the quantitative separation of U from (U, Th)O 2 and (U, Pu)O 2. X-ray diffraction, X-ray fluorescence, thermal analysis and chemical analysis techniques were used for the characterization of the products formed during the reactions.

Interfacial Reactivity Benchmarking of the Sodium Ion Conductors Na3PS4 and Sodium β-Alumina for Protected Sodium Metal Anodes and Sodium All-Solid-State Batteries.

PubMed

Wenzel, Sebastian; Leichtweiss, Thomas; Weber, Dominik A; Sann, Joachim; Zeier, Wolfgang G; Janek, Jürgen

2016-10-05

The interfacial stability of solid electrolytes at the electrodes is crucial for an application of all-solid-state batteries and protected electrodes. For instance, undesired reactions between sodium metal electrodes and the solid electrolyte form charge transfer hindering interphases. Due to the resulting large interfacial resistance, the charge transfer kinetics are altered and the overvoltage increases, making the interfacial stability of electrolytes the limiting factor in these systems. Driven by the promising ionic conductivities of Na 3 PS 4 , here we explore the stability and viability of Na 3 PS 4 as a solid electrolyte against metallic Na and compare it to that of Na-β″-Al 2 O 3 (sodium β-alumina). As expected, Na-β″-Al 2 O 3 is stable against sodium, whereas Na 3 PS 4 decomposes with an increasing overall resistance, making Na-β″-Al 2 O 3 the electrolyte of choice for protected sodium anodes and all-solid-state batteries.

Expansion during the formation of the magnesium aluminate spinel (MgAl(2)O(4)) from its basic oxide (MgO and Al(2)O(3)) powders

NASA Astrophysics Data System (ADS)

Duncan, Flavia Cunha

The extraordinary expansion during the reaction sintering of the magnesium aluminate spinel (MgAl2O4) from its basic oxide (MgO and Al2O3) powders was studied. Experimental series of different size fractions of the reacting materials were formulated to produce the Mg-Al spinel. After batches were prepared, specimens were compacted and fired in air from 1200° to 1700°C for a fixed firing time. A separate set of specimens was fired as a function of time to determine the reaction kinetic parameters. Dimensional changes confirmed that extraordinary expansions of three to four times greater than the prediction from the reaction of solids occur. The solid-state reactions were monitored by X-ray diffraction. The activation energy of the spinel reaction formation was determined to be 280 +/- 20 kJ/mol. It is believed to be associated with the diffusivity of Mg 2+ in either magnesia or spinel during the development of the final spinel structure. New porosity developed in the compacts during the reaction formation of spinel. Scanning electron microscopy confirmed that the magnesia evaporated leaving behind porous magnesia grains, condensed on the alumina particles and reacted to form a shell of spinel. Hollow spinel particles resulted from the original particles of alumina. These porosities generated within the reacting materials influenced the expansions. Final volumetric expansion could potentially reach 56% as a result of the reaction of solids and the porosity generation within MgO and Al2O3. Models of a single alumina particle with and without development of internal porosity were developed. 3-D arrangements of particles showed additional porosity, influencing on the expansions. The decrease in porosity of some specimens fired at higher temperatures indicated that sintering and densification occur simultaneously with the reaction formation of spinel. The decrease in the interparticle porosity limits the full expansion of the particulates to levels lower than the predictions of the model. A term that accounts for this shrinkage should be a significant addition to the model of expansion. Although the spinel forming reaction for most of the particle systems reached near completion, the resulting porous specimens could be viewed as powder compacts in the early stages of sintering and densification.

Comparative study of phase transition and textural changes upon calcination of two commercial titania samples: A pure anatase and a mixed anatase-rutile

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kordouli, Eleana; Dracopoulos, Vassileios; Vaimakis, Tiverios

2015-12-15

The effect of calcination temperature and time on structural and textural changes of two commercial TiO{sub 2} samples (pure anatase and a mixture of anatase and rutile) has been investigated using N{sub 2} physisorption, ex-situ and in-situ X-ray powder diffraction, differential scanning calorimetry and UV–vis diffuse reflectance spectroscopy. The increase of the calcination temperature (up to 700 °C) and time (up to 8 h) causes only textural changes in the pure anatase, whereas a transformation of the anatase to rutile takes place, in addition, in the mixed titania (containing anatase and rutile). The textural changes observed in pure anatase samplemore » were attributed to solid state diffusion leading to an increase in the size of anatase nanocrystals, through sintering. Thus, the mean pore diameter shifts to higher values and the pore volume and specific surface area decrease. The successful application of the Johnson–Mehl–Avrami–Kolmogorov model in the kinetic data concerning the pure anatase indicates a mass transfer control of sintering process. Similar textural changes were also observed upon calcination of the sample containing anatase and rutile. In this case not only sintering but the anatase to rutile transformation contributes also to the textural changes. Kinetic analysis showed that the rutile nanocrystals in the mixed titania served as seed for by-passing the high energy barrier nucleation step allowing/facilitating thus the anatase to rutile transformation. A fine control of the anatase to rutile ratio and thus of energy-gap and the population of hetero-junctions may be obtained by adjusting the calcination temperature and time. - Graphical Abstract: Dependence of anatase content of P25 on the calcination temperature (600 °C (■), 650 °C (●), 700 °C (▲)) and time. - Highlights: • Increase of calcination temperature up to 800 °C and time up to 8 h causes only textural changes in pure anatase • Progressive transformation of anatase to rutile with time takes place in the mixed titania above 600 °C • A high activation energy barrier inhibits the solid state transformation in pure anatase • Rutile nanocrystals in mixed titania serve as seeding for favouring transformation • Calcination temperature and time allow a fine control of E{sub g} and heterojunctions population in mixed titania.« less

SEPARATION OF PLUTONIUM VALUES FROM URANIUM AND FISSION PRODUCT VALUES

DOEpatents

Maddock, A.G.; Booth, A.H.

1960-09-13

Separation of plutonium present in small amounts from neutron irradiated uranium by making use of the phenomenon of chemisorption is described. Plutonium in the tetravalent state is chemically absorbed on a fluoride in solid form. The steps for the separation comprise dissolving the irradiated uranium in nitric acid, oxidizing the plutonium in the resulting solution to the hexavalent state, adding to the solution a soluble calcium salt which by the common ion effect inhibits dissolution of the fluoride by the solution, passing the solution through a bed or column of subdivided calcium fluoride which has been sintered to about 8OO deg C to remove the chemisorbable fission products, reducing the plutonium in the solution thus obtained to the tetravalent state, and again passing the solution through a similar bed or column of calcium fluoride to selectively absorb the plutonium, which may then be recovered by treating the calcium fluoride with a solution of ammonium oxalate.

Coarsening in Solid-Liquid Mixtures Studied on the Space Shuttle

NASA Technical Reports Server (NTRS)

Caruso, John J.

1999-01-01

Ostwald ripening, or coarsening, is a process in which large particles in a two-phase mixture grow at the expense of small particles. It is a ubiquitous natural phenomena occurring in the late stages of virtually all phase separation processes. In addition, a large number of commercially important alloys undergo coarsening because they are composed of particles embedded in a matrix. Many of them, such as high-temperature superalloys used for turbine blade materials and low-temperature aluminum alloys, coarsen in the solid state. In addition, many alloys, such as the tungsten-heavy metal systems, coarsen in the solid-liquid state during liquid phase sintering. Numerous theories have been proposed that predict the rate at which the coarsening process occurs and the shape of the particle size distribution. Unfortunately, these theories have never been tested using a system that satisfies all the assumptions of the theory. In an effort to test these theories, NASA studied the coarsening process in a solid-liquid mixture composed of solid tin particles in a liquid lead-tin matrix. On Earth, the solid tin particles float to the surface of the sample, like ice in water. In contrast, in a microgravity environment this does not occur. The microstructures in the ground- and space-processed samples (see the photos) show clearly the effects of gravity on the coarsening process. The STS-83-processed sample (right image) shows nearly spherical uniformly dispersed solid tin particles. In contrast, the identically processed, ground-based sample (left image) shows significant density-driven, nonspherical particles, and because of the higher effective solid volume fraction, a larger particle size after the same coarsening time. The "Coarsening in Solid-Liquid Mixtures" (CSLM) experiment was conducted in the Middeck Glovebox facility (MGBX) flown aboard the shuttle in the Microgravity Science Laboratory (MSL-1/1R) on STS-83/94. The primary objective of CSLM is to measure the temporal evolution of the solid particles during coarsening.

Microwave dielectric properties of CaCu3Ti4O12-Al2O3 composite

NASA Astrophysics Data System (ADS)

Rahman, Mohd Fariz Ab; Abu, Mohamad Johari; Karim, Saniah Ab; Zaman, Rosyaini Afindi; Ain, Mohd Fadzil; Ahmad, Zainal Arifin; Mohamed, Julie Juliewatty

2016-07-01

(1-x)CaCu3Ti4O12 + (x)Al2O3 composite (0 ≤ x ≤0.25) was prepared via conventional solid-state reaction method. The fabrication of sample was started with synthesizing stoichiometric CCTO from CaCO3, CuO and TiO2 powders, then wet-mixed in deionized water for 24 h. The process was continued with calcined CCTO powder at 900 °C for 12 h before sintered at 1040 °C for 10 h. Next, the calcined CCTO powder with different amount of Al2O3 were mixed for 24 h, then palletized and sintered at 1040 °C for 10. X-ray diffraction analysis on the sintered samples showed that CCTO powder was in a single phase, meanwhile the trace of secondary peaks which belong to CaAl2O4 and Corundum (Al2O3) could be observed in the other samples Scanning electron microscopy analysis showed that the grain size of the sample is firstly increased with addition of Al2O3 (x = 0.01), then become smaller with the x > 0.01. Microwave dielectric properties showed that the addition of Al2O3 (x = 0.01) was remarkably reduced the dielectric loss while slightly increased the dielectric permittivity. However, further addition of Al2O3 was reduced both dielectric loss and permittivity at least for an order of magnitude.

Thermal Test on Target with Pressed Disks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Woloshun, Keith Albert; Dale, Gregory E.; Olivas, Eric Richard

A thorough test of the thermal performance of a target for Mo 99 production using solid Mo 100 target to produce the Mo 99 via a gamma-n reaction has previously been conducted at Argonne National Laboratory (ANL). The results are reported in “Zero Degree Line Mo Target Thermal Test Results and Analysis,” LANL report Number LA-UR-15-23134 dated 3/27/15. This target was comprised of 25 disks 1 mm thick and 12 mm in diameter, separated by helium coolant gaps 0.5 mm wide. The test reported in the above referenced report was conducted with natural Mo disks all cut from commercial rod.more » The production plant will have Mo 100 disks pressed and sintered using a process being developed at Oak Ridge National Laboratory (ORNL). The structural integrity of press-and-sinter disks is of some concern. The test reported herein included 4 disks made by the ORNL process and placed in the high heat, and therefore high thermal stress, region of the target. The electron beam energy was 23 MeV for these tests. Beam spot size was 3.5 mm horizontal and 3 mm vertical, FWHM. The thermal stress test of pressed-and-sintered disks resulted in no mechanical failures. The induced thermal stresses were below yield stress for natural Mo, indicating that up to that stress state no inherent deficiencies in the mechanical properties of the fabricated disks were evident.« less

SnO2/CNT nanocomposite supercapacitors fabricated using scanning atmospheric-pressure plasma jets

NASA Astrophysics Data System (ADS)

Xu, Chang-Han; Chiu, Yi-Fan; Yeh, Po-Wei; Chen, Jian-Zhang

2016-08-01

SnO2/CNT electrodes for supercapacitors are fabricated by first screen-printing pastes containing SnO2 nanoparticles and CNTs on carbon cloth, following which nitrogen atmospheric pressure plasma jet (APPJ) sintering is performed at various APPJ scan rates. The APPJ scan rates change the time intervals for which the reactive plasma species and the heat of the nitrogen APPJs influence the designated sintering spot on the carbon cloth, resulting in APPJ-sintered SnO2/CNT nanocomposites with different properties. The water contact angle decreases with the APPJ scan rate. The improved wettability can facilitate the penetration of the electrolyte into the nanopores of the SnO2/CNT nanocomposites, thereby improving the charge storage and specific capacitance of the supercapacitors. Among the three tested APPJ scan rates, 1.5, 3, and 6 mm s-1, the SnO2/CNT supercapacitor sintered by APPJ under the lowest APPJ scan rate of 1.5 mm s-1 shows the best specific capacitance of ˜90 F g-1 as evaluated by cyclic voltammetry under a potential scan rate of 2 mV s-1. A high APPJ scan rate may result in low degree of materials activation and sintering, leading to poorer performance of SnO2/CNT supercapacitors. The results suggest the feasibility of an APPJ roll-to-roll process for the fabrication of SnO2/CNT nanocomposite supercapacitors.

Development of Al2O3 electrospun fibers prepared by conventional sintering method or plasma assisted surface calcination

NASA Astrophysics Data System (ADS)

Mudra, E.; Streckova, M.; Pavlinak, D.; Medvecka, V.; Kovacik, D.; Kovalcikova, A.; Zubko, P.; Girman, V.; Dankova, Z.; Koval, V.; Duzsa, J.

2017-09-01

In this paper, the electrospinning method was used for preparation of α-Al2O3 microfibers from PAN/Al(NO3)3 precursor solution. The precursor fibers were thermally treated by conventional method in furnace or low-temperature plasma induced surface sintering method in ambient air. The four different temperatures of PAN/Al(NO3)3 precursors were chosen for formation of α-Al2O3 phase by conventional sintering way according to the transition features observed in the TG/DSC analysis. In comparison, the low-temperature plasma treatment at atmospheric pressure was used as an alternative sintering method at the exposure times of 5, 10 and 30 min. FTIR analysis was used for evaluation of residual polymer after plasma induced calcination and for studying the mechanism of polymer degradation. The polycrystalline alumina fibers arranged with the nanoparticles was created continuously throughout the whole volume of the sample. On the other side the low temperature approach, high density of reactive species and high power density of plasma generated at atmospheric pressure by used plasma source allowed rapid removal of polymer in preference from the surface of fibers leading to the formation of composite ceramic/polymer fibers. This plasma induced sintering of PAN/Al(NO3)3 can have obvious importance in industrial applications where the ceramic character of surface with higher toughness of the fibers are required.

Mechanical parameters of strontium doped hydroxyapatite sintered using microwave and conventional methods.

PubMed

Curran, Declan J; Fleming, Thomas J; Towler, Mark R; Hampshire, Stuart

2011-11-01

The effects of ion substitution in hydroxyapatite (HA) on crystal structure and lattice stability is investigated in the green state and post sintering. The effects of ion incorporation on the biaxial flexural strength and hardness are also investigated. Sintering is carried out at 1200 °C using comparative conventional and microwave regimes. Post sintering, the effects of ion incorporation manifest as an increase in the lattice d-spacings and a reduction of the crystallite size. Some HA decomposition occurs with β-TCP stabilisation in conventional sintering (CS), but this phase is destabilised during microwave sintering (MS), generating α-TCP. Conventional sintering (CS) allows higher densification in the undoped samples. Overall, for the Sr-doped compositions, the MS samples retain higher amounts of HA and experience higher density levels compared to the CS samples. Published by Elsevier Ltd.

Study of Ti 4+ substitution in ZrW 2O 8 negative thermal expansion materials

NASA Astrophysics Data System (ADS)

De Buysser, Klaartje; Van Driessche, Isabel; Putte, Bart Vande; Schaubroeck, Joseph; Hoste, Serge

2007-08-01

Powder XRD-analysis and thermo-mechanical analysis on sintered TiO 2-WO 3-ZrO 2 mixtures revealed the formation of Zr 1-xTi xW 2O 8 solid solutions. A noticeable decrease in unit cell parameter ' a' and in the order-disorder transition temperature could be seen in the case of Zr 1-xTi xW 2O 8 solid solutions. Studies performed on other ZrW 2O 8 solid solutions have attributed an increase in phase transition temperature to a decrease in free lattice volume, whereas a decrease in phase transition temperature was suggested to be due to the presence of a more disordered state. Our studies indicate that the phase transition temperature in our materials is strongly influenced by the bond dissociation energy of the substituting ion-oxygen bond. A decrease in bond strength may compensate for the effect of a decrease in lattice free volume, lowering the phase transition temperature as the degree of substitution by Ti 4+ increases. This hypothesis is proved by differential scanning calorimetry.

Advanced Ceramic Technology for Space Applications at NASA MSFC

NASA Technical Reports Server (NTRS)

Alim, Mohammad A.

2003-01-01

The ceramic processing technology using conventional methods is applied to the making of the state-of-the-art ceramics known as smart ceramics or intelligent ceramics or electroceramics. The sol-gel and wet chemical processing routes are excluded in this investigation considering economic aspect and proportionate benefit of the resulting product. The use of ceramic ingredients in making coatings or devices employing vacuum coating unit is also excluded in this investigation. Based on the present information it is anticipated that the conventional processing methods provide identical performing ceramics when compared to that processed by the chemical routes. This is possible when sintering temperature, heating and cooling ramps, peak temperature (sintering temperature), soak-time (hold-time), etc. are considered as variable parameters. In addition, optional calcination step prior to the sintering operation remains as a vital variable parameter. These variable parameters constitute a sintering profile to obtain a sintered product. Also it is possible to obtain identical products for more than one sintering profile attributing to the calcination step in conjunction with the variables of the sintering profile. Overall, the state-of-the-art ceramic technology is evaluated for potential thermal and electrical insulation coatings, microelectronics and integrated circuits, discrete and integrated devices, etc. applications in the space program.

Mechanical strength and thermophysical properties of PM212: A high temperature self-lubricating powder metallurgy composite

NASA Technical Reports Server (NTRS)

Edwards, Phillip M.; Sliney, Harold E.; Dellacorte, Christopher; Whittenberger, J. Daniel; Martineau, Robert R.

1990-01-01

A powder metallurgy composite, PM212, composed of metal bonded chromium carbide and solid lubricants is shown to be self-lubricating to a maximum application temperature of 900 C. The high temperature compressive strength, tensile strength, thermal expansion and thermal conductivity data needed to design PM212 sliding contact bearings and seals are reported for sintered and isostatically pressed (HIPed) versions of PM212. Other properties presented are room temperature density, hardness, and elastic modulus. In general, both versions appear to have adequate strength to be considered as sliding contact bearing materials, but the HIPed version, which is fully dense, is much stronger than the sintered version which contains about 20 percent pore volume. The sintered material is less costly to make, but the HIPed version is better where high compressive strength is important.

Method of preparing a sintered lithium aluminate structure for containing electrolyte

DOEpatents

Sim, James W.; Kinoshita, Kimio

1981-01-01

A porous sintered tile is formed of lithium aluminate for retaining molten lectrolyte within a fuel cell. The tile is prepared by reacting lithium hydroxide in aqueous solution with alumina particles to form beta lithium aluminate particles. The slurry is evaporated to dryness and the solids dehydrated to form a beta lithium aluminate powder. The powder is compacted into the desired shape and sintered at a temperature in excess of 1200 K. but less than 1900 K. to form a porous integral structure that is subsequently filled with molten electrolyte. A tile of this type is intended for use in containing molten alkali metal carbonates as electolyte for use in a fuel cell having porous metal or metal oxide electrodes for burning a fuel gas such as hydrogen and/or carbon monoxide with an oxidant gas containing oxygen.

Silver Oxalate Ink with Low Sintering Temperature and Good Electrical Property

NASA Astrophysics Data System (ADS)

Yang, Wendong; Wang, Changhai; Arrighi, Valeria

2018-02-01

Favorable conductivity at low temperature is desirable for flexible electronics technology, where formulation of a suitable ink material is very critical. In this paper, a type of silver organic decomposable ink (10 wt.% silver content) was formulated by using as-prepared silver oxalate and butylamine, producing silver films with good uniformity and conductivity on a polyimide substrate after sintering below 130°C (15.72 μΩ cm) and even at 100°C (36.29 μΩ cm). Silver oxalate powder with good properties and an appropriate solid amine complex with lower decomposition temperature were synthesized, both differing from those reported in the literature. The influence of the factors on the electrical properties of the produced silver films such as sintering temperature and time was studied in detail and the relationship between them was demonstrated.

Electrical and dielectric properties of ZnO and CeO{sub 2} doped ZrTi{sub 2}O{sub 6} ceramic

DOE Office of Scientific and Technical Information (OSTI.GOV)

George, Aneesh; Thomas, Jijimon K.; John, Annamma

2014-01-28

Zirconium oxide (ZrO{sub 2}) and titanium dioxide (TiO{sub 2}) are the important catalyst supports, since it has acidic and basic properties. The intermediate phase zirconium titanate ZrTi{sub 2}O{sub 6}, which is a solid solution with Zr:Ti ratio 1:2 has outstanding dielectric properties. The effects of doping of ZnO and CeO{sub 2} on the dielectric and electrical properties of ZrTi{sub 2}O{sub 6} ceramic are investigated. On adding 0.5 wt% ZnO, the dielectric constant is increased but, on adding CeO{sub 2}, the dielectric constant is decreased. The bulk density of pure sample sintered at 1530 °C is 91% of theoretical density whilemore » that of the doped samples sintered at 1450 °C is more than 94% of theoretical density. Scanning electron micrographs reveal that the samples are well sintered with minimum porosity. The semicircle behavior in the Cole-Cole plots at room temperature reveals that the samples are good ionic conductor. The induced impedance is reduced for doped samples and this can be used as a material for electrolyte in Solid Oxide Fuel Cell.« less

Effect of fabrication parameters on coating properties of tubular solid oxide fuel cell electrolyte prepared by vacuum slurry coating

NASA Astrophysics Data System (ADS)

Son, Hui-Jeong; Song, Rak-Hyun; Lim, Tak-Hyoung; Lee, Seung-Bok; Kim, Sung-Hyun; Shin, Dong-Ryul

The process of vacuum slurry coating for the fabrication of a dense and thin electrolyte film on a porous anode tube is investigated for application in solid oxide fuel cells. 8 mol% yttria stabilized zirconia is coated on an anode tube by vacuum slurry-coating process as a function of pre-sintering temperature of the anode tube, vacuum pressure, slurry concentration, number of coats, and immersion time. A dense electrolyte layer is formed on the anode tube after final sintering at 1400 °C. With decrease in the pre-sintering temperature of the anode tube, the grain size of the coated electrolyte layer increases and the number of surface pores in the coating layer decreases. This is attributed to a reduced difference in the respective shrinkage of the anode tube and the electrolyte layer. The thickness of the coated electrolyte layer increases with the content of solid powder in the slurry, the number of dip-coats, and the immersion time. Although vacuum pressure has no great influence on the electrolyte thickness, higher vacuum produces a denser coating layer, as confirmed by low gas permeability and a reduced number of defects in the coating layer. A single cell with the vacuum slurry coated electrolyte shows a good performance of 620 mW cm -2 (0.7 V) at 750 °C. These experimental results indicate that the vacuum slurry-coating process is an effective method to fabricate a dense thin film on a porous anode support.

Equilibrium, kinetic, and reactive transport models for plutonium

NASA Astrophysics Data System (ADS)

Schwantes, Jon Michael

Equilibrium, kinetic, and reactive transport models for plutonium (Pu) have been developed to help meet environmental concerns posed by past war-related and present and future peacetime nuclear technologies. A thorough review of the literature identified several hurdles that needed to be overcome in order to develop capable predictive tools for Pu. These hurdles include: (1) missing or ill-defined chemical equilibrium and kinetic constants for environmentally important Pu species; (2) no adequate conceptual model describing the formation of Pu oxy/hydroxide colloids and solids; and (3) an inability of two-phase reactive transport models to adequately simulate Pu behavior in the presence of colloids. A computer program called INVRS K was developed that integrates the geochemical modeling software of PHREEQC with a nonlinear regression routine. This program provides a tool for estimating equilibrium and kinetic constants from experimental data. INVRS K was used to regress on binding constants for Pu sorbing onto various mineral and humic surfaces. These constants enhance the thermodynamic database for Pu and improve the capability of current predictive tools. Time and temperature studies of the Pu intrinsic colloid were also conducted and results of these studies were presented here. Formation constants for the fresh and aged Pu intrinsic colloid were regressed upon using INVRS K. From these results, it was possible to develop a cohesive diagenetic model that describes the formation of Pu oxy/hydroxide colloids and solids. This model provides for the first time a means of deciphering historically unexplained observations with respect to the Pu intrinsic colloid, as well as a basis for simulating the behavior within systems containing these solids. Discussion of the development and application of reactive transport models is also presented and includes: (1) the general application of a 1-D in flow, three-phase (i.e., dissolved, solid, and colloidal), reactive transport model; (2) a simulation of the effects of dissolution of PuO2 solid and radiolysis on the behavior of Pu diffusing out of a confined pore space; and (3) application of a steady-state three phase reactive transport model to groundwater at the Nevada Test Site.

Effects of sintering temperature on the microstructural evolution and wear behavior of WCp reinforced Ni-based coatings

NASA Astrophysics Data System (ADS)

Chen, Chuan-hui; Bai, Yang; Ye, Xu-chu

2014-12-01

This article focuses on the microstructural evolution and wear behavior of 50wt%WC reinforced Ni-based composites prepared onto 304 stainless steel substrates by vacuum sintering at different sintering temperatures. The microstructure and chemical composition of the coatings were investigated by X-ray diffraction (XRD), differential thermal analysis (DTA), scanning and transmission electron microscopy (SEM and TEM) equipped with energy-dispersive X-ray spectroscopy (EDS). The wear resistance of the coatings was tested by thrust washer testing. The mechanisms of the decomposition, dissolution, and precipitation of primary carbides, and their influences on the wear resistance have been discussed. The results indicate that the coating sintered at 1175°C is composed of fine WC particles, coarse M6C (M=Ni, Fe, Co, etc.) carbides, and discrete borides dispersed in solid solution. Upon increasing the sintering temperature to 1225°C, the microstructure reveals few incompletely dissolved WC particles trapped in larger M6C, Cr-rich lamellar M23C6, and M3C2 in the austenite matrix. M23C6 and M3C2 precipitates are formed in both the γ/M6C grain boundary and the matrix. These large-sized and lamellar brittle phases tend to weaken the wear resistance of the composite coatings. The wear behavior is controlled simultaneously by both abrasive wear and adhesive wear. Among them, abrasive wear plays a major role in the wear process of the coating sintered at 1175°C, while the effect of adhesive wear is predominant in the coating sintered at 1225°C.

Wafer-scale development and experimental verification of 0.36 mm2 228 mV open-circuit-voltage solid-state CMOS-compatible glucose fuel cell

NASA Astrophysics Data System (ADS)

Arata, Shigeki; Hayashi, Kenya; Nishio, Yuya; Kobayashi, Atsuki; Nakazato, Kazuo; Niitsu, Kiichi

2018-04-01

The world’s smallest (0.36 mm2) solid-state CMOS-compatible glucose fuel cell, which exhibits an open-circuit voltage (OCV) of 228 mV and a power generation density of 1.32 µW/cm2 with a 30 mM glucose solution, is reported in this paper. Compared with conventional wet etching, dry etching (reactive ion etching) for patterning minimizes damage to the anode and cathode, resulting in a cell with a small size and a high OCV, sufficient for CMOS circuit operation.

Multicycle study on chemical-looping combustion of simulated coal gas with a CaSO{sub 4} oxygen carrier in a fluidized bed reactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Qilei Song; Rui Xiao; Zhongyi Deng

2008-11-15

The cyclic test of a CaSO{sub 4}-based oxygen carrier (natural anhydrite) in alternating reducing simulated coal gas and oxidizing conditions was performed at 950{degree}C in a fluidized bed reactor at atmospheric pressure. A high concentration of CO{sub 2} was obtained in the reduction. The H{sub 2} and CO conversions and CO{sub 2} yield increased initially and final decreased significantly. The release of SO{sub 2} and H{sub 2}S during the cyclic test was found to be responsible for the decrease of reactivity of a CaSO{sub 4} oxygen carrier. The oxygen carrier conversion after the reduction reaction decreased gradually in the cyclicmore » test. Through the comparison of mass-based reaction rates as a function of mass conversion at typical cycles, it was also evident that the reactivity of a CaSO{sub 4} oxygen carrier increased for the initial cycles but finally decreased after around 15 cycles. X-ray diffraction analysis revealed that the presence and intensity of the reduction sulfur species was in accordance with the results of gas conversion. The content of CaO was higher than expected, suggesting the formation of SO{sub 2} and H{sub 2}S during the cycles. Surface morphology analysis demonstrates that the natural anhydrite particle surface varied from impervious to porous after the cyclic test. It was also observed that the small grains on the surface of the oxygen carrier sintered in the cyclic tests. Energy-dispersive spectrum analysis also demonstrated the decrease of oxygen intensity after reduction, and CaO became the main component after the 20th oxidation. Pore structure analysis suggested that the particles agglomerated or sintered in the cyclic tests. The possible method for sulfur mitigation is proposed. Finally, some basic consideration on the design criteria of a CLC system for solid fuels using a CaSO{sub 4} oxygen carrier is discussed by the references and provides direction for future work. 49 refs., 10 figs., 5 tabs.« less

Fabrication of Titanium Oxide-Based Composites by Reactive SPS Sintering and Their Thermoelectric Properties

NASA Astrophysics Data System (ADS)

Fuda, K.; Shoji, T.; Kikuchi, S.; Kunihiro, Y.; Sugiyama, S.

2013-07-01

Titanium oxide-based composites containing (1) Nb, (2) Nb and Sr, and (3) Sr and La were fabricated by a combination of wet processing and reactive spark plasma sintering in which the metal oxide components were reduced by reaction with titanium nitride. If only TiO2 was used as the starting material, several Magneli-type phases of oxygen-deficient titanium oxides were obtained. When mixed with Nb ions with Ti:Nb = 0.9:0.1, microsegregation of Nb ions was observed (case 1). If Sr was added, a perovskite, SrTiO3 (STO) phase occurred (case 2), which contained La ions in the case of La addition (case 3). The sintered compacts consisted largely of grains of about 1 μm in size. In the case of Ti-Nb combination (case 1), a unique stripe pattern also appeared inside the grains. The electrical conductivity increased monotonically with increasing temperature in the case of the pure Magneli phases and the Nb-containing composite, whereas bow-shaped temperature dependences with a maximum were observed in the case of the composites containing STO phases. The Seebeck coefficients were commonly negative, and the absolute values increased with temperature. The thermal conductivity was between 2 W m-1 K-1 and 4 W m-1 K-1 in the temperature range from room temperature to 800°C. A maximum ZT of 0.34 was achieved at 800°C (case 2).

On the Theory of Reactive Mixtures for Modeling Biological Growth

PubMed Central

Ateshian, Gerard A.

2013-01-01

Mixture theory, which can combine continuum theories for the motion and deformation of solids and fluids with general principles of chemistry, is well suited for modeling the complex responses of biological tissues, including tissue growth and remodeling, tissue engineering, mechanobiology of cells and a variety of other active processes. A comprehensive presentation of the equations of reactive mixtures of charged solid and fluid constituents is lacking in the biomechanics literature. This study provides the conservation laws and entropy inequality, as well as interface jump conditions, for reactive mixtures consisting of a constrained solid mixture and multiple fluid constituents. The constituents are intrinsically incompressible and may carry an electrical charge. The interface jump condition on the mass flux of individual constituents is shown to define a surface growth equation, which predicts deposition or removal of material points from the solid matrix, complementing the description of volume growth described by the conservation of mass. A formu-lation is proposed for the reference configuration of a body whose material point set varies with time. State variables are defined which can account for solid matrix volume growth and remodeling. Constitutive constraints are provided on the stresses and momentum supplies of the various constituents, as well as the interface jump conditions for the electrochem cal potential of the fluids. Simplifications appropriate for biological tissues are also proposed, which help reduce the governing equations into a more practical format. It is shown that explicit mechanisms of growth-induced residual stresses can be predicted in this framework. PMID:17206407

High Capacity Garnet-Based All-Solid-State Lithium Batteries: Fabrication and 3D-Microstructure Resolved Modeling.

PubMed

Finsterbusch, Martin; Danner, Timo; Tsai, Chih-Long; Uhlenbruck, Sven; Latz, Arnulf; Guillon, Olivier

2018-06-21

The development of high-capacity, high-performance all-solid-state batteries requires the specific design and optimization of its components, especially on the positive electrode side. For the first time, we were able to produce a completely inorganic mixed positive electrode consisting only of LiCoO 2 and Ta-substituted Li 7 La 3 Zr 2 O 12 (LLZ:Ta) without the use of additional sintering aids or conducting additives, which has a high theoretical capacity density of 1 mAh/cm 2 . A true all-solid-state cell composed of a Li metal negative electrode, a LLZ:Ta garnet electrolyte, and a 25 μm thick LLZ:Ta + LiCoO 2 mixed positive electrode was manufactured and characterized. The cell shows 81% utilization of theoretical capacity upon discharging at elevated temperatures and rather high discharge rates of 0.1 mA (0.1 C). However, even though the room temperature performance is also among the highest reported so far for similar cells, it still falls far short of the theoretical values. Therefore, a 3D reconstruction of the manufactured mixed positive electrode was used for the first time as input for microstructure-resolved continuum simulations. The simulations are able to reproduce the electrochemical behavior at elevated temperature favorably, however fail completely to predict the performance loss at room temperature. Extensive parameter studies were performed to identify the limiting processes, and as a result, interface phenomena occurring at the cathode active material/solid-electrolyte interface were found to be the most probable cause for the low performance at room temperature. Furthermore, the simulations are used for a sound estimation of the optimization potential that can be realized with this type of cell, which provides important guidelines for future oxide based all-solid-state battery research and fabrication.

Borax as flux on sintering of iron Ancor Steel 1000® under glow discharge

NASA Astrophysics Data System (ADS)

Ariza Suarez, H. G.; Sarmiento Santos, A.; Ortiz Otálora, C. A.

2016-02-01

This work studies the flux effect of borax (di sodium tetraborate decahydrate) on sintering of iron Ancor Steel 1000® in abnormal glow discharge. The incidence of the percentage by weight of borax and the sintering temperature in the process were observed. Samples of powder metallurgical iron were prepared with proportions of 0.50%, 2.0%, 4.0% and 6.0% by weight of borax using the procedures of powder metallurgy. The samples were sintered at 800 and 1100°C for 30min, by glow discharge at low pressure in a reducing atmosphere composed of 20% H2+80% Ar. The samples in compact green-state were analyzed by TGA-DSC to determine the fusion process and mass loss during sintering. The analysis of microhardness and density, shows that at a sintering temperature of 800°C the sample density decreases and the sample microhardness increases with respect to sintered samples without borax. Sintered samples were analysed by DRX showing the absence of precipitates.

Arsenic speciation in sinter mineralization from a hydrothermal channel of El Tatio geothermal field, Chile

NASA Astrophysics Data System (ADS)

Alsina, Marco A.; Zanella, Luciana; Hoel, Cathleen; Pizarro, Gonzalo E.; Gaillard, Jean-François; Pasten, Pablo A.

2014-10-01

El Tatio geothermal field is the principal natural source of arsenic for the Loa River, the main surface water resource in the hyper-arid Atacama Desert (Antofagasta Region, Northern Chile). Prior investigations by bulk X-ray absorption spectroscopy have identified hydrous ferric oxides as the principal arsenic-containing phase in sinter material from El Tatio, suggesting sorption as the main mechanism for arsenic scavenging by the solid phases of these hot spring environments. Here we examine siliceous sinter material sampled from a hydrothermal channel using synchrotron based X-ray micro-probe techniques, including As and Fe Kα X-ray fluorescence (μ-XRF), As K-edge X-ray absorption near edge structure (μ-XANES), and X-ray diffraction (μ-XRD). Least-squares linear fitting of μ-XANES spectra shows that arsenic is predominantly present as arsenate sorbed on hydrous ferric oxides (63% molar proportion), but we also identify nodular arsenide micro-mineralizations (37% molar proportion) similar to loellingite (FeAs2), not previously detected during bulk-scale analysis of the sinter material. Presence of arsenide mineralizations indicates development of anoxic environments on the surface of the siliceous sinter, and suggests a more complex biogeochemistry for arsenic than previously observed for circum-neutral pH brine hot spring environments.

Effect of Acetylene Black Content in Li4Ti5O12 Xerogel Solid-State Anode Materials on Half-Cell Li-ion Batteries Performance

NASA Astrophysics Data System (ADS)

Abdurrahman, N. M.; Priyono, B.; Syahrial, A. Z.; Subhan, A.

2017-07-01

The effect of Acetylene Black (AB) additive contents in lithium titanate/Li4Ti5O12 (LTO) anode on Li-ion Batteries performance is studied in this work. The LTO active material for Li-ion batteries anode was successfully synthesized using sol-gel method to form TiO2 xerogel continued by mixing process with LiOH in ball-mill and then sintered to obtain spinel LTO. The LTO powder is characterized by X-Ray Diffraction (XRD), scanning electron microscopy-Energy Dispersive Spectroscopy (SEM-EDS), and Brunauer-Emmett-Teller (BET). The spinel LTO and TiO2 rutile were detected by XRD diffractogram. The LTO powder is in the form of agglomerates structure. This powder then was mixed with PVDF binder (10%wt) and AB additives with various amount from 10%wt (LTO2 Ac-1), 12%wt (LTO2 Ac-2), and 15%wt (LTO2 Ac-3) of total weight solid content to form electrode sheet. Half-cell coin battery was made with lithium metal foil as a counter electrode. Cyclic voltammetry (CV), Electrochemical-impedance spectroscopy (EIS), and charge discharge (CD) test used to examine the battery performance. The highest resistance value is obtained in LTO2 Ac-3 sample with 15%wt of AB. It might be caused by the formation of side reaction product on electrode surface at initial cycle due to high reactivity of LTO2 Ac-3 electrode. The highest initial capacity at CV test and CD test was obtained in LTO2 Ac-1 (10%wt AB) sample, due to the best proportion of active material content in the compound. While, in the charge-discharge test at high current rate, the best sample rate-capability performance belongs to LTO2 Ac-3 sample (15%wt AB), which still have 24.12 mAh/g of discharge capacity at 10 C with 71.34% capacity loss.

High calcination of ferroelectric BaTiO₃ doped Fe nanoceramics prepared by a solid-state sintering method.

PubMed

Samuvel, K; Ramachandran, K

2015-07-05

This study examined the effects of the combination of starting materials on the properties of solid-state reacted BaTiO3 using two different types of BaCO3 and TiO2. In addition, the effect of mechanochemical activation by high energy milling and the Ba/Ti molar ratio on the reaction temperature, particle size and tetragonality were investigated. The TiO2 phase and size plays a major role in increasing the reaction temperature and particle size. With the optimum selection of starting materials and processing conditions, BaTiO3 with a particle size <200 nm (Scherrer's formula) and a tetragonality c/a of approximately 1.007 was obtained. Broadband dielectric spectroscopy is applied to investigate the electrical properties of disordered perovskite-like ceramics in a wide temperature range. From the X-ray diffraction analysis it was found that the newly obtained BaTi0.5Fe0.5O3 ceramics consist of two chemically different phases. The electric modulus M∗ formalism used in the analysis enabled us to distinguish and separate the relaxation processes, dominated by marked conductivity in the ε∗(ω) representation. Interfacial effects on the dielectric properties of the samples have been understood by Cole-Cole plots in complex impedance and modulus formalism. Modulus formalism has identified the effects of both grain and grain boundary microstructure on the dielectric properties, particularly in solid state routed samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Solid state recycling of aluminium alloys via a porthole die hot extrusion process: Scaling up to production

NASA Astrophysics Data System (ADS)

Paraskevas, Dimos; Kellens, Karel; Deng, Yelin; Dewulf, Wim; Kampen, Carlos; Duflou, Joost R.

2017-10-01

Whereas industrial symbiosis has led to increased energy and resource efficiency in process industries, this concept has not yet been applied in discrete product manufacturing. Metal scrap is first conventionally recycled, for which substantial energy and resource efficiency losses have been reported. Recent research has however proven the feasibility of `meltless' recycling of light metal scrap, yielding a first glimpse of potential industrial symbiosis. Various solid state recycling techniques (such as recycling via hot extrusion or Spark Plasma Sintering) have been proposed for scrap consolidation directly into bulk products or semis by physical disruption and dispersion of the oxide surface film by imposing significant plastic and shear strain. Solid State Recycling (SSR) methods can omit substantial material losses as they bypass the metallurgical recycling step. In this context the case of direct production of bulk aluminium profiles via hot extrusion at industrial scale is demonstrated within this paper. The extrusion tests were performed directly into the production line, highlighting the scaling up potentials and the industrial relevance of this research. A significant amount of machining chips were collected, chemically cleaned and cold compacted into chip based billets with ˜80% relative density. Afterwards the scrap consolidation was achieved by imposing significant plastic and shear deformation into the material during hot extrusion through a modified 2-porthole extrusion die-set. The production process sequence along with microstructural investigations and mechanical properties comparison of the cast based profile used as reference versus the chip based profile are presented.

High calcination of ferroelectric BaTiO3 doped Fe nanoceramics prepared by a solid-state sintering method

NASA Astrophysics Data System (ADS)

Samuvel, K.; Ramachandran, K.

2015-07-01

This study examined the effects of the combination of starting materials on the properties of solid-state reacted BaTiO3 using two different types of BaCO3 and TiO2. In addition, the effect of mechanochemical activation by high energy milling and the Ba/Ti molar ratio on the reaction temperature, particle size and tetragonality were investigated. The TiO2 phase and size plays a major role in increasing the reaction temperature and particle size. With the optimum selection of starting materials and processing conditions, BaTiO3 with a particle size <200 nm (Scherrer's formula) and a tetragonality c/a of approximately 1.007 was obtained. Broadband dielectric spectroscopy is applied to investigate the electrical properties of disordered perovskite-like ceramics in a wide temperature range. From the X-ray diffraction analysis it was found that the newly obtained BaTi0.5Fe0.5O3 ceramics consist of two chemically different phases. The electric modulus M∗ formalism used in the analysis enabled us to distinguish and separate the relaxation processes, dominated by marked conductivity in the ε∗(ω) representation. Interfacial effects on the dielectric properties of the samples have been understood by Cole-Cole plots in complex impedance and modulus formalism. Modulus formalism has identified the effects of both grain and grain boundary microstructure on the dielectric properties, particularly in solid state routed samples.

Fabrication and microstructure of cerium doped lutetium aluminum garnet (Ce:LuAG) transparent ceramics by solid-state reaction method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Junlang, E-mail: lijunlangx@163.com; Xu, Jian, E-mail: xu.jian.57z@st.kyoto-u.ac.jp; Graduate School of Human and Environmental Studies, Division of Materials Function, Kyoto University, Kyoto 606-8501

2014-07-01

Highlights: • We fabricate Ce doped lutetium aluminum garnet ceramics by solid-state method. • The raw materials include Lu{sub 2}O{sub 3} nanopowders synthesized by co-precipitation method. • The density of the transparent ceramics reach 99.7% of the theoretical value. • The optical transmittance of the bulk ceramic at 550 nm was 57.48%. • Some scattering centers decrease the optical characteristic of the ceramic. - Abstract: Polycrystalline Ce{sup 3+} doped lutetium aluminum garnet (Ce:LuAG) transparent ceramics fabricated by one step solid-state reaction method using synthetic nano-sized Lu{sub 2}O{sub 3}, commercial α-Al{sub 2}O{sub 3} and CeO{sub 2} powders were investigated in thismore » paper. The green compacts shaped by the mixed powders were successfully densified into Ce:LuAG transparent ceramics after vacuum sintering at 1750 °C for 10 h. The in-line optical transmittance of the Ce:LuAG ceramic made by home-made Lu{sub 2}O{sub 3} powders could reach 57.48% at 550 nm, which was higher than that of the ceramic made by commercial Lu{sub 2}O{sub 3} powders (22.96%). The microstructure observation showed that light scattering centers caused by micro-pores, aluminum segregation and refraction index inhomogeneities induced the decrease of optical transparency of the Ce:LuAG ceramics, which should be removed and optimized in the future work.« less

Ni-SDC cermet anode for medium-temperature solid oxide fuel cell with lanthanum gallate electrolyte

NASA Astrophysics Data System (ADS)

Zhang, Xinge; Ohara, Satoshi; Maric, Radenka; Mukai, Kazuo; Fukui, Takehisa; Yoshida, Hiroyuki; Nishimura, Masayoshi; Inagaki, Toru; Miura, Kazuhiro

The polarization properties and microstructure of Ni-SDC (samaria-doped ceria) cermet anodes prepared from spray pyrolysis (SP) composite powder, and element interface diffusion between the anode and a La 0.9Sr 0.1Ga 0.8Mg 0.2O 3- δ (LSGM) electrolyte are investigated as a function of anode sintering temperature. The anode sintered at 1250°C displays minimum anode polarization (with anode ohmic loss), while the anode prepared at 1300°C has the best electrochemical overpotential, viz., 27 mV at 300 mA cm -2 operating at 800°C. The anode ohmic loss gradually increases with increase in the sintering temperature at levels below 1300°C, and sharply increases at 1350°C. Electron micrographs show a clear grain growth at sintering temperatures higher than 1300°C. The anode microstructure appears to be optimized at 1300°C, in which nickel particles form a network with well-connected SDC particles finely distributed over the surfaces of the nickel particles. The anode sintered at 1350°C has severe grain growth and an apparent interface diffusion of nickel from the anode to the electrolyte. The nickel interface diffusion is assumed to be the main reason for the increment in ohmic loss, and the resulting loss in anode performance. The findings suggest that sintering Ni-SDC composite powder near 1250°C is the best method to prepare the anode on a LSGM electrolyte.

A green synthesis of a layered titanate, potassium lithium titanate; lower temperature solid-state reaction and improved materials performance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ogawa, Makoto, E-mail: waseda.ogawa@gmail.com; Department of Earth Sciences, Waseda University, 1-6-1 Nishiwaseda, Shinjuku-ku, Tokyo 169-8050; Morita, Masashi, E-mail: m-masashi@y.akane.waseda.jp

2013-10-15

A layered titanate, potassium lithium titanate, with the size range from 0.1 to 30 µm was prepared to show the effects of the particle size on the materials performance. The potassium lithium titanate was prepared by solid-state reaction as reported previously, where the reaction temperature was varied. The reported temperature for the titanate preparation was higher than 800 °C, though 600 °C is good enough to obtain single-phase potassium lithium titanate. The lower temperature synthesis is cost effective and the product exhibit better performance as photocatalysts due to surface reactivity. - Graphical abstract: Finite particle of a layered titanate, potassiummore » lithium titanate, was prepared by solid-state reaction at lower temperature to show modified materials performance. Display Omitted - Highlights: • Potassium lithium titanate was prepared by solid-state reaction. • Lower temperature reaction resulted in smaller sized particles of titanate. • 600 °C was good enough to obtain single phased potassium lithium titanate. • The product exhibited better performance as photocatalyst.« less

Preparation of reactive beta-dicalcium silicate

DOEpatents

Shen, M.S.; Chen, J.M.; Yang, R.T.

1980-02-28

This invention relates to the preparation of fine particles of reactive beta-dicalcium silicate by means of a solid state process which comprises firing a mixture of calcium sulfate, silica, and a reducing additive selected from the group consisting of calcium sulfide, carbon, carbon monoxide, methane, and hydrogen, at a temperature of about 850 to 1000/sup 0/C. A carrier gas such as nitrogen or carbon dioxide may also be added, if desired. A high concentration of sulfur dioxide is a by-product of this process.

Preparation of reactive beta-dicalcium silicate

DOEpatents

Shen, Ming-Shing; Chen, James M.; Yang, Ralph T.

1982-01-01

This invention relates to the preparation of fine particles of reactive beta-dicalcium silicate by means of a solid state process which comprises firing a mixture of calcium sulfate, silica and a reducing additive selected from the group consisting of calcium sulfide, carbon, carbon monoxide, methane and hydrogen, at a temperature of about 850.degree.-1000.degree. C. A carrier gas such as nitrogen or carbon dioxide may also be added, if desired. A high concentration of sulfur dioxide is a by-product of this process.

Process Simulation of Cold Pressing and Sintering of Armstrong CP-Ti Powders

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gorti, Sarma B; Sabau, Adrian S; Peter, William H

A computational methodology is presented for the process simulation of cold pressing and sintering of Armstrong CP-Ti powders. Since the powder consolidation is governed by specific pressure-dependent constitutive equations, solution algorithms were developed for the ABAQUS user material subroutine, UMAT, for computing the plastic strain increments based on an implicit integration of the nonlinear yield function, flow rule, and hardening equations. Sintering was simulated using a model based on diffusional creep using the user subroutine CREEP. The initial mesh, stress, and density for the simulation of sintering were obtained from the results of the cold pressing simulation, minimizing the errorsmore » from decoupling the cold pressing and sintering simulations. Numerical simulation results are presented for the cold compaction followed by a sintering step of the Ti powders. The numerical simulation results for the relative density were compared to those measured from experiments before and after sintering, showing that the relative density can be accurately predicted. Notice: This manuscript has been authored by UT-Battelle, LLC, under Contract No. DE-AC05-00OR22725 with the U.S. Department of Energy. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce the published form of this manuscript, or allow others to do so, for United States Government purposes. ACKNOWLEDGEMENTS This research was sponsored by the U.S. DOE, and carried out at ORNL, under Contract DE-AC05-00OR22725 with UT-Battelle, LLC. This research was sponsored by the U.S. DOE, EERE Industrial Technology Program Office under CPS Agreement # 17881.« less

Anti-aging Friction of Carbonate Fault Mirror and its Microstructural Interpretation

NASA Astrophysics Data System (ADS)

Park, Y.; Ree, J. H.; Hirose, T.

2017-12-01

In our slide-hold-slide (SHS) friction tests on carbonate fault rocks, fault mirror (FM), light reflective mirror-like fault surface, shows almost zero or slightly negative aging rate of friction (`anti-aging' friction), whereas carbonate faults without FM exhibit a positive aging rate. We analyzed microstructures from three types of carbonate faults to explore the cause of the anti-aging friction of FM. The three types of fault rocks before SHS tests were made from Carrara marble; (i) FM, (ii) crushed gouge of former FM (CF), and (iii) gouge produced by pre-shearing of Carrara marble (PR). The fault zone of FM before SHS tests consists of sintered nanograin patches smeared into negative asperities of wall rocks (thickness up to 150 μm) and a sintered gouge layer between wall rocks (thickness up to 200 μm) that is composed of tightly-packed nanograins (50-500 nm in size) with triple junctions and angular-subangular fragments (a few-100 μm) of sintered nanograin aggregates. A straight and discrete Y-shear surface defines a boundary between the gouge layer and the nanograin patches or between the layer and wall rock. CF specimens before SHS tests are composed of patches of sintered nanograins as in FM specimens and a porous gouge layer with finer nanograins (a few-20 nm in size) and angular fragments of former FM. PR specimens before SHS tests are composed of damaged wall rocks and porous gouge with finer nanograins (a few-tens of μm). After SHS tests, sintered appearance of grains within the fault zones of CF and PR indicates the increase in interparticle bonding and also in contact area by grain aggregation. In contrast, the gouge layer of FM specimens after SHS tests consists mostly of angular fragments of sintered nanograin aggregates. The angular shape of the fragments indicates little increase in bonding and contact area between the fragments. Tightly sintered nanograins in FM specimens would have a lower chemical reactivity with their size coarser and sintering stronger than those of CF and PR. Furthermore, a high wear resistance of sintered nanograins of FM would prohibit generation of fine wear debris which may have led to the strenghtened interparticle bonding. Our results imply that anti-aging friction may be a common behavior other rocks' FM too, once they are composed of tightly sintered nanograins.

Sintered bentonite ceramics for the immobilization of cesium- and strontium-bearing radioactive waste

NASA Astrophysics Data System (ADS)

Ortega, Luis Humberto

The Advanced Fuel Cycle Initiative (AFCI) is a Department of Energy (DOE) program, that has been investigating technologies to improve fuel cycle sustainability and proliferation resistance. One of the program's goals is to reduce the amount of radioactive waste requiring repository disposal. Cesium and strontium are two primary heat sources during the first 300 years of spent nuclear fuel's decay, specifically isotopes Cs-137 and Sr-90. Removal of these isotopes from spent nuclear fuel will reduce the activity of the bulk spent fuel, reducing the heat given off by the waste. Once the cesium and strontium are separated from the bulk of the spent nuclear fuel, the isotopes must be immobilized. This study is focused on a method to immobilize a cesium- and strontium-bearing radioactive liquid waste stream. While there are various schemes to remove these isotopes from spent fuel, this study has focused on a nitric acid based liquid waste. The waste liquid was mixed with the bentonite, dried then sintered. To be effective sintering temperatures from 1100 to 1200°C were required, and waste concentrations must be at least 25 wt%. The product is a leach resistant ceramic solid with the waste elements embedded within alumino-silicates and a silicon rich phase. The cesium is primarily incorporated into pollucite and the strontium into a monoclinic feldspar. The simulated waste was prepared from nitrate salts of stable ions. These ions were limited to cesium, strontium, barium and rubidium. Barium and rubidium will be co-extracted during separation due to similar chemical properties to cesium and strontium. The waste liquid was added to the bentonite clay incrementally with drying steps between each addition. The dry powder was pressed and then sintered at various temperatures. The maximum loading tested is 32 wt. percent waste, which refers to 13.9 wt. percent cesium, 12.2 wt. percent barium, 4.1 wt. percent strontium, and 2.0 wt. percent rubidium. Lower loadings of waste were also tested. The final solid product was a hard dense ceramic with a density that varied from 2.12 g/cm3 for a 19% waste loading with a 1200°C sintering temperature to 3.03 g/cm 3 with a 29% waste loading and sintered at 1100°C. Differential Scanning Calorimetry and Thermal Gravimetric Analysis (DSC-TGA) of the loaded bentonite displayed mass loss steps which were consistent with water losses in pure bentonite. Water losses were complete after dehydroxylation at ˜650°C. No mass losses were evident beyond the dehydroxylation. The ceramic melts at temperatures greater than 1300°C. Light flash analysis found heat capacities of the ceramic to be comparable to those of strontium and barium feldspars as well as pollucite. Thermal conductivity improved with higher sintering temperatures, attributed to lower porosity. Porosity was minimized in 1200°C sinterings. Ceramics with waste loadings less than 25 wt% displayed slump, the lowest waste loading, 15 wt% bloated at a 1200°C sintering. Waste loading above 25 wt% produced smooth uniform ceramics when sintered >1100°C. Sintered bentonite may provide a simple alternative to vitrification and other engineered radioactive waste-forms.

Microstructure and Mechanical Behavior of Porous Ti–6Al–4V Processed by Spherical Powder Sintering

PubMed Central

Reig, Lucía; Tojal, Concepción; Busquets, David J.; Amigó, Vicente

2013-01-01

Reducing the stiffness of titanium is an important issue to improve the behavior of this material when working together with bone, which can be achieved by generating a porous structure. The aim of this research was to analyze the porosity and mechanical behavior of Ti–6Al–4V porous samples developed by spherical powder sintering. Four different microsphere sizes were sintered at temperatures ranging from 1300 to 1400 °C for 2, 4 and 8 h. An open, interconnected porosity was obtained, with mean pore sizes ranging from 54.6 to 140 µm. The stiffness of the samples diminished by as much as 40% when compared to that of solid material and the mechanical properties were affected mainly by powder particles size. Bending strengths ranging from 48 to 320 MPa and compressive strengths from 51 to 255 MPa were obtained. PMID:28788365

Microstructure and Mechanical Behavior of Porous Ti-6Al-4V Processed by Spherical Powder Sintering.

PubMed

Reig, Lucía; Tojal, Concepción; Busquets, David J; Amigó, Vicente

2013-10-23

Reducing the stiffness of titanium is an important issue to improve the behavior of this material when working together with bone, which can be achieved by generating a porous structure. The aim of this research was to analyze the porosity and mechanical behavior of Ti-6Al-4V porous samples developed by spherical powder sintering. Four different microsphere sizes were sintered at temperatures ranging from 1300 to 1400 °C for 2, 4 and 8 h. An open, interconnected porosity was obtained, with mean pore sizes ranging from 54.6 to 140 µm. The stiffness of the samples diminished by as much as 40% when compared to that of solid material and the mechanical properties were affected mainly by powder particles size. Bending strengths ranging from 48 to 320 MPa and compressive strengths from 51 to 255 MPa were obtained.

Effect of sintering in a hydrogen atmosphere on the density and coercivity of (Sm,Zr)(Co,Cu,Fe)Z permanent magnets

NASA Astrophysics Data System (ADS)

Burkhanov, G. S.; Dormidontov, N. A.; Kolchugina, N. B.; Dormidontov, A. G.

2018-04-01

The effect of heat treatments in manufacturing (Sm,Zr)(Co,Cu,Fe)Z-based permanent magnets sintered in a hydrogen atmosphere on their properties has been studied. It was shown that the dynamics of the magnetic hardening of the studied magnets during heat treatments, in whole, corresponds to available concepts of phase transformations in five-component precipitation-hardened SmCo-based alloys. Peculiarities of the studied compositions consist in the fact that the coercive force magnitude of magnets quenched from the isothermal aging temperature is higher by an order of magnitude than those available in the literature. It was noted that, in using the selected manufacturing procedure, the increase in the density of samples does not finish at the sintering stage but continues in the course of solid-solution heat treatment.

Direct observation of grain rotations during coarsening of a semisolid Al–Cu alloy

PubMed Central

Dake, Jules M.; Oddershede, Jette; Sørensen, Henning O.; Werz, Thomas; Shatto, J. Cole; Uesugi, Kentaro; Schmidt, Søren; Krill, Carl E.

2016-01-01

Sintering is a key technology for processing ceramic and metallic powders into solid objects of complex geometry, particularly in the burgeoning field of energy storage materials. The modeling of sintering processes, however, has not kept pace with applications. Conventional models, which assume ideal arrangements of constituent powders while ignoring their underlying crystallinity, achieve at best a qualitative description of the rearrangement, densification, and coarsening of powder compacts during thermal processing. Treating a semisolid Al–Cu alloy as a model system for late-stage sintering—during which densification plays a subordinate role to coarsening—we have used 3D X-ray diffraction microscopy to track the changes in sample microstructure induced by annealing. The results establish the occurrence of significant particle rotations, driven in part by the dependence of boundary energy on crystallographic misorientation. Evidently, a comprehensive model for sintering must incorporate crystallographic parameters into the thermodynamic driving forces governing microstructural evolution. PMID:27671639

Ice sintering timescales at the surface of Europa and implications for surface properties

NASA Astrophysics Data System (ADS)

Molaro, Jamie; Phillips, Cynthia B.; Meirion-Griffith, Gareth

2017-10-01

The planned exploration of Europa by NASA’s Europa Clipper Mission and the possibility of a future Europa lander have driven the need to characterize its surface strength, roughness, porosity, thermal conductivity, and regolith depth in order to accurately interpret remote sensing data and develop appropriate spacecraft landing systems. Many processes contribute to Europa’s landscape evolution, such as sputtering, mass wasting, thermal segregation, and impact gardening, driving the creation and distribution of icy regolith across the surface. While the efficacy of these processes are not well constrained, any amount of regolith emplaced at the surface will undergo subsequent processing due to sintering. Ice sintering is a form of frost metamorphism whereby contacting ice grains experience the diffusion of material into their contact region, forming a “neck” between them and densifying over time. Over long enough timescales, ice aggregates will sinter into solid material, which may contribute to the incorporation of non-ice material into Europa’s subsurface and help to drive subsurface chemistry. Sintering also interacts with other processes, adding to the complexity of icy surface evolution. For example, sputtering preferentially removes larger grains and may enhance sintering rates, and changes in ice porosity may affect the response of the surface to micrometeorite impacts.Quantifying the effects of ice sintering will allow us to predict the microstructural properties of Europa’s surface at spacecraft scales. To this end, we have modeled pressure-less (no overburden) sintering of spherical water-ice grains and validated the results with a laboratory experiment. We also modeled ice at the surface of Europa to obtain a first-order approximation of the sintering timescale and surface properties. Preliminary results indicate that ice grains will experience neck growth but not significant densification over Europa’s surface age, suggesting that loose surface ice forms a weak and porous crust. Furthermore, our results suggest that existing models do not accurately quantify all stages of the sintering process for ice, emphasizing the need for more laboratory studies on this topic.

Oxygen-vacancy-related dielectric relaxation in SrBi2Ta1.8V0.2O9 ferroelectrics

NASA Astrophysics Data System (ADS)

Wu, Yun; Forbess, Mike J.; Seraji, Seana; Limmer, Steven J.; Chou, Tammy P.; Cao, Guozhong

2001-05-01

The strontium bismuth tantalate vanadate, SrBi2Ta1.8V0.2O9, (SBTV) layered perovskite ferroelectrics were made by solid state powder sintering. It was found that the SBTV ferroelectrics had the same crystal structure as that of strontium bismuth tantalate, SrBi2Ta2O9 (SBT), but an increased paraferroelectric transition temperature at ˜360 °C as compared to 305 °C for SBT. In addition, SBTV ferroelectrics showed a frequency dispersion at low frequencies and broadened dielectric peaks at the paraferroelectric transition temperature that shifted to a higher temperature with a reduced frequency. However, after a postsintering annealing at 850 °C in air for 60 h, SBTV ferroelectrics showed reduced dielectric constants and tangent loss, particularly at high temperatures. In addition, no frequency dependence of paraferroelectric transition was found in the annealed SBTV ferroelectrics. Furthermore, there was a significant reduction in dc conductivity with annealing. The prior results implied that the dielectric relaxation in the as-sintered SBTV ferroelectrics was most likely due to the oxygen-vacancy-related dielectric relaxation instead of relaxor ferroelectric behavior.

Transport, electronic, and structural properties of nanocrystalline CuAlO2 delafossites

NASA Astrophysics Data System (ADS)

Durá, O. J.; Boada, R.; Rivera-Calzada, A.; León, C.; Bauer, E.; de la Torre, M. A. López; Chaboy, J.

2011-01-01

This work reports on the effect of grain size on the electrical, thermal, and structural properties of CuAlO2 samples obtained by solid-state reaction combined with ball milling. Electrical characterization made in microcrystalline and nanocrystalline samples shows that the electrical conductivity decreases several orders of magnitude for the nanocrystalline samples, and, in addition, there is a large discrepancy between the activation energies associated to thermoelectric power ES. The study of the Cu K-edge x-ray absorption spectra of the CuAlO2 samples shows that the local structure around Cu is preserved after the sintering process, indicating that the observed behavior of the electrical conductivity is of intrinsic origin. Complex conductivity measurements as a function of frequency allow us to discard grain-boundaries effects on the electrical transport. Thus, the changes in σ(T) and S(T) are interpreted in terms of charge localization in the framework of small polarons. This is in agreement with the analysis of the near-edge region of the absorption spectra, which indicates that sintering favors the Cu-O hybridization. As a consequence, oxygen atoms progressively lose their capability of trapping holes, and the electrical conductivity is also enhanced.

Structure and Dielectric Properties of (Sr0.2Ca0.488Nd0.208) TiO3-Li3NbO4 Ceramic Composites

NASA Astrophysics Data System (ADS)

Xia, C. C.; Chen, G. H.

2017-12-01

The new ceramic composites of (1-x) Li3NbO4-x (Sr0.2Ca0.488Nd0.208)TiO3 were prepared by the conventional solid state reaction method. The sintering behavior, phase composition, microstructure and microwave dielectric properties of the ceramics were investigated specially. The SEM and XRD results show that (1-x) Li3NbO4-x (Sr0.2Ca0.488Nd0.208) TiO3 (0.35≤x≤0.5) composites were composed of two phase, i.e. perovskite and Li3NbO4. With the increase of x, the ɛr increases from 27.1 to 38.7, Q×f decreases from 55000 GHz to 16770 GHz, and the τ f increases from -49 ppm/°C to 226.7 ppm/°C. The optimized dielectric properties with ɛr∼31.4, Q×f~16770GHz and τf~-8.1ppm/°C could be obtained as x=0.4 sintered at 1100°C for 4h. The as-prepared ceramic is expected to be used in resonators, filters, and other microwave devices.

Effect of the powder characteristics of Sisub3Nsub4 on the microstructure of sintered bodies

NASA Technical Reports Server (NTRS)

Woetting, G.; Hausner, H.

1981-01-01

Silicon nitride powders sintered with the addition of 2 wt% Mg0 to 95% theoretical density after attrition milling and subsequent purification were evaluated. Preparation of the powders is described. The powder characteristics (specific surfaces, iron concentration, and oxygen content), and density, weight loss, and phase state of the sinter bodies as a function of powder preparation are presented.

2011 Dynamics at Surfaces Gordon Research Conference (August 7-12, 2011, Salve Regina University, Newport, Rhode Island)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Greg Sitz

2011-08-12

The 2011 Gordon Conference on Dynamics at Surfaces is the 32nd anniversary of a meeting held every two years that is attended by leading researchers in the area of experimental and theoretical dynamics at liquid and solid surfaces. The conference focuses on the dynamics of the interaction of molecules with either liquid or solid surfaces, the dynamics of the outermost layer of liquid and solid surfaces and the dynamics at the liquid-solid interface. Specific topics that are featured include state-to-state scattering dynamics, chemical reaction dynamics, non-adiabatic effects in reactive and inelastic scattering of molecules from surfaces, single molecule dynamics atmore » surfaces, surface photochemistry, ultrafast dynamics at surfaces, and dynamics at water interfaces. The conference brings together investigators from a variety of scientific disciplines including chemistry, physics, materials science, geology, biophysics, and astronomy.« less

Multilayer ceramic oxide solid electrolyte for fuel cells and electrolysis cells and method for fabrication thereof

NASA Technical Reports Server (NTRS)

Schroeder, James E. (Inventor); Anderson, Harlan U. (Inventor)

1990-01-01

An unitary layered ceramic structure is disclosed which comprises co-sintered layers. The co-sintered structure comprises a sintered central layer of yttria stabilized zirconia (YSZ) which is about 8 mole percent yttria and having a density of at least about 95% of theoretical, and sintered outer layers of strontium lanthanum manganite (LSM) having the approximate molecular composition La.sub.0.8 Sr.sub.0.2 MnO.sub.3, having a density from about 50 to about 60% of theoretical, and having interconnected porosity from about 40 to 50% with an interconnected pore diameter from about one micron to about five microns. The sintered central layer is sandwiched by and bonded and sintered to the outer layers and is essentially free of significant amounts of manganese. A process for making the unitary composition-of-matter is also disclosed which involves tape casting a LSM tape and then on top thereof casting a YSZ tape. The process comprises presintering LSM powder at 1250.degree. F., crushing the presintered commercially available LSM powder, forming a slurry with the crushed LSM, a binder and solvent, tape casting the slurry and allowing the slurry to air dry. A mixture of commercially available submicron size particle YSZ powder is milled with a dispersant and solvent to disperse the YSZ particles thereby forming a dispersed YSZ slurry. The YSZ slurry is then tape cast on the dried LSM tape. If desired, a third layer of LSM can be cast on top of the dried YSZ layer. After drying the composite LSM/YSZ and LSM/YSZ/LSM tapes are fired at 1300.degree. C. No migration of manganese into the YSZ layer was observed with scanning electron microscope/edax in the sintered multilayer tape.

Multilayer ceramic oxide solid electrolyte for fuel cells and electrolysis cells

NASA Technical Reports Server (NTRS)

Schroeder, James E. (Inventor); Anderson, Harlan U. (Inventor)

1991-01-01

A unitary layered ceramic structure is disclosed which comprises co-sintered layers. The co-sintered structure comprises a sintered central layer of yttria stabilized zirconia (YSZ) which is about 8 mole percent yttria and having a density of at least about 95% of theoretical, and sintered outer layers of strontium lanthanum manganite (LSM) having the approximate molecular composition La.sub.0.8 Sr.sub.0.2 MnO.sub.3, having a density from about 50 to about 60% of theoretical, and having interconnected porosity from about 40 to 50% with an interconnected pore diameter from about one micron to about five microns. The sintered central layer is sandwiched by and bonded and sintered to the outer layers and is essentially free of significant amounts of manganese. A process for making the unitary composition-of-matter is also disclosed which involves tape casting a LSM tape and then on top thereof casting a YSZ tape. The process comprises presintering LSM powder at 1250.degree. F., crushing the presintered commercially available LSM powder, forming a slurry with the crushed LSM, a binder and solvent, tape casting the slurry and allowing the slurry to air dry. A mixture of commercially available submicron size particle YSZ powder is milled with a dispersant and solvent to disperse the YSZ particles thereby forming a dispersed YSZ slurry. The YSZ slurry is then tape cast on the dried LSM tape. If desired, a third layer of LSM can be cast on top of the dried YSZ layer. After drying the composite LSM/YSZ and LSM/YSZ/LSM tapes are fired at 1300.degree. C. No migration of manganese into the YSZ layer was observed with scanning electron microscope/edax in the sintered multilayer tape.

Interfacial characterization in carbon nanotube reinforced aluminum matrix composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Housaer, F., E-mail: francois.housaer@ed.univ-lille1.fr; Beclin, F., E-mail: franck.beclin@univ-lille1.fr; Touzin, M., E-mail: matthieu.touzin@univ-lille1.fr

2015-12-15

In this work, the effects of the sintering parameters, such as temperature and the techniques used (HP and SPS), on CNT/Al composite interfaces are studied. The major role of the native aluminum oxide (Al{sub 2}O{sub 3}) layer covering the aluminum grains is highlighted. It is shown that, for a sintering temperature below 620 °C, the amorphous Al{sub 2}O{sub 3} layer prevents the reaction between aluminum and carbon. For greater sintering temperatures, the breaking of the oxide layer due to its crystallization leads to the formation of aluminum carbide (Al{sub 4}C{sub 3}) by reaction between aluminum and the CNT. The Al{submore » 4}C{sub 3} crystals grow perpendicularly to the matrix grain boundaries by thermally activated diffusion of the carbon atoms coming from the CNT. It is also demonstrated that, by limiting the sintering time, which is the case in SPS, it is possible to limit the growth of the Al{sub 4}C{sub 3} crystals and thus to preserve the CNT. - Highlights: • The high reactivity between CNT and Al matrix, resulting Al{sub 4}C{sub 3} formation during the sintering process is highlighted. • We demonstrate, thanks to in-situ TEM observations, that Al{sub 4}C{sub 3} crystals grow into aluminum grains by carbon diffusion. • The native aluminum oxide around the aluminum particles prevents the diffusion of carbon into the aluminum grains. • We show that the protective layer can be broken because of its crystallization, leading to the formation of Al{sub 4}C{sub 3}. • SPS, by limiting the sintering duration, is an interesting way for preparing CNT/Al composites without carbide formation.« less

Investigation on the effect of sintering temperature on kaolin hollow fibre membrane for dye filtration.

PubMed

Mohtor, Nur Hamizah; Othman, Mohd Hafiz Dzarfan; Ismail, Ahmad Fauzi; Rahman, Mukhlis A; Jaafar, Juhana; Hashim, Nur Awanis

2017-07-01

Despite its extraordinary price, ceramic membrane can still be able to surpass polymeric membrane in the applications that require high temperature and pressure conditions, as well as harsh chemical environment. In order to alleviate the high cost of ceramic material that still becomes one of the major factors that contributes to the high production cost of ceramic membrane, various attempts have been made to use low cost ceramic materials as alternatives to well-known expensive ceramic materials such as alumina, silica, and zirconia in the fabrication of ceramic membrane. Thus, local Malaysian kaolin has been chosen as the ceramic material in this study for the preparation of kaolin hollow fibre membrane since it is inexpensive and naturally abundant in Malaysia. Due to the fact that the sintering process plays a prominent role in obtaining the desired morphology, properties, and performances of prepared ceramic membrane, the aim of this work was to study the effect of different sintering temperatures applied (ranging from 1200 to 1500 °C) in the preparation of kaolin hollow fibre membrane via dry/wet phase inversion-based spinning technique and sintering process. The morphology and properties of membrane were then characterised by SEM, AFM, FTIR, XRD, and three-point bending test, while the performances of membrane were investigated by conducting water permeation and Reactive Black 5 (RB5) dye rejection tests. From the experimental results obtained, the sintering temperature of 1400 °C could be selected as the optimum sintering temperature in preparing the kaolin hollow fibre membrane with the dense sponge-like structure of separation layer that resulted in the good mechanical strength of 70 MPa with the appreciable water permeation of 75 L/h m 2  bar and RB5 rejection of 68%.

Nanoscale Solid State Batteries Enabled by Thermal Atomic Layer Deposition of a Lithium Polyphosphazene Solid State Electrolyte

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pearse, Alexander J.; Schmitt, Thomas E.; Fuller, Elliot J.

Several active areas of research in novel energy storage technologies, including three-dimensional solid state batteries and passivation coatings for reactive battery electrode components, require conformal solid state electrolytes. We describe an atomic layer deposition (ALD) process for a member of the lithium phosphorus oxynitride (LiPON) family, which is employed as a thin film lithium-conducting solid electrolyte. The reaction between lithium tert-butoxide (LiO tBu) and diethyl phosphoramidate (DEPA) produces conformal, ionically conductive thin films with a stoichiometry close to Li 2PO 2N between 250 and 300°C. The P/N ratio of the films is always 1, indicative of a particular polymorph ofmore » LiPON which closely resembles a polyphosphazene. Films grown at 300°C have an ionic conductivity of (6.51 ± 0.36)×10 -7 S/cm at 35°C, and are functionally electrochemically stable in the window from 0 to 5.3V vs. Li/Li +. We demonstrate the viability of the ALD-grown electrolyte by integrating it into full solid state batteries, including thin film devices using LiCoO 2 as the cathode and Si as the anode operating at up to 1 mA/cm 2. The high quality of the ALD growth process allows pinhole-free deposition even on rough crystalline surfaces, and we demonstrate the fabrication and operation of thin film batteries with the thinnest (<40nm) solid state electrolytes yet reported. Finally, we show an additional application of the moderate-temperature ALD process by demonstrating a flexible solid state battery fabricated on a polymer substrate.« less

Nanoscale Solid State Batteries Enabled by Thermal Atomic Layer Deposition of a Lithium Polyphosphazene Solid State Electrolyte

DOE PAGES

Pearse, Alexander J.; Schmitt, Thomas E.; Fuller, Elliot J.; ...

2017-04-10

Several active areas of research in novel energy storage technologies, including three-dimensional solid state batteries and passivation coatings for reactive battery electrode components, require conformal solid state electrolytes. We describe an atomic layer deposition (ALD) process for a member of the lithium phosphorus oxynitride (LiPON) family, which is employed as a thin film lithium-conducting solid electrolyte. The reaction between lithium tert-butoxide (LiO tBu) and diethyl phosphoramidate (DEPA) produces conformal, ionically conductive thin films with a stoichiometry close to Li 2PO 2N between 250 and 300°C. The P/N ratio of the films is always 1, indicative of a particular polymorph ofmore » LiPON which closely resembles a polyphosphazene. Films grown at 300°C have an ionic conductivity of (6.51 ± 0.36)×10 -7 S/cm at 35°C, and are functionally electrochemically stable in the window from 0 to 5.3V vs. Li/Li +. We demonstrate the viability of the ALD-grown electrolyte by integrating it into full solid state batteries, including thin film devices using LiCoO 2 as the cathode and Si as the anode operating at up to 1 mA/cm 2. The high quality of the ALD growth process allows pinhole-free deposition even on rough crystalline surfaces, and we demonstrate the fabrication and operation of thin film batteries with the thinnest (<40nm) solid state electrolytes yet reported. Finally, we show an additional application of the moderate-temperature ALD process by demonstrating a flexible solid state battery fabricated on a polymer substrate.« less

Hepatitis B reactivation and rituximab: a new boxed warning and considerations for solid organ transplantation.

PubMed

Martin, S T; Cardwell, S M; Nailor, M D; Gabardi, S

2014-04-01

Use of rituximab, a chimeric monoclonal antibody directed at the CD20 antigen, continues to increase in solid organ transplantation (SOT) for several off-label uses. In September 2013, the United States Food and Drug Administration (FDA) issued a Drug Safety Communication to oncology, rheumatology and pharmacy communities outlining a new Boxed Warning for rituximab. Citing 109 cases of fatal hepatitis B virus (HBV) reactivation in persons receiving rituximab therapy with previous or chronic HBV infection documented in their Adverse Event Reporting System (AERS), the FDA recommends screening for HBV serologies in all patients planned to receive rituximab and antiviral prophylaxis in any patient with a positive history of HBV infection. There is a lack of data pertaining to this topic in the SOT population despite an increase in off-label indications. Previous reports suggest patients receiving rituximab, on average, were administered six doses prior to HBV reactivation. Recommendations on prophylaxis, treatment and re-challenging patients with therapy after resolution of reactivation remain unclear. Based on data from the FDA AERS and multiple analyses in oncology, SOT providers utilizing rituximab should adhere to the FDA warnings and recommendations regarding HBV reactivation until further data are available in the SOT population. © Copyright 2014 The American Society of Transplantation and the American Society of Transplant Surgeons.

Electrical characterization of Mn doped-(Ba{sub 0.3}Sr{sub 0.7})Mn{sub x}(Ti{sub 0.9}Zr{sub 0.1}){sub 1-x}O{sub 3} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahmood, A.; Materials Research Laboratory, Institute of Physics & Electronics, University of Peshawar, 25120; Department of Engineering Materials, University of Sheffield, Sheffield S1 3JD

2015-12-15

Highlights: • Solid state processing of the (Ba{sub 0.3}Sr{sub 0.7})Mn{sub x}(Ti{sub 0.9}Zr{sub 0.1}){sub 1−x}O{sub 3} ceramics. • Mn incorporated on the Ti-site into the host lattice of (Ba{sub 0.3}Sr{sub 0.7})Mn{sub x}(Ti{sub 0.9}Zr{sub 0.1}){sub 1−x}O{sub 3}. • NTCR behavior was observed in the sintered samples. - Abstract: (Ba{sub 0.3}Sr{sub 0.7})Mn{sub x}(Ti{sub 0.9}Zr{sub 0.1}){sub 1-x}O{sub 3} (x = 0.00, 0.013, 0.015 and 0.05) ceramics were prepared by solid state sintering route at the 1500 °C for 6 h in air. Effect of Mn substitution on the structure of Ba{sub 0.3}Sr{sub 0.7}(Ti0{sub .9}Zr{sub 0.1}){sub 1−x}O{sub 3} perovskite was investigated systematically. Dielectric and impedancemore » spectroscopic studies were conducted to understand the electronic microstructure of the Ba{sub 0.3}Sr{sub 0.7}(Ti0{sub .9}Zr{sub 0.1}){sub 1−x}O{sub 3} ceramics. Sample with x = 0.05 showed the highest dielectric constant (ϵ{sub r} = 1826) and low dielectric loss (tanδ = 0.001) at 10 kHz, around the room temperature, while the sample with x = 0.00 showed good microwave (MW) dielectric properties (Qf{sub o} = 838 and ϵ{sub r} = 550). The impedance spectroscopic analysis confirmed the electrical homogeneity of the samples with x = 0.013, 0.015 and 0.05, where grain boundaries dominated the conduction mechanism. Similarly, the sample with x = 0.00 was found to possess both grain boundary and bulk resistive contributions.« less

A Li-Garnet composite ceramic electrolyte and its solid-state Li-S battery

NASA Astrophysics Data System (ADS)

Huang, Xiao; Liu, Cai; Lu, Yang; Xiu, Tongping; Jin, Jun; Badding, Michael E.; Wen, Zhaoyin

2018-04-01

A high strength Li-Garnet solid electrolyte composite ceramic is successfully prepared via conventional solid state method with Li6.4La3Zr1.4Ta0.6O12 and nano MgO powders. Well sintered ceramic pellets and bars are obtained with 0-9 wt.% MgO. Fracture strength is approximately 135 MPa for composite ceramics with 5-9 wt.% MgO, which is ∼50% higher than that of pure Li6.4La3Zr1.4Ta0.6O12 (90 MPa). Lithium-ion conductivity of the composite is above 5 × 10-4 S cm-1 at room temperature; comparable to the pure Li6.4La3Zr1.4Ta0.6O12 material. SEM cross-sections of the composite ceramic shows a much more uniform microstructure comparing with pure ones, owing to the grain growth inhibition effect of the MgO second phase. A battery cell consisting of Li/composite ceramics/Sulfur-Carbon at 25 °C exhibits a capacity of 685 mAh g-1 at 0.2 C at the 200th cycle, while maintaining a coulombic efficiency of 100%. These results indicate that the composite ceramic Li6.4La3Zr1.4Ta0.6O12-MgO is promising for the production of electrolyte membrane and fabrication of Li-Sulfur batteries.

Rheological changes of polyamide 12 under oscillatory shear

NASA Astrophysics Data System (ADS)

Mielicki, C.; Gronhoff, B.; Wortberg, J.

2014-05-01

Changes in material properties as well as process deviation prevent Laser Sintering (LS) technology from manufacturing of quality assured parts in a series production. In this context, the viscosity of Polyamide 12 (PA12) is assumed to possess the most significant influence, as it determines the sintering velocity, the resistance towards melt formation and the bonding strength of sintered layers. Moreover, the viscosity is directly related to the structure of the molten polymer. In particular, it has been recently reported that LS process conditions lead to structural changes of PA12 affecting viscosity and coalescence of adjacent polymer particles, i.e. melt formation significantly. Structural change of PA12 was understood as a post condensation. Its influence on viscosity was described by a time and temperature depending rheological model whereas time dependence was considered by a novel structural change shift factor which was derived from melt volume rate data. In combination with process data that was recorded using online thermal imaging, the model is suitable to control the viscosity (processability of the material) as result of material and process properties. However, as soon as laser energy is exposed to the powder bed PA12 undergoes a phase transition from solid to molten state. Above the melting point, structural change is expected to occur faster due to a higher kinetic energy and free volume of the molten polymer. Oscillatory shear results were used to study the influence of aging time and for validation of the novel structural change shift factor and its model parameters which were calibrated based on LS processing condition.

The Influence of Interstitial Ga and Interfacial Au (sub 2)P (sub 3) on the Electrical and Metallurgical Behavior of Au-Contacted III-V Semiconductors

NASA Technical Reports Server (NTRS)

Weizer, Victor G.; Fatemi, Navid S.

1991-01-01

The introduction of a very small amount of Ga into Au contact metallization on InP is shown to have a significant effect on both the metallurgical and electrical behavior of that contact system. Ga atoms in the interstices of the Au lattice are shown to be effective in preventing the solid state reactions that normally take place between Au and InP during contact sintering. In addition to suppressing the metallurgical interaction, the presence of small amounts of Ga is shown to cause an order of magnitude reduction in the specific contact resistivity. Evidence is presented that the reactions of GaP and GaAs with Au contacts are also drastically affected by the presence of Ga. The sintering behavior of the Au-GaP and the Au-GaAs systems (as contrasted with that of the Au-InP system) is explained as due to the presence of interstitial Ga in the contact metallization. Finally the large, two-to-three order of magnitude drop in the contact resistance that occurs in the Au-InP system upon sintering at 400 degrees Centigrade is shown to be a result of the formation of an Au (sub 2) P (sub 3) layer at the metal-semiconductor interface. Contact resistivities in the 10 (sup -6) ohm square centimeter range are obtained for as-deposited Au on InP when a thin (20 Angstrom) layer of Au (sub 2) P (sub 3) is introduced between the InP and the Au contacts.

Fabrication of Lead-free (K0.5Na0.5)1- x Ag x NbO3 Ferroelectric Ceramics and Their Dielectric Properties

NASA Astrophysics Data System (ADS)

Byun, Jaeduk; Hyun, June Won; Kim, Yeon Jung; Bobor, Kristóf

2018-03-01

In this study, lead-free (K0.5Na0.5)1- x Ag x NbO3 ( x = 0.00, 0.10, 0.15, 0.20, 0.25, and 0.30) ferroelectric ceramics were fabricated using solid-state synthesis without A-site and B-site manufacturing step. The (K0.5Na0.5)1- x Ag x NbO3 ceramics were sintered at 1110 °C for 4 h after calcination at 800 °C for 3 h. The sintered sample was dense, and the grain size was 1.02 7.8 μm. For x ≤ 0.2, the sintered ceramic samples had a single perovskite structure. The temperature dependence of the dielectric constant in the (K0.5Na0.5)1- x Ag x NbO3 was measured at 1 kHz using an LCR meter. The high dielectric constant properties could be obtained in (K0.5Na0.5)1- x Ag x NbO3 ceramics. The orthorhombic-to-tetragonal phase transition temperature and ferroelectric Curie temperature decreased linearly with increasing mole fraction of the Ag content. The Curie temperature shifted from 393 °C for (K0.5Na0.5)NbO3 ceramics to 317 °C for (K0.5Na0.5)0.7Ag0.3NbO3 ceramics. The maximum dielectric constant was 8930 at 330 °C in the (K0.5Na0.5)0.8Ag0.2NbO3 ceramics.

Ferroelectric and optical properties of `Ba-doped' new double perovskites

NASA Astrophysics Data System (ADS)

Parida, B. N.; Panda, Niranjan; Padhee, R.; Parida, R. K.

2018-06-01

Solid solution of Pb1.5Ba0.5BiNbO6 ceramic is explored here to obtain its ferroelectric and optical properties. The polycrystalline sample was prepared by a standard solid state reaction route. Room temperature XRD and FTIR spectra of the compound exhibit an appreciable change in its crystal structure of Pb2BiNbO6 on addition of 'Ba' in A site. The surface morphology of the gold-plated sintered pellet sample recorded by SEM exhibits a uniform distribution of small grains with well-defined grain boundaries. Detailed studies on the nature of polarization and variation of dielectric constant, tangent loss with temperature as well as frequency indicate the existence of Ferro-electricity in the sample. Using UV-Vis spectroscopy, the optical band gap of the studied sample has been estimated as 2.1 eV, which is useful for photo catalytic devices. Photoluminescence analysis of the powder sample shows a strong red photoluminescence with blue excitation, which is basically useful for LED.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sitler, Steven J.; Raja, Krishnan S.; Charit, Indrajit

Spark plasma sintered transition metal diborides such as HfB 2, ZrB 2 and their solid solutions were investigated as electrode materials for electrochemical hydrogen evolutions reactions (HER) in 1 M H 2SO 4 and 1 M NaOH electrolytes. HfB 2 and ZrB 2 formed complete solid solutions when mixed in 1:1, 1:4, and 4:1 ratios and they were stable in both electrolytes. The HER kinetics of the diborides were slower in the basic solution than in the acidic solutions. The Tafel slopes in 1 M H 2SO 4 were in the range of 0.15 - 0.18 V/decade except for puremore » HfB 2 which showed a Tafel slope of 0.38 V/decade. In 1 M NaOH the Tafel slopes were in the range of 0.12 - 0.27 V/decade. The composition of Hf xZr 1-xB 2 solid solutions with x = 0.2 - 0.8, influenced the exchange current densities, overpotentials and Tafel slopes of the HER. As a result, the EIS data were fitted with a porous film equivalent circuit model in order to better understand the HER behavior. In addition, modeling calculations, using density functional theory approach, were carried out to estimate the density of states and band structure of the boride solid solutions.« less

Laser Sintered Porous Ti-6Al-4V Implants Stimulate Vertical Bone Growth.

PubMed

Cheng, Alice; Cohen, David J; Kahn, Adrian; Clohessy, Ryan M; Sahingur, Kaan; Newton, Joseph B; Hyzy, Sharon L; Boyan, Barbara D; Schwartz, Zvi

2017-08-01

The objective of this study was to examine the ability of 3D implants with trabecular-bone-inspired porosity and micro-/nano-rough surfaces to enhance vertical bone ingrowth. Porous Ti-6Al-4V constructs were fabricated via laser-sintering and processed to obtain micro-/nano-rough surfaces. Male and female human osteoblasts were seeded on constructs to analyze cell morphology and response. Implants were then placed on rat calvaria for 10 weeks to assess vertical bone ingrowth, mechanical stability and osseointegration. All osteoblasts showed higher levels of osteocalcin, osteoprotegerin, vascular endothelial growth factor and bone morphogenetic protein 2 on porous constructs compared to solid laser-sintered controls. Porous implants placed in vivo resulted in an average of 3.1 ± 0.6 mm 3 vertical bone growth and osseointegration within implant pores and had significantly higher pull-out strength values than solid implants. New bone formation and pull-out strength was not improved with the addition of demineralized bone matrix putty. Scanning electron images and histological results corroborated vertical bone growth. This study indicates that Ti-6Al-4V implants fabricated by additive manufacturing to have porosity based on trabecular bone and post-build processing to have micro-/nano-surface roughness can support vertical bone growth in vivo, and suggests that these implants may be used clinically to increase osseointegration in challenging patient cases.

Dense garnet-like Li5La3Nb2O12 solid electrolyte prepared by self-consolidation method

NASA Astrophysics Data System (ADS)

Zhao, Pengcheng; Xiang, Yu; Xu, Yan; Wen, Yuehua; Zhang, Wenfeng; Zhu, Xiayu; Li, Meng; Zhang, Sontong; Ming, Hai; Jin, Zhaoqing; Cao, Gaoping

2018-06-01

Li5La3Nb2O12 (LLNO) is a typical garnet-like solid electrolyte with solitary cubic structure. However, its ionic conductivity is relatively low due to the low relative density when prepared by cold isostatic pressing method, which usually involves high-pressure machines, poor productivity, tedious pressing operations, and low density. In this paper, self-consolidation method is developed to sinter dense LLNO electrolyte. Although not any pressing operations are employed in the entire process, the relative density of LLNO is promoted up to 95%, which is much higher than the reported values of 45-80%. SEM images reveal that the sample is built by huge particles in size of 80 μm indicating that there are few boundaries in the sample. Moreover, a rich content of Li-Al-O compounds is detected out in the boundary areas, which may act as sintering aids for the sample to consolidate automatically. According to the highest density, the bulk ionic conductivity of LLNO sample reaches up to 1.61 × 10-4 S cm-1 at 30 °C, which is in the same order of magnitude as the value of cubic Li7La3Zr2O12 electrolyte. This work verifies the self-consolidation mechanism for the sintering of ceramic electrolytes and could significantly facilitate the development of LLNO membrane technology.

40 CFR 261.23 - Characteristic of reactivity.

Code of Federal Regulations, 2014 CFR

2014-07-01

... Section 261.23 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) IDENTIFICATION AND LISTING OF HAZARDOUS WASTE Characteristics of Hazardous Waste § 261.23 Characteristic of reactivity. (a) A solid waste exhibits the characteristic of reactivity if a representative...

40 CFR 261.23 - Characteristic of reactivity.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Section 261.23 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) IDENTIFICATION AND LISTING OF HAZARDOUS WASTE Characteristics of Hazardous Waste § 261.23 Characteristic of reactivity. (a) A solid waste exhibits the characteristic of reactivity if a representative...

40 CFR 261.23 - Characteristic of reactivity.

Code of Federal Regulations, 2011 CFR

2011-07-01

... Section 261.23 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) IDENTIFICATION AND LISTING OF HAZARDOUS WASTE Characteristics of Hazardous Waste § 261.23 Characteristic of reactivity. (a) A solid waste exhibits the characteristic of reactivity if a representative...

40 CFR 261.23 - Characteristic of reactivity.

Code of Federal Regulations, 2013 CFR

2013-07-01

... Section 261.23 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) IDENTIFICATION AND LISTING OF HAZARDOUS WASTE Characteristics of Hazardous Waste § 261.23 Characteristic of reactivity. (a) A solid waste exhibits the characteristic of reactivity if a representative...

40 CFR 261.23 - Characteristic of reactivity.

Code of Federal Regulations, 2012 CFR

2012-07-01

... Section 261.23 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) IDENTIFICATION AND LISTING OF HAZARDOUS WASTE Characteristics of Hazardous Waste § 261.23 Characteristic of reactivity. (a) A solid waste exhibits the characteristic of reactivity if a representative...

Dielectric and magnetic studies of BaTi0.5Fe0.5O3 ceramic materials, synthesized by solid state sintering.

PubMed

Samuvel, K; Ramachandran, K

2015-02-05

A comparative study of the surface morphology, dielectric and magnetic properties of the BaTi0.5Fe0.5O3 (BTFO) ceramics materials. This has been carried out by synthesizing the samples in different routes. BTFO samples have shown single phased 12R type hexagonal structure with R3m, P4mm space group. Interfacial effects on the dielectric properties of the samples have been understood by Cole-Cole plots in complex impedance and modulus formalism. It has been identified that huge dielectric constant (10(3)-10(6)) at lower frequencies is largely contributed by the heterogeneous electronic microstructure at the interfaces of grains. Modulus formalism has identified the effects of both grain and grain boundary microstructure on the dielectric properties, particularly in chemical routed samples. The order of grain boundary resistivity suggests the semiconductor/insulator class of the material. The grain boundary resistivity of the mechanical alloyed samples is remarkably lower than the solid state and chemical routed samples. Few samples have of the samples have exhibited signature of ferromagnetism at the room temperature. Copyright © 2014 Elsevier B.V. All rights reserved.

Radical-induced chemistry from VUV photolysis of interstellar ice analogues containing formaldehyde

NASA Astrophysics Data System (ADS)

Butscher, Teddy; Duvernay, Fabrice; Danger, Grégoire; Chiavassa, Thierry

2016-09-01

Surface processes and radical chemistry within interstellar ices are increasingly suspected to play an important role in the formation of complex organic molecules (COMs) observed in several astrophysical regions and cometary environments. We present new laboratory experiments on the low-temperature solid state formation of complex organic molecules - glycolaldehyde, ethylene glycol, and polyoxymethylene - through radical-induced reactivity from VUV photolysis of formaldehyde in water-free and water-dominated ices. Radical reactivity and endogenous formation of COMs were monitored in situ via infrared spectroscopy in the solid state and post photolysis with temperature programmed desorption (TPD) using a quadripole mass spectrometer. We show the ability of free radicals to be stored when formed at low temperature in water-dominated ices, and to react with other radicals or on double bonds of unsaturated molecules when the temperature increases. It experimentally confirms the role of thermal diffusion in radical reactivity. We propose a new pathway for formaldehyde polymerisation induced by HCO radicals that might explain some observations made by the Ptolemy instrument on board the Rosetta lander Philae. In addition, our results seem to indicate that H-atom additions on H2CO proceed preferentially through CH2OH intermediate radicals rather than the CH3O radical.

ZrB 2-HfB 2 solid solutions as electrode materials for hydrogen reaction in acidic and basic solutions

DOE PAGES

Sitler, Steven J.; Raja, Krishnan S.; Charit, Indrajit

2016-11-09

Spark plasma sintered transition metal diborides such as HfB 2, ZrB 2 and their solid solutions were investigated as electrode materials for electrochemical hydrogen evolutions reactions (HER) in 1 M H 2SO 4 and 1 M NaOH electrolytes. HfB 2 and ZrB 2 formed complete solid solutions when mixed in 1:1, 1:4, and 4:1 ratios and they were stable in both electrolytes. The HER kinetics of the diborides were slower in the basic solution than in the acidic solutions. The Tafel slopes in 1 M H 2SO 4 were in the range of 0.15 - 0.18 V/decade except for puremore » HfB 2 which showed a Tafel slope of 0.38 V/decade. In 1 M NaOH the Tafel slopes were in the range of 0.12 - 0.27 V/decade. The composition of Hf xZr 1-xB 2 solid solutions with x = 0.2 - 0.8, influenced the exchange current densities, overpotentials and Tafel slopes of the HER. As a result, the EIS data were fitted with a porous film equivalent circuit model in order to better understand the HER behavior. In addition, modeling calculations, using density functional theory approach, were carried out to estimate the density of states and band structure of the boride solid solutions.« less

Selective laser sintering in biomedical engineering.

PubMed

Mazzoli, Alida

2013-03-01

Selective laser sintering (SLS) is a solid freeform fabrication technique, developed by Carl Deckard for his master's thesis at the University of Texas, patented in 1989. SLS manufacturing is a technique that produces physical models through a selective solidification of a variety of fine powders. SLS technology is getting a great amount of attention in the clinical field. In this paper the characteristics features of SLS and the materials that have been developed for are reviewed together with a discussion on the principles of the above-mentioned manufacturing technique. The applications of SLS in tissue engineering, and at-large in the biomedical field, are reviewed and discussed.

In situ formation of a 3D core-shell and triple-conducting oxygen reduction reaction electrode for proton-conducting SOFCs

NASA Astrophysics Data System (ADS)

Zhang, Zhenbao; Wang, Jian; Chen, Yubo; Tan, Shaozao; Shao, Zongping; Chen, Dengjie

2018-05-01

BaZrxCeyY1-x-yO3-δ are recognized proton-conducting electrolyte materials for proton-conducting solid oxide fuel cells (H+-SOFCs) below 650 °C. Here Co cations are incorporated into the BaZr0.4Ce0.4Y0.2O3-δ (BZCY) scaffold to generate a 3D core-shell and triple-conducting (H+/O2-/e-) electrode in situ via infiltrating and reactive sintering. The core is the bulk BZCY scaffold, while the shell is composed of the cubic Ba(Zr0.4Ce0.4Y0.2)1-xCoxO3-δ, cubic spinel Co3O4 and cubic fluorite (Ce, Zr, Y)O2. The obtained electrode exhibits an excellent compatibility with the BZCY electrolyte, and performs well in yielding a low and stable polarization resistance for oxygen reduction reaction for intermediate-temperature H+-SOFCs. In particular, it achieves polarization resistances as low as 0.094 and 0.198 Ω cm2 at 650 and 600 °C in wet air (3% H2O) when the sintering temperature for the electrode is 900 °C. In addition, a symmetrical cell also exhibits operation stability of 70 h at 650 °C. Furthermore, a fuel cell assembled with the 3D core-shell and triple-conducting electrode delivers a peak power density of ∼330 mW cm-2 at 650 °C. The substantially improved electrochemical performance and high stability are ascribed to the unique core-shell structure and the formation of Ba(Zr0.4Ce0.4Y0.2)1-xCoxO3-δ in the shell.

Tribological Properties of Aluminium Alloy Composites Reinforced with Multi-Layer Graphene—The Influence of Spark Plasma Texturing Process

PubMed Central

Kostecki, Marek; Woźniak, Jarosław; Cygan, Tomasz; Petrus, Mateusz; Olszyna, Andrzej

2017-01-01

Self-lubricating composites are designed to obtain materials that reduce energy consumption, improve heat dissipation between moving bodies, and eliminate the need for external lubricants. The use of a solid lubricant in bulk composite material always involves a significant reduction in its mechanical properties, which is usually not an optimal solution. The growing interest in multilayer graphene (MLG), characterised by interesting properties as a component of composites, encouraged the authors to use it as an alternative solid lubricant in aluminium matrix composites instead of graphite. Aluminium alloy 6061 matrix composite reinforced with 2–15 vol % of MLG were synthesised by the spark plasma sintering process (SPS) and its modification, spark plasma texturing (SPT), involving deformation of the pre-sintered body in a larger diameter matrix. It was found that the application of the SPT method improves the density and hardness of the composites, resulting in improved tribological properties, particularly in the higher load regime. PMID:28796172

Hydroxyapatite scaffolds processed using a TBA-based freeze-gel casting/polymer sponge technique.

PubMed

Yang, Tae Young; Lee, Jung Min; Yoon, Seog Young; Park, Hong Chae

2010-05-01

A novel freeze-gel casting/polymer sponge technique has been introduced to fabricate porous hydroxyapatite scaffolds with controlled "designer" pore structures and improved compressive strength for bone tissue engineering applications. Tertiary-butyl alcohol (TBA) was used as a solvent in this work. The merits of each production process, freeze casting, gel casting, and polymer sponge route were characterized by the sintered microstructure and mechanical strength. A reticulated structure with large pore size of 180-360 microm, which formed on burn-out of polyurethane foam, consisted of the strut with highly interconnected, unidirectional, long pore channels (approximately 4.5 microm in dia.) by evaporation of frozen TBA produced in freeze casting together with the dense inner walls with a few, isolated fine pores (<2 microm) by gel casting. The sintered porosity and pore size generally behaved in an opposite manner to the solid loading, i.e., a high solid loading gave low porosity and small pore size, and a thickening of the strut cross section, thus leading to higher compressive strengths.

On the Role of the Electrical Field in Spark Plasma Sintering of UO2+x

PubMed Central

Tyrpekl, Vaclav; Naji, Mohamed; Holzhäuser, Michael; Freis, Daniel; Prieur, Damien; Martin, Philippe; Cremer, Bert; Murray-Farthing, Mairead; Cologna, Marco

2017-01-01

The electric field has a large effect on the stoichiometry and grain growth of UO2+x during Spark Plasma Sintering. UO2+x is gradually reduced to UO2.00 as a function of sintering temperature and time. A gradient in the oxidation state within the pellets is observed in intermediate conditions. The shape of the gradient depends unequivocally on the direction of the electrical field. The positive surface of the pellet shows a higher oxidation state compared to the negative one. An area with larger grain size is found close to the positive electrode, but not in contact with it. We interpret these findings with the redistribution of defects under an electric field, which affect the stoichiometry of UO2+x and thus the cation diffusivity. The results bear implications for understanding the electric field assisted sintering of UO2 and non-stoichiometric oxides in general. PMID:28422164

On the Role of the Electrical Field in Spark Plasma Sintering of UO2+x

NASA Astrophysics Data System (ADS)

Tyrpekl, Vaclav; Naji, Mohamed; Holzhäuser, Michael; Freis, Daniel; Prieur, Damien; Martin, Philippe; Cremer, Bert; Murray-Farthing, Mairead; Cologna, Marco

2017-04-01

The electric field has a large effect on the stoichiometry and grain growth of UO2+x during Spark Plasma Sintering. UO2+x is gradually reduced to UO2.00 as a function of sintering temperature and time. A gradient in the oxidation state within the pellets is observed in intermediate conditions. The shape of the gradient depends unequivocally on the direction of the electrical field. The positive surface of the pellet shows a higher oxidation state compared to the negative one. An area with larger grain size is found close to the positive electrode, but not in contact with it. We interpret these findings with the redistribution of defects under an electric field, which affect the stoichiometry of UO2+x and thus the cation diffusivity. The results bear implications for understanding the electric field assisted sintering of UO2 and non-stoichiometric oxides in general.

Reduction of Iron-Oxide-Carbon Composites: Part I. Estimation of the Rate Constants

NASA Astrophysics Data System (ADS)

Halder, S.; Fruehan, R. J.

2008-12-01

A new ironmaking concept using iron-oxide-carbon composite pellets has been proposed, which involves the combination of a rotary hearth furnace (RHF) and an iron bath smelter. This part of the research focuses on studying the two primary chemical kinetic steps. Efforts have been made to experimentally measure the kinetics of the carbon gasification by CO2 and wüstite reduction by CO by isolating them from the influence of heat- and mass-transport steps. A combined reaction model was used to interpret the experimental data and determine the rate constants. Results showed that the reduction is likely to be influenced by the chemical kinetics of both carbon oxidation and wüstite reduction at the temperatures of interest. Devolatilized wood-charcoal was observed to be a far more reactive form of carbon in comparison to coal-char. Sintering of the iron-oxide at the high temperatures of interest was found to exert a considerable influence on the reactivity of wüstite by virtue of altering the internal pore surface area available for the reaction. Sintering was found to be predominant for highly porous oxides and less of an influence on the denser ores. It was found using an indirect measurement technique that the rate constants for wüstite reduction were higher for the porous iron-oxide than dense hematite ore at higher temperatures (>1423 K). Such an indirect mode of measurement was used to minimize the influence of sintering of the porous oxide at these temperatures.

Valorization of lignite combustion residues and ferroalumina in the production of aggregates.

PubMed

Anagnostopoulos, I M; Stivanakis, V E; Angelopoulos, G N; Papamantellos, D C

2010-02-15

The present research study investigates the synergy of industrial solid by-products from lignite combustion (fly ash and bottom ash) and aluminum production (ferroalumina) in the production of lightweight aggregates (LWA). The process consists of two stages, pelletization and sintering. Bottom ash (BA) is used as the principal raw material in mixtures while ferroalumina (FAL) is added in lower percentages (5-30 wt%). BA carbon content is used as the fuel of sintering process in high temperatures, around 1250 degrees C, and gas generation is responsible for porous structure formation. Physical properties such as porosity, water absorption and bulk density, of sintering products are measured. Increase of FAL percentage in sintering mixtures results in decrease of porosity from 61% to 35% and of water absorption from 61% to 21% and in increase of bulk density from 1.02 g/cm(3) to 1.80 g/cm(3) of the produced aggregates. Aggregates produced by FAL addition up to 20 wt% are characterized as LWA. Aggregates formed are used in the production of concrete specimens. Compressive strength of concrete increases by increasing FAL addition in aggregates from 5 wt% to 15 wt% (highest strength value), while decrease by increasing FAL addition from 20 wt% to 30 wt%. FAL addition in lignite ashes sintering mixtures (up to 15 wt%) is considered as an important parameter for enhancing aggregates strength.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Yuxing; Yan, Pengfei; Xiao, Jie

It is widely recognized that Al plays a dual role in the fabrication of garnet-type solid electrolytes, i.e., as a dopant that stabilizes the cubic structure and a sintering aid that facilitates the densification. However, the sintering effect of Al2O3 has not been well understood so far because Al is typically “unintentionally” introduced into the sample from the crucible during the fabrication process. In this study, we have investigated the sintering effect of Al on the phase composition, microstructure, and ionic conductivity of Li6.5La3Zr1.5Ta0.5O12 by using an Al-free crucible and intentionally adding various amounts of γ-Al2O3. It was found thatmore » the densification of Li6.5La3Zr1.5Ta0.5O12 occurred via liquid-phase sintering, with evidence of morphology change among different compositions. Among all of the compositions, samples with 0.05 mol of Al per unit formula of garnet oxide (i.e., 0.3 wt% Al2O3) exhibited the optimal microstructure and the highest total ionic conductivity of 5 10-4 S cm-1 at room temperature.« less

The effect of processing parameters and solid concentration on the mechanical and microstructural properties of freeze-casted macroporous hydroxyapatite scaffolds.

PubMed

Farhangdoust, S; Zamanian, A; Yasaei, M; Khorami, M

2013-01-01

The design and fabrication of macroporous hydroxyapatite scaffolds, which could overcome current bone tissue engineering limitations, have been considered in recent years. In the current study, controlled unidirectional freeze-casting at different cooling rates was investigated. In the first step, different slurries with initial hydroxyapatite concentrations of 7-37.5 vol.% were prepared. In the next step, different cooling rates from 2 to 14 °C/min were applied to synthesize the porous scaffold. Additionally, a sintering temperature of 1350 °C was chosen as an optimum temperature. Finally, the phase composition (by XRD), microstructure (by SEM), mechanical characteristics, and the porosity of sintered samples were assessed. The porosity of the sintered samples was in a range of 45-87% and the compressive strengths varied from 0.4 MPa to 60 MPa. The mechanical strength of the scaffolds increased as a function of initial concentration, cooling rate, and sintering temperature. With regards to mechanical strength and pore size, the samples with the initial concentration and the cooling rate of 15 vol.% and 5 °C/min, respectively, showed better results. Copyright © 2012 Elsevier B.V. All rights reserved.

Stable solidification of silica-based ammonium molybdophosphate by allophane: Application to treatment of radioactive cesium in secondary solid wastes generated from fukushima.

PubMed

Wu, Yan; Lee, Chuan-Pin; Mimura, Hitoshi; Zhang, Xiaoxia; Wei, Yuezhou

2018-01-05

Silica-based ammonium molybdophosphate (AMP/SiO 2 ) is an absorbent material that can effectively remove Cs from radioactive-contaminated wastewater (RCW) generated by Fukushima nuclide accident. Pressing/sintering method was used for final disposal of secondary waste (spent absorbent) to achieve the volume reduction of AMP-Cs/SiO 2 (AMP/SiO 2 saturation adsorption of Cs) and stable solidification of Cs by adding natural allophane. The structure of AMP-Cs completely collapsed at approximately 700°C, and most Mo and P species in AMP sublimed. The optimal sintering temperature was estimated as 900°C. The stable crystalline phase of Cs 4 Al 4 Si 20 O 48 was recrystallized by the reaction of Cs 2 O, Al 2 O 3 , and SiO 2 , and the immobilization ratio of Cs was approximately 100%. The leachability of Cs from the sintered product in distilled water was approximately 0.41%. The high immobilization and low leachability of Cs were attributed to the excellent solidification properties of the sintered products of AMP-Cs/SiO 2 -allophane. Copyright © 2017 Elsevier B.V. All rights reserved.

Temperature-dependent ac conductivity and dielectric response of vanadium doped CaCu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Sen, A.; Maiti, U. N.; Thapa, R.; Chattopadhyay, K. K.

2011-09-01

Successful incorporation of vanadium dopant within the giant dielectric material CaCu 3Ti 4O12 (CCTO) through a conventional solid-state sintering process is achieved and its influence on the dielectric as well as electrical properties as a function of temperature and frequency is reported here. Proper crystalline phase formation together with dopant induced lattice constant shrinkage was confirmed through X-ray diffraction. The temperature dependence of the dielectric constant at different constant frequencies was investigated. We infer that the correlated barrier hopping (CBH) model is dominant in the conduction mechanism of the ceramic as per the temperature-dependent ac conductivity measurements. The electronic parameters such as density of the states at the Fermi level, N( E f) and hopping distance, R ω of the ceramic were also calculated using this model.

Effects of K-Doping on Thermoelectric Properties of Bi1- x K x CuOTe

NASA Astrophysics Data System (ADS)

An, Tae-Ho; Lim, Young Soo; Seo, Won-Seon; Park, Cheol-Hee; Yoo, Mi Duk; Park, Chan; Lee, Chang Hoon; Shim, Ji Hoon

2017-05-01

The effects of K-doping on the thermoelectric properties of Bi1- x K x CuOTe ( x = 0 to 0.08) have been investigated. The compounds were synthesized by a one-step solid-state reaction method and consolidated by a spark plasma sintering process. As the amount of K-doping was increased, the electrical and thermal conductivities increased while the Seebeck coefficient decreased due to increasing hole concentration. A ZT value of 0.69 was obtained for the compound K0.01Bi0.99CuOTe at 700 K, to the best of our knowledge the highest value reported for this material system. The origin of this enhanced ZT is discussed in terms of the density of states effective mass estimated by a single parabolic band model and electronic structures calculated based on density functional theory.

The Scripps Research Institute (La Jolla, CA)

DOEpatents

Schultz, Peter G.; Wang, Lei

2010-01-05

The invention provides proteins attached to solid supports, and methods of preparing such solid support-bound proteins are provided. The proteins are attached to solid supports by means of an unnatural amino acid incorporated into the protein, which unnatural amino acid includes a reactive group that can react with a second reactive group that is attached to a solid support.

Study on structural, dielectric, ferroelectric and piezoelectric properties of Ba doped Lead Zirconate Titanate Ceramics

NASA Astrophysics Data System (ADS)

Dipti; Juneja, J. K.; Singh, Sangeeta; Raina, K. K.; Prakash, Chandra

2013-12-01

The perovskite Pb(1-x)BaxZr0.55Ti0.45O3 material (x=0.00, 0.01, 0.02, 0.03, 0.05, and 0.07) was synthesized by solid state reaction route. Green bodies were sintered at 1250 °C. All samples were subjected to X-ray diffraction analysis and they were found to be in single phase. Dielectric properties were studied as a function of temperature and frequency. Ferroelectric properties were studied as a function of temperature. Remnant polarization, saturation polarization and coercive field were determined for all the samples using ferroelectric loops. Piezoelectric properties such as d33 and electromechanical coupling factor (kp) were also measured at room temperature for all samples.

The effect of temperature on ferroelectric properties of CaCu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Kumar, Sandeep; Ahlawat, Neetu; Punia, Suman

2014-04-01

CaCu3Ti4O12 (CCTO) ceramic was synthesized by conventional solid-state reaction technique and sintered at 1353K for 10 hours. The dielectric properties of CCTO were analyzed in 1Hz-5 MHz frequency range, from room temperature to 413K. The ferroelectric properties of CCTO were analyzed at various frequencies viz. 50 Hz, 100 Hz and 200 Hz at temperatures (298K to 413K). Result of these investigation points that with increasing temperature the values of coercive field (Ec) and remnant polarization (Pr) decrease while maximum polarization (Pmax) increases non-linearly. P-E hysteresis loop of CCTO goes to slimed and a ferroelectric to Para-electric phase transition is observed at 403K.

Structural Integration of Silicon Solar Cells and Lithium-ion Batteries Using Printed Electronics

NASA Astrophysics Data System (ADS)

Kang, Jin Sung

Inkjet printing of electrode using copper nanoparticle ink is presented. Electrode was printed on a flexible glass epoxy composite substrate using drop on demand piezoelectric dispenser and was sintered at 200°C in N 2 gas condition. The printed electrodes were made with various widths and thicknesses. Surface morphology of electrode was analyzed using scanning electron microscope (SEM) and atomic force microscope (AFM). Reliable dimensions for printed electronics were found from this study. Single-crystalline silicon solar cells were tested under four-point bending to find the feasibility of directly integrating them onto a carbon fiber/epoxy composite laminate. These solar cells were not able to withstand 0.2% strain. On the other hand, thin-film amorphous silicon solar cells were subjected to flexural fatigue loadings. The current density-voltage curves were analyzed at different cycles, and there was no noticeable degradation on its performance up to 100 cycles. A multifunctional composite laminate which can harvest and store solar energy was fabricated using printed electrodes. The integrated printed circuit board (PCB) was co-cured with a carbon/epoxy composite laminate by the vacuum bag molding process in an autoclave; an amorphous silicon solar cell and a thin-film solid state lithium-ion (Li-ion) battery were adhesively joined and electrically connected to a thin flexible PCB; and then the passive components such as resistors and diodes were electrically connected to the printed circuit board by silver pasting. Since a thin-film solid state Li-ion battery was not able to withstand tensile strain above 0.4%, thin Li-ion polymer batteries were tested under various mechanical loadings and environmental conditions to find the feasibility of using the polymer batteries for our multifunctional purpose. It was found that the Li-ion polymer batteries were stable under pressure and tensile loading without any noticeable degradation on its charge and discharge performances. Also, the active materials did not decompose at 80°C, and the battery was performing well under low temperature of -27°C. Lastly, the batteries were embedded inside a carbon fiber/epoxy composite laminate to characterize their performance under fatigue loading. Finally, an intense pulsed light (IPL) was used to sinter printed silver nanoink patterns. X-ray diffraction (XRD) was used to find grain size of printed silver nanoink patterns. From these analyses it was confirmed that IPL is able to adequately sinter silver nanoink patterns for printed electronics without degradation of the substrates in less than 30 ms.

Compression selective solid-state chemistry

NASA Astrophysics Data System (ADS)

Hu, Anguang

Compression selective solid-state chemistry refers to mechanically induced selective reactions of solids under thermomechanical extreme conditions. Advanced quantum solid-state chemistry simulations, based on density functional theory with localized basis functions, were performed to provide a remarkable insight into bonding pathways of high-pressure chemical reactions in all agreement with experiments. These pathways clearly demonstrate reaction mechanisms in unprecedented structural details, showing not only the chemical identity of reactive intermediates but also how atoms move along the reaction coordinate associated with a specific vibrational mode, directed by induced chemical stress occurred during bond breaking and forming. It indicates that chemical bonds in solids can break and form precisely under compression as we wish. This can be realized through strongly coupling of mechanical work to an initiation vibrational mode when all other modes can be suppressed under compression, resulting in ultrafast reactions to take place isothermally in a few femtoseconds. Thermodynamically, such reactions correspond to an entropy minimum process on an isotherm where the compression can force thermal expansion coefficient equal to zero. Combining a significantly brief reaction process with specific mode selectivity, both statistical laws and quantum uncertainty principle can be bypassed to precisely break chemical bonds, establishing fundamental principles of compression selective solid-state chemistry. Naturally this leads to understand the ''alchemy'' to purify, grow, and perfect certain materials such as emerging novel disruptive energetics.

Dielectric Properties of Sol-Gel Derived Barium Strontium Titanate and Microwave Sintering of Ceramics

NASA Astrophysics Data System (ADS)

Selmi, Fathi A.

This thesis consists of two areas of research: (1) sol-gel processing of Ba_{rm 1-x}Sr_{rm x} TiO_3 ceramics and their dielectric properties measurement; and (2) microwave versus conventional sintering of ceramics such as Al_2 O_3, Ba_{ rm 1-x}Sr_{rm x}TiO_3, Sb-doped SnO _2 and YBa_2Cu _3O_7. Sol-gel powders of BaTiO_3, SrTiO_3, and their solid solutions were synthesized by the hydrolysis of titanium isopropoxide and Ba and Sr methoxyethoxides. The loss tangent and dielectric constant of both sol-gel and conventionally prepared and sintered Ba_{rm 1-x}Sr _{rm x}TiO _3 ceramics were investigated at high frequencies. The sol-gel prepared ceramics showed higher dielectric constant and lower loss compared to those prepared conventionally. Ba _{rm 1-x}Sr _{rm x}TiO_3 ceramics were tunable with applied bias, indicating the potential use of this material for phase shifter applications. Porous Ba_{0.65}Sr _{0.35}TiO_3 was also investigated to lower the dielectric constant. Microwave sintering of alpha -Al_2O_3 and SrTiO_3 was investigated using an ordinary kitchen microwave oven (2.45 GHz; 600 Watts). The use of microwaves with good insulation of alpha -Al_2O_3 and SrTiO_3 samples resulted in their rapid sintering with good final densities of 96 and 98% of the theoretical density, respectively. A comparison of grain size for conventionally and microwave sintered SrTiO_3 samples did not show a noticeable difference. However, the grain size of microwave sintered alpha-Al_2O _3 was found to be larger than that of conventionally sintered sample. These results show that rapid sintering of ceramics can be achieved by using microwave radiation. The sintering behavior of coprecipitated Sb-doped SnO_2 was investigated using microwave power absorption. With microwave power, samples were sintered at 1450^circC for 20 minutes and showed a density as high as 99.9% of theoretical. However, samples fired in a conventional electric furnace at the same temperature for 4 hours showed only 60% of theoretical density. Microwave sintering also led to improvement in terms of uniform structure and electrical properties. Ba_{0.65}Sr _{0.35}TiO_3 was sintered using the microwave power at 1300 ^circC for 10 minutes. A density of 99% was achieved with small and uniform grain size. Superconducting powders have been successfully prepared by the sol-gel process and sintered and annealed using microwave power. Sintering and densification was achieved in a shorter time with microwave heating than with conventional heating and microwave heating appears to result in refined microstructure.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brozek, Eric M. ..; Washton, Nancy M.; Mueller, Karl T.

A series of silsesquioxane nanoparticles containing reactive internal organic functionalities throughout the entire particle body have been synthesized using a surfactant-free method with organosilanes as the sole precursors and a base catalyst. The organic functional groups incorporated are vinyl, allyl, mercapto, cyanoethyl, and cyanopropyl groups. The sizes and morphologies of the particles were characterized using SEM and nitrogen adsorption, while the compositions were confirmed using TGA, FT-IR, solid state NMR, and elemental analysis. The accessibility and reactivity of the functional groups inside the particles were demonstrated by performing bromination and reduction reactions in the interior of the particles.

Synthesis and sintering of UN-UO2 fuel composites

NASA Astrophysics Data System (ADS)

Jaques, Brian J.; Watkins, Jennifer; Croteau, Joseph R.; Alanko, Gordon A.; Tyburska-Püschel, Beata; Meyer, Mitch; Xu, Peng; Lahoda, Edward J.; Butt, Darryl P.

2015-11-01

The design and development of an economical, accident tolerant fuel (ATF) for use in the current light water reactor (LWR) fleet is highly desirable for the future of nuclear power. Uranium mononitride has been identified as an alternative fuel with higher uranium density and thermal conductivity when compared to the benchmark, UO2, which could also provide significant economic benefits. However, UN by itself reacts with water at reactor operating temperatures. In order to reduce its reactivity, the addition of UO2 to UN has been suggested. In order to avoid carbon impurities, UN was synthesized from elemental uranium using a hydride-dehydride-nitride thermal synthesis route prior to mixing with up to 10 wt% UO2 in a planetary ball mill. UN and UN - UO2 composite pellets were sintered in Ar - (0-1 at%) N2 to study the effects of nitrogen concentration on the evolved phases and microstructure. UN and UN-UO2 composite pellets were also sintered in Ar - 100 ppm N2 to assess the effects of temperature (1700-2000 °C) on the final grain morphology and phase concentration.

Evolving microstructure, magnetic properties and phase transition in a mechanically alloyed Ni0.5Zn0.5Fe2O4 single sample

NASA Astrophysics Data System (ADS)

Ismail, Ismayadi; Hashim, Mansor; Kanagesan, Samikannu; Ibrahim, Idza Riati; Nazlan, Rodziah; Wan Ab Rahman, Wan Norailiana; Abdullah, Nor Hapishah; Mohd Idris, Fadzidah; Bahmanrokh, Ghazaleh; Shafie, Mohd Shamsul Ezzad; Manap, Masni

2014-02-01

We report on an investigation to unravel the dependence of magnetic properties on microstructure while they evolve in parallel under the influence of sintering temperature of a single sample of Ni0.5Zn0.5Fe2O4 synthesized via mechanical alloying. A single sample, instead of the normally practiced approach of using multiple samples, was sintered at various sintering temperatures from 500 °C to 1400 °C. The morphology of the samples was studied by means of scanning electron microscopy (SEM) equipped with EDX; density measurement was conducted using the Archimedes principle; and hysteresis measurement was carried out using a B-H hysteresisgraph system. XRD data showed that the first appearance of a single phase was at 800 °C and an amorphous phase was traced at lower sintering temperatures. We correlated the microstructure and the magnetic properties and showed that the important grain-size threshold for the appearance of significant ordered magnetism (mainly ferromagnetism) was about ≥0.3 µm. We found that there were three stages of magnetic phase evolution produced via the sintering process with increasing temperatures. The first stage was dominated by paramagnetic states with some superparamagnetic behavior; the second stage was influenced by moderately ferromagnetic states and some paramagnetic states; and the third stage consisted of strongly ferromagnetic states with negligible paramagnetic states. We found that three factors sensitively influenced the sample's content of ordered magnetism—the ferrite-phase crystallinity degree, the number of grains above the critical grain size and the number of large enough grains for domain wall accommodation.

77 FR 16679 - Emergency Planning and Notification; Emergency Planning and List of Extremely Hazardous...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-03-22

...The U.S. Environmental Protection Agency (EPA or the Agency) is taking final action to revise the manner for applying the threshold planning quantities (TPQs) for those extremely hazardous substances (EHSs) that are non-reactive solid chemicals in solution. This revision allows facilities subject to the Emergency Planning requirements that have a non-reactive solid EHS in solution, to first multiply the amount of the solid chemical in solution on-site by 0.2 before determining if this quantity equals or exceeds the lower published TPQ. This change is based on data that shows less potential for non-reactive solid chemicals in solution to remain airborne and dispersed beyond a facility's fence line in the event of an accidental release. Previously, EPA assumed that 100% of non-reactive solid chemicals in solution could become airborne and dispersed beyond the fenceline in the event of an accidental release.

Study, selection, and preparation of solid cationic conductors

NASA Technical Reports Server (NTRS)

Roth, W. L.; Mitoff, S. P.; King, R. N.

1972-01-01

Crystal chemical principles and transport theory were used to predict structures and specific compounds which might find application as solid electrolytes in rechargeable high energy and high power density batteries operating at temperatures less than 200 C. More than twenty compounds were synthesized or obtained and screened by nuclear magnetic resonance and conductivity. Many were densified by sintering or hot pressing. Encouraging results were obtained for nine of these materials but none have yet been good ionic conductors at low temperature.

Method to fabricate high performance tubular solid oxide fuel cells

DOEpatents

Chen, Fanglin; Yang, Chenghao; Jin, Chao

2013-06-18

In accordance with the present disclosure, a method for fabricating a solid oxide fuel cell is described. The method includes forming an asymmetric porous ceramic tube by using a phase inversion process. The method further includes forming an asymmetric porous ceramic layer on a surface of the asymmetric porous ceramic tube by using a phase inversion process. The tube is co-sintered to form a structure having a first porous layer, a second porous layer, and a dense layer positioned therebetween.

In situ solid-state electrochemistry of mass-selected ions at well-defined electrode–electrolyte interfaces

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prabhakaran, Venkateshkumar; Johnson, Grant E.; Wang, Bingbing

2016-11-07

Molecular-level understanding of electrochemical processes occurring at electrode-electrolyte interfaces (EEI) is key to the rational development of high-performance and sustainable electrochemical technologies. This article reports the development and first application of solid-state in situ electrochemical probes to study redox and catalytic processes occurring at well-defined EEI generated using soft-landing of mass- and charge-selected cluster ions (SL). In situ electrochemical probes with excellent mass transfer properties are fabricated using carefully-designed nanoporous ionic liquid membranes. SL enables deposition of pure active species that are not obtainable with other techniques onto electrode surfaces with precise control over charge state, composition, and kinetic energy.more » SL is, therefore, a unique tool for studying fundamental processes occurring at EEI. For the first time using an aprotic electrochemical probe, the effect of charge state (PMo12O403-/2-) and the contribution of building blocks of Keggin polyoxometalate (POM) clusters to redox processes are characterized by populating EEI with novel POM anions generated by electrospray ionization and gas phase dissociation. Additionally, a proton conducting electrochemical probe has been developed to characterize the reactive electrochemistry (oxygen reduction activity) of bare Pt clusters (Pt40 ~1 nm diameter), thus demonstrating the capability of the probe for studying reactions in controlled gaseous environments. The newly developed in situ electrochemical probes combined with ion SL provide a versatile method to characterize the EEI in solid-state redox systems and reactive electrochemistry at precisely-defined conditions. This capability will advance molecular-level understanding of processes occurring at EEI that are critical to many energy-related technologies.« less

Local structure in solid solutions of stabilised zirconia with actinide dioxides (UO{sub 2}, NpO{sub 2})

DOE Office of Scientific and Technical Information (OSTI.GOV)

Walter, Marcus, E-mail: marcus.walter@vkta.d; Somers, Joseph; Bouexiere, Daniel

2011-04-15

The local structure of (Zr,Lu,U)O{sub 2-x} and (Zr,Y,Np)O{sub 2-x} solid solutions has been investigated by extended X-ray absorption fine structure (EXAFS). Samples were prepared by mixing reactive (Zr,Lu)O{sub 2-x} and (Zr,Y)O{sub 2-x} precursor materials with the actinide oxide powders, respectively. Sintering at 1600 {sup o}C in Ar/H{sub 2} yields a fluorite structure with U(IV) and Np(IV). As typical for stabilised zirconia the metal-oxygen and metal-metal distances are characteristic for the different metal ions. The bond lengths increase with actinide concentration, whereas highest adaptation to the bulk stabilised zirconia structure was observed for U---O and Np---O bonds. The Zr---O bond showsmore » only a slight increase from 2.14 A at 6 mol% actinide to 2.18 A at infinite dilution in UO{sub 2} and NpO{sub 2}. The short interatomic distance between Zr and the surrounding oxygen and metal atoms indicate a low relaxation of Zr with respect to the bulk structure, i.e. a strong Pauling behaviour. -- Graphical abstract: Metal-oxygen bond distances in (Zr,Lu,U)O{sub 2-x} solid solutions with different oxygen vacancy concentrations (Lu/Zr=1 and Lu/Zr=0.5). Display Omitted Research Highlights: {yields} EXAFS indicates high U and Np adaption to the bulk structure of stabilised zirconia. {yields} Zr---O bond length is 2.18 A at infinite Zr dilution in UO{sub 2} and NpO{sub 2}. {yields} Low relaxation (strong Pauling behaviour) of Zr explains its low solubility in UO{sub 2}.« less

Combining reactive sputtering and rapid thermal processing for synthesis and discovery of metal oxynitrides

DOE PAGES

Zhou, Lan; Suram, Santosh K.; Becerra-Stasiewicz, Natalie; ...

2015-05-27

Recent efforts have demonstrated enhanced tailoring of material functionality with mixed-anion materials, yet exploratory research with mixed-anion chemistries is limited by the sensitivity of these materials to synthesis conditions. In order to synthesize a particular metal oxynitride compound by traditional reactive annealing we require specific, limited ranges of both oxygen and nitrogen chemical potentials in order to establish equilibrium between the solid-state material and a reactive atmosphere. While using Ta-O-N as an example system, we describe a combination of reactive sputter deposition and rapid thermal processing for synthesis of mixed-anion inorganic materials. Heuristic optimization of reactive gas pressures to attainmore » a desired anion stoichiometry is discussed, and the ability of rapid thermal processing to enable amorphous to crystalline transitions without preferential anion loss is demonstrated through the controlled synthesis of nitride, oxide and oxynitride phases.« less

Mechanochemical Synthesis of Two Polymorphs of the Tetrathiafulvalene-Chloranil Charge Transfer Salt: An Experiment for Organic Chemistry

ERIC Educational Resources Information Center

Wixtrom, Alex; Buhler, Jessica; Abdel-Fattah, Tarek

2014-01-01

Mechanochemical syntheses avoid or considerably reduce the use of reaction solvents, thus providing green chemistry synthetic alternatives that are both environmentally friendly and economically advantageous. The increased solid-state reactivity generated by mechanical energy imparted to the reactants by grinding or milling can offer alternative…

Precise non-steady-state characterization of solid active materials with no preliminary mechanistic assumptions

DOE PAGES

Constales, Denis; Yablonsky, Gregory S.; Wang, Lucun; ...

2017-04-25

This paper presents a straightforward and user-friendly procedure for extracting a reactivity characterization of catalytic reactions on solid materials under non-steady-state conditions, particularly in temporal analysis of products (TAP) experiments. The kinetic parameters derived by this procedure can help with the development of detailed mechanistic understanding. The procedure consists of the following two major steps: 1) Three “Laplace reactivities” are first determined based on the moments of the exit flow pulse response data; 2) Depending on a select kinetic model, kinetic constants of elementary reaction steps can then be expressed as a function of reactivities and determined accordingly. In particular,more » we distinguish two calculation methods based on the availability and reliability of reactant and product data. The theoretical results are illustrated using a reverse example with given parameters as well as an experimental example of CO oxidation over a supported Au/SiO 2 catalyst. The procedure presented here provides an efficient tool for kinetic characterization of many complex chemical reactions.« less

Air-stable nZVI formation mediated by glutamic acid: solid-state storable material exhibiting 2D chain morphology and high reactivity in aqueous environment

NASA Astrophysics Data System (ADS)

Siskova, Karolina; Tucek, Jiri; Machala, Libor; Otyepkova, Eva; Filip, Jan; Safarova, Klara; Pechousek, Jiri; Zboril, Radek

2012-03-01

We report a new chemical approach toward air-stable nanoscale zero-valent iron (nZVI). The uniformly sized (approx. 80 nm) particles, formed by the reduction of Fe(II) salt by borohydride in the presence of glutamic acid, are coated by a thin inner shell of amorphous ferric oxide/hydroxide and a secondary shell consisting of glutamic acid. The as-prepared nanoparticles stabilized by the inorganic-organic double shell create 2D chain morphologies. They are storable for several months under ambient atmosphere without the loss of Fe(0) relative content. They show one order of magnitude higher rate constant for trichlorethene decomposition compared with the pristine particles possessing only the inorganic shell as a protective layer. This is the first example of the inorganic-organic (consisting of low-molecular weight species) double-shell stabilized nanoscale zero-valent iron material being safely transportable in solid-state, storable on long-term basis under ambient conditions, environmentally acceptable for in situ applications, and extraordinarily reactive if contacted with reducible pollutants, all in one.

Chemical Passivation of Li(exp +)-Conducting Solid Electrolytes

NASA Technical Reports Server (NTRS)

West, William; Whitacre, Jay; Lim, James

2008-01-01

Plates of a solid electrolyte that exhibits high conductivity for positive lithium ions can now be passivated to prevent them from reacting with metallic lithium. Such passivation could enable the construction and operation of high-performance, long-life lithium-based rechargeable electrochemical cells containing metallic lithium anodes. The advantage of this approach, in comparison with a possible alternative approach utilizing lithium-ion graphitic anodes, is that metallic lithium anodes could afford significantly greater energy-storage densities. A major impediment to the development of such cells has been the fact that the available solid electrolytes having the requisite high Li(exp +)-ion conductivity are too highly chemically reactive with metallic lithium to be useful, while those solid electrolytes that do not react excessively with metallic lithium have conductivities too low to be useful. The present passivation method exploits the best features of both extremes of the solid-electrolyte spectrum. The basic idea is to coat a higher-conductivity, higher-reactivity solid electrolyte with a lower-conductivity, lower-reactivity solid electrolyte. One can then safely deposit metallic lithium in contact with the lower-reactivity solid electrolyte without incurring the undesired chemical reactions. The thickness of the lower-reactivity electrolyte must be great enough to afford the desired passivation but not so great as to contribute excessively to the electrical resistance of the cell. The feasibility of this method was demonstrated in experiments on plates of a commercial high-performance solid Li(exp +)- conducting electrolyte. Lithium phosphorous oxynitride (LiPON) was the solid electrolyte used for passivation. LiPON-coated solid-electrolyte plates were found to support electrochemical plating and stripping of Li metal. The electrical resistance contributed by the LiPON layers were found to be small relative to overall cell impedances.

Lead-free Bi(Mg0.5Ti0.5)O3-modified 0.875Bi0.5Na0.5TiO3-0.125BaTiO3 ferroelectric ceramics with tetragonal structure and large field-induced strains

NASA Astrophysics Data System (ADS)

Li, Ling; Zhu, Mankang; Ren, Xiaowei; Wei, Qiumei; Zheng, Mupeng; Hou, Yudong

2017-12-01

A electrostrictive ceramics were designed by introducing Bi(Mg0.5Ti0.5)O3 into 0.875Bi0.5Na0.5TiO3-0.125BaTiO3 with tetragonal structure. All the specimens prepared by a conventional solid sintering technique exhibit the excellent sintering ability with a high relative density over 97%. It is found that, as BMT added, the specimens undergo a structure crossover from ferroelectric P4mm to ergodic P4bm, and the coexistence of both tetragonal structures takes bridge between them. A large field-induced strain of 0.30% and field-independent strain coefficient of 0.0254 m4/C2 occur at 4 mol.% BMT added. This material with excellent sinterability is suitable for the application in actuators and microposition controllers.

SPS-RS technique for solid-phase “in situ” synthesis of biocompatible ZrO2 porous ceramics

NASA Astrophysics Data System (ADS)

Shichalin, O. O.; Medkov, M. A.; Grishchenko, D. N.; Mayorov, V. Yu; Fedorets, A. N.; Belov, A. A.; Golub, A. V.; Gridasova, E. A.; Papynov, E. K.

2018-02-01

The prospective method of spark plasma sintering-reaction synthesis (SPS-RS) for fabrication of ceramics based on ZrO2 and biocompatible with living tissue is presented. Nanostructured ceramics has high mechanical strength (more than 400 MPa) and controlled porosity depending on specified sintering conditions. Biocompatible phases Ca10(PO4)6(OH)2 are formed “in situ” during SPS sintering of ZrO2 powder due to chemical interaction of phosphate precursors preliminary introduced into the mixture. The effective method to improve (to develop) porous structure of bioceramics obtained by SPS or SPS-RS techniques using poreforming agent (carbon black) is proposed. Suggested original SPS-RS “in situ” technique provides fabrication of new ZrO2 ceramics containing biocompatible phosphate components and possessing unique structural and mechanical characteristics. Such ceramics is indispensable for bone-ceramic implants that are able to activate processes of osteogenesis during bone tissue recovery.

Prediction of La0.6Sr0.4Co0.2Fe0.8O3 cathode microstructures during sintering: Kinetic Monte Carlo (KMC) simulations calibrated by artificial neural networks

NASA Astrophysics Data System (ADS)

Yan, Zilin; Kim, Yongtae; Hara, Shotaro; Shikazono, Naoki

2017-04-01

The Potts Kinetic Monte Carlo (KMC) model, proven to be a robust tool to study all stages of sintering process, is an ideal tool to analyze the microstructure evolution of electrodes in solid oxide fuel cells (SOFCs). Due to the nature of this model, the input parameters of KMC simulations such as simulation temperatures and attempt frequencies are difficult to identify. We propose a rigorous and efficient approach to facilitate the input parameter calibration process using artificial neural networks (ANNs). The trained ANN reduces drastically the number of trial-and-error of KMC simulations. The KMC simulation using the calibrated input parameters predicts the microstructures of a La0.6Sr0.4Co0.2Fe0.8O3 cathode material during sintering, showing both qualitative and quantitative congruence with real 3D microstructures obtained by focused ion beam scanning electron microscopy (FIB-SEM) reconstruction.

High-pressure melting curve of hydrogen.

PubMed

Davis, Sergio M; Belonoshko, Anatoly B; Johansson, Börje; Skorodumova, Natalia V; van Duin, Adri C T

2008-11-21

The melting curve of hydrogen was computed for pressures up to 200 GPa, using molecular dynamics. The inter- and intramolecular interactions were described by the reactive force field (ReaxFF) model. The model describes the pressure-volume equation of state solid hydrogen in good agreement with experiment up to pressures over 150 GPa, however the corresponding equation of state for liquid deviates considerably from density functional theory calculations. Due to this, the computed melting curve, although shares most of the known features, yields considerably lower melting temperatures compared to extrapolations of the available diamond anvil cell data. This failure of the ReaxFF model, which can reproduce many physical and chemical properties (including chemical reactions in hydrocarbons) of solid hydrogen, hints at an important change in the mechanism of interaction of hydrogen molecules in the liquid state.

Method and apparatus for making articles from particle based materials

DOEpatents

Moorhead, Arthur J.; Menchhofer, Paul A.

1995-01-01

A method and apparatus for the production of articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with the invention, a thermally settable slurry containing a relatively high concentration of the particles is conveyed through an elongate flow area having a desired cross-sectional configuration. The slurry is heated as it is advanced through the flow area causing the slurry to set or harden in a shape which conforms to the cross-sectional configuration of the flow area. The material discharges from the flow area as a self-supporting solid of near net final dimensions. The article may then be sintered to consolidate the particles and provide a high density product.

Microstructure and mechanical properties of NiCoCrAlYTa alloy processed by press and sintering route

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pereira, J.C., E-mail: jpereira@uc.edu.ve; Centro de Investigaciones en Mecánica, Facultad de Ingeniería, Universidad de Carabobo; Zambrano, J.C.

2015-03-15

Nickel-based superalloys such as NiCoCrAlY are widely used in high-temperature applications, such as gas turbine components in the energy and aerospace industries, due to their strength, high elastic modulus, and high-temperature oxidation resistance. However, the processing of these alloys is complex and costly, and the alloys are currently used as a bond coat in thermal barrier coatings. In this work, the effect of cold press and sintering processing parameters on the microstructure and mechanical properties of NiCoCrAlY alloy were studied using the powder metallurgy route as a new way to obtain NiCoCrAlYTa samples from a gas atomized prealloyed powder feedstock.more » High mechanical strength and adequate densification up to 98% were achieved. The most suitable compaction pressure and sintering temperature were determined for NiCoCrAlYTa alloy through microstructure characterization. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and energy dispersive spectroscopy microanalysis (EDS) were performed to confirm the expected γ-Ni matrix and β-NiAl phase distribution. Additionally, the results demonstrated the unexpected presence of carbides and Ni–Y-rich zones in the microstructure due to the powder metallurgy processing parameters used. Thus, microhardness, nanoindentation and uniaxial compression tests were conducted to correlate the microstructure of the alloy samples with their mechanical properties under the different studied conditions. The results show that the compaction pressure did not significantly affect the mechanical properties of the alloy samples. In this work, the compaction pressures of 400, 700 and 1000 MPa were used. The sintering temperature of 1200 °C for NiCoCrAlYTa alloy was preferred; above this temperature, the improvement in mechanical properties is not significant due to grain coarsening, whereas a lower temperature produces a decrease in mechanical properties due to high porosity and poor solid-state diffusion. - Graphical abstract: Display Omitted - Highlights: • We made NiCoCrAlYTa alloy by a conventional powder metallurgy route. • High densification and adequate strength were observed. • The presence of unexpected carbides found along γ/γ and γ/β grain boundaries was detected. • The effect of cold press and sintering processing parameters on the microstructure and mechanical properties were studied.« less

Effect of Silver Flakes in Silver Paste on the Joining Process and Properties of Sandwich Power Modules (IGBTs Chip/Silver Paste/Bare Cu)

NASA Astrophysics Data System (ADS)

Zhao, Su-Yan; Li, Xin; Mei, Yun-Hui; Lu, Guo-Quan

2016-11-01

In this study, a silver paste has been introduced for attaching chips onto bare Cu substrates (without coating) without applying pressure. Small nano-thickness Ag flakes, measuring 1 μm-5 μm length, were embedded uniformly in Ag nanoparticles for improving the density of the material. The presence of silver flakes in the silver paste affected the joining process and its microstructure. Microstructure characterization revealed that densification of the silver layer was affected by the presence of silver flakes as the flakes coarsened and formed reactive in situ nanoparticles, which facilitated the sintering between the flakes and the incorporated nanoparticles. Coarsening of silver flakes depended on the sintering temperature, time, and the atmosphere, which affected the decomposition and burning out of organics presented on the surface of the flakes. A high-density silver layer was obtained due to the presence of compact silver flakes. With an increase in the microstructure density, a higher bonding strength and a lower thermal impedance of the sintered joints were achieved. On performing pressureless sintering at 270°C for 30 min under 99.99% N2 or 4% H2/N2, the bonding strength and thermal impedance for 11 × 11 mm2 chips were excellent, measuring approximately 21.9 MPa and 0.077°C/W, respectively.

Feed gas contaminant removal in ion transport membrane systems

DOEpatents

Underwood, Richard Paul [Allentown, PA; Makitka, III, Alexander; Carolan, Michael Francis [Allentown, PA

2012-04-03

An oxygen ion transport membrane process wherein a heated oxygen-containing gas having one or more contaminants is contacted with a reactive solid material to remove the one or more contaminants. The reactive solid material is provided as a deposit on a support. The one or more contaminant compounds in the heated oxygen-containing gas react with the reactive solid material. The contaminant-depleted oxygen-containing gas is contacted with a membrane, and oxygen is transported through the membrane to provide transported oxygen.

Phase stabilization in transparent Lu2O3:Eu ceramics by lattice expansion

NASA Astrophysics Data System (ADS)

Seeley, Z. M.; Dai, Z. R.; Kuntz, J. D.; Cherepy, N. J.; Payne, S. A.

2012-11-01

Gadolinium lutetium oxide transparent ceramics doped with europium (Gd,Lu)2O3:Eu were fabricated via vacuum sintering and hot isostatic pressing (HIP). Nano-scale starting powder with the composition GdxLu1.9-xEu0.1O3 (x = 0, 0.3, 0.6, 0.9, 1.0, and 1.1) were uniaxially pressed and sintered under high vacuum at 1625 °C to obtain ˜97% dense structures with closed porosity. Sintered compacts were then subjected to 200 MPa argon gas at temperatures between 1750 and 1900 °C to reach full density. It was observed that a small portion of the Eu3+ ions were exsolved from the Lu2O3 cubic crystal lattice and concentrated at the grain boundaries, where they precipitated into a secondary monoclinic phase creating optical scattering defects. Addition of Gd3+ ions into the Lu2O3 cubic lattice formed the solid solution (Gd,Lu)2O3:Eu and stretched the lattice parameter allowing the larger Eu3+ ions to stay in solid solution, reducing the secondary phase and improving the transparency of the ceramics. Excess gadolinium, however, resulted in a complete phase transformation to monoclinic at pressures and temperatures sufficient for densification. Light yield performance was measured and all samples show equal amounts of the characteristic Eu3+ luminescence, indicating gadolinium addition had no adverse effect. This material has potential to improve the performance of high energy radiography devices.

Synthesis and Characterizations of Novel Ca-Mg-Ti-Fe-Oxides Based Ceramic Nanocrystals and Flexible Film of Polydimethylsiloxane Composite with Improved Mechanical and Dielectric Properties for Sensors

PubMed Central

Tripathy, Ashis; Pramanik, Sumit; Manna, Ayan; Azrin Shah, Nabila Farhana; Shasmin, Hanie Nadia; Radzi, Zamri; Abu Osman, Noor Azuan

2016-01-01

Armalcolite, a rare ceramic mineral and normally found in the lunar earth, was synthesized by solid-state step-sintering. The in situ phase-changed novel ceramic nanocrystals of Ca-Mg-Ti-Fe based oxide (CMTFOx), their chemical reactions and bonding with polydimethylsiloxane (PDMS) were determined by X-ray diffraction, infrared spectroscopy, and microscopy. Water absorption of all the CMTFOx was high. The lower dielectric loss tangent value (0.155 at 1 MHz) was obtained for the ceramic sintered at 1050 °C (S1050) and it became lowest for the S1050/PDMS nanocomposite (0.002 at 1 MHz) film, which was made by spin coating at 3000 rpm. The excellent flexibility (static modulus ≈ 0.27 MPa and elongation > 90%), viscoelastic property (tanδ = E″/E′: 0.225) and glass transition temperature (Tg: −58.5 °C) were obtained for S1050/PDMS film. Parallel-plate capacitive and flexible resistive humidity sensors have been developed successfully. The best sensing performance of the present S1050 (3000%) and its flexible S1050/PDMS composite film (306%) based humidity sensors was found to be at 100 Hz, better than conventional materials. PMID:26927116

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

PubMed Central

Mehdizadeh Dehkordi, Arash; Bhattacharya, Sriparna; Darroudi, Taghi; Zeng, Xiaoyu; Alshareef, Husam N.; Tritt, Terry M.

2015-01-01

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3. PMID:26327483

Synthesis and electrical properties of BaBiO 3 and high resistivity BaTiO 3 –BaBiO 3 ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Nitish; Golledge, Stephen L.; Cann, David P.

2016-12-01

Ceramics of the composition BaBiO3 (BB) were sintered in oxygen to obtain a single phase with monoclinic II2/mm symmetry as suggested by high-resolution X-ray diffraction. X-ray photoelectron spectroscopy confirmed the presence of bismuth in two valence states - 3+ and 5+. Optical spectroscopy showed presence of a direct bandgap at ~ 2.2eV and a possible indirect bandgap at ~ 0.9eV. This combined with determination of the activation energy for conduction of 0.25eV, as obtained from ac impedance spectroscopy, suggested that a polaron-mediated conduction mechanism was prevalent in BB. The BB ceramics were crushed, mixed with BaTiO3 (BT), and sintered tomore » obtain BT–BB solid solutions. All the ceramics had tetragonal symmetry and exhibited a normal ferroelectric-like dielectric response. Using ac impedance and optical spectroscopy, it was shown that resistivity values of BT–BB were orders of magnitude higher than BT or BB alone, indicating a change in the fundamental defect equilibrium conditions. A shift in the site occupancy of Bi to the A-site is proposed to be the mechanism for the increased electrical resistivity.« less

Novel ultra-low temperature co-fired microwave dielectric ceramic at 400 degrees and its chemical compatibility with base metal

PubMed Central

Di, Zhou; Li-Xia, Pang; Ze-Ming, Qi; Biao-Bing, Jin; Xi, Yao

2014-01-01

A novel NaAgMoO4 material with spinel-like structure was synthesized by using the solid state reaction method and the ceramic sample was well densified at an extreme low sintering temperature about 400°C. Rietveld refinement of the crystal structure was performed using FULLPROF program and the cell parameters are a = b = c = 9.22039 Å with a space group F D −3 M (227). High performance microwave dielectric properties, with a permittivity ~7.9, a Qf value ~33,000 GHz and a temperature coefficient of resonant frequency ~−120 ppm/°C, were obtained. From X-ray diffraction (XRD) and Energy Dispersive Spectrometer (EDS) analysis of the co-fired sample, it was found that the NaAgMoO4 ceramic is chemically compatible with both silver and aluminum at the sintering temperature and this makes it a promising candidate for the ultra-low temperature co-fired ceramics technology. Analysis of infrared and THz spectra indicated that dielectric polarizability at microwave region of the NaAgMoO4 ceramic was equally contributed by ionic displasive and electronic polarizations. Its small microwave dielectric permittivity can also be explained well by the Shannon's additive rule. PMID:25099530

The phase compositions and microwave dielectric properties of Li2Zn(Ti1-xSnx)3O8 ceramics

NASA Astrophysics Data System (ADS)

Lu, Xuepeng; Hu, Jie; Chen, Haoyuan; Xu, Wensheng; Li, Shuai

2017-08-01

The Li2Zn(Ti1-xSnx)3O8 (0.02≤x≤0.20) ceramics were prepared by the conventional solid-state ceramic route. The sintering behavior, phase compositions, microstructures and microwave dielectric properties of Li2Zn(Ti1-xSnx)3O8 ceramics were thoroughly investigated. The XRD patterns of Li2Zn(Ti1-xSnx)3O8 ceramics exhibited a single spinel as the main phase in the x value range of 0.02-0.08. The dielectric constants decreased linearly with increasing the substitution of Sn, which was mainly controlled by dielectric polarizabilities and secondary phase. The variation of Q×f values was dependent on average grain sizes and secondary phase. The τf values of Li2Zn(Ti1-xSnx)3O8 ceramics became more negative with higher substitution of Sn, which was related to the variations of their cell volumes. Typically, the Li2Zn(Ti0.92Sn0.08)3O8 ceramic sintered at 1075 °C for 4h exhibited good microwave dielectric properties: ɛr= 24.4, Q×f=89300 GHz, τf= -16.0 ppm/°C.

Synthesis and Characterizations of Novel Ca-Mg-Ti-Fe-Oxides Based Ceramic Nanocrystals and Flexible Film of Polydimethylsiloxane Composite with Improved Mechanical and Dielectric Properties for Sensors.

PubMed

Tripathy, Ashis; Pramanik, Sumit; Manna, Ayan; Shah, Nabila Farhana Azrin; Shasmin, Hanie Nadia; Radzi, Zamri; Abu Osman, Noor Azuan

2016-02-27

Armalcolite, a rare ceramic mineral and normally found in the lunar earth, was synthesized by solid-state step-sintering. The in situ phase-changed novel ceramic nanocrystals of Ca-Mg-Ti-Fe based oxide (CMTFOx), their chemical reactions and bonding with polydimethylsiloxane (PDMS) were determined by X-ray diffraction, infrared spectroscopy, and microscopy. Water absorption of all the CMTFOx was high. The lower dielectric loss tangent value (0.155 at 1 MHz) was obtained for the ceramic sintered at 1050 °C (S1050) and it became lowest for the S1050/PDMS nanocomposite (0.002 at 1 MHz) film, which was made by spin coating at 3000 rpm. The excellent flexibility (static modulus ≈ 0.27 MPa and elongation > 90%), viscoelastic property (tanδ = E″/E': 0.225) and glass transition temperature (Tg: -58.5 °C) were obtained for S1050/PDMS film. Parallel-plate capacitive and flexible resistive humidity sensors have been developed successfully. The best sensing performance of the present S1050 (3000%) and its flexible S1050/PDMS composite film (306%) based humidity sensors was found to be at 100 Hz, better than conventional materials.

Morphology, structure, optical, and electrical properties of AgSbO3

NASA Astrophysics Data System (ADS)

Yi, Z. G.; Liu, Y.; Withers, R. L.

2010-07-01

The morphology of defect pyrochlore-type, AgSbO3 microparticle/nanoparticles obtained via solid state reaction evolve from irregular to Fullerene-like polyhedra before finally decomposing into metal-organic framework-5 like particles with increase in sintering temperature. The defect pyrochlore-type AgSbO3 particles are slightly Ag deficient while the valence of the antimony ion is shown to be +5 giving rise to a probable stoichiometry of Ag1-xSbVO3-x/2, with x˜0.01-0.04. A highly structured diffuse intensity distribution observed via electron diffraction is interpreted in terms of correlated displacements of one-dimensional (1D) silver ion chains along ⟨110⟩ directions. A redshifting in the absorption edges in UV-visible absorption spectra is observed for samples prepared at sintering temperatures higher than 1000 °C and attributed to the surface plasma resonance effect associated with small amounts of excess metallic Ag on the Ag1-xSbVO3-x/2 particles. An electrical properties investigation of the silver antimonate samples via dielectric, conductivity, and electric modulus spectroscopy shows a prominent dielectric relaxation associated with grain boundaries. The silver ion conductivity is associated with correlated displacements of 1D silver ion chains along ⟨110⟩ directions.

Development of Dielectric Material with Ceramic Matrix Composite (CMC) Produced from Kaolinite and CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yin, Wong Swee; Hassan, Jumiah; Hashim, Mansor

Ceramic matrix composites (CMC) combine reinforcing ceramic phases, CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) with a ceramic matrix, kaolinite to create materials with new and superior properties. 10% and 20% CCTO were prepared by using a conventional solid state reaction method. CMC samples were pre-sintered at 800 deg. C and sintered at 1000 deg. C. The dielectric properties of samples were measured using HP 4192A LF Impedance Analyzer. Microstructures of the samples were observed using an optical microscope. XRD was used to determine the crystalline structure of the samples. The AFM showed the morphology of the samples. The results showed thatmore » the dielectric constant and dielectric loss factor of both samples are frequency dependent. At 10 Hz, the dielectric constant is 10{sup 11} for both samples. The CMC samples were independent with temperature with low dielectric constant in the frequency range of 10{sup 4}-10{sup 6} Hz. Since the CMC samples consist of different amount of kaolinite, so each sample exhibit different defect mechanism. Different reaction may occur for different composition of material. The effects of processing conditions on the microstructure and electrical properties of CMC are also discussed.« less

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties.

PubMed

Mehdizadeh Dehkordi, Arash; Bhattacharya, Sriparna; Darroudi, Taghi; Zeng, Xiaoyu; Alshareef, Husam N; Tritt, Terry M

2015-08-15

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

Ionic Conductivity and Air Stability of Al-Doped Li₇La₃Zr₂O₁₂ Sintered in Alumina and Pt Crucibles.

PubMed

Xia, Wenhao; Xu, Biyi; Duan, Huanan; Guo, Yiping; Kang, Hongmei; Li, Hua; Liu, Hezhou

2016-03-02

Li7La3Zr2O12 (LLZO) is a promising electrolyte material for all-solid-state battery due to its high ionic conductivity and good stability with metallic lithium. In this article, we studied the effect of crucibles on the ionic conductivity and air stability by synthesizing 0.25Al doped LLZO pellets in Pt crucibles and alumina crucibles, respectively. The results show that the composition and microstructure of the pellets play important roles influencing the ionic conductivity, relative density, and air stability. Specifically, the 0.25Al-LLZO pellets sintered in Pt crucibles exhibit a high relative density (∼96%) and high ionic conductivity (4.48 × 10(-4) S cm(-1)). The ionic conductivity maintains 3.6 × 10(-4) S cm(-1) after 3-month air exposure. In contrast, the ionic conductivity of the pellets from alumina crucibles is about 1.81 × 10(-4) S cm(-1) and drops to 2.39 × 10(-5) S cm(-1) 3 months later. The large grains and the reduced grain boundaries in the pellets sintered in Pt crucibles are favorable to obtain high ionic conductivity and good air stability. X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy results suggest that the formation of Li2CO3 on the pellet surface is probably another main reason, which is also closely related to the relative density and the amount of grain boundary within the pellets. This work stresses the importance of synthesis parameters, crucibles included, to obtain the LLZO electrolyte with high ionic conductivity and good air stability.

Mechanical and physical behavior of newly developed functionally graded materials and composites of stainless steel 316L with calcium silicate and hydroxyapatite.

PubMed

Ataollahi Oshkour, Azim; Pramanik, Sumit; Mehrali, Mehdi; Yau, Yat Huang; Tarlochan, Faris; Abu Osman, Noor Azuan

2015-09-01

This study aimed to investigate the structural, physical and mechanical behavior of composites and functionally graded materials (FGMs) made of stainless steel (SS-316L)/hydroxyapatite (HA) and SS-316L/calcium silicate (CS) employing powder metallurgical solid state sintering. The structural analysis using X-ray diffraction showed that the sintering at high temperature led to the reaction between compounds of the SS-316L and HA, while SS-316L and CS remained intact during the sintering process in composites of SS-316L/CS. A dimensional expansion was found in the composites made of 40 and 50 wt% HA. The minimum shrinkage was emerged in 50 wt% CS composite, while the maximum shrinkage was revealed in samples with pure SS-316L, HA and CS. Compressive mechanical properties of SS-316L/HA decreased sharply with increasing of HA content up to 20 wt% and gradually with CS content up to 50 wt% for SS-316L/CS composites. The mechanical properties of the FGM of SS-316L/HA dropped with increase in temperature, while it was improved for the FGM of SS-316L/CS with temperature enhancement. It has been found that the FGMs emerged a better compressive mechanical properties compared to both the composite systems. Therefore, the SS-316L/CS composites and their FGMs have superior compressive mechanical properties to the SS-316L/HA composites and their FGMs and also the newly developed FGMs of SS-316L/CS with improved mechanical and enhanced gradation in physical and structural properties can potentially be utilized in the components with load-bearing application. Copyright © 2015 Elsevier Ltd. All rights reserved.

Synthesis and characterisation of novel low temperature ceramic and its implementation as substrate in dual segment CDRA

NASA Astrophysics Data System (ADS)

Kumari, Preeti; Tripathi, Pankaj; Sahu, Bhagirath; Singh, S. P.; Parkash, Om; Kumar, Devendra

2018-02-01

Li2O-(2-3x)MgO-(x)Al2O3-P2O5 (LMAP) (x = 0.00-0.08) ceramic system was prepared through solid state synthesis route at different sintering temperatures (800-925 °C). A small addition of Al2O3 (x = 0.02) in LMAP ceramics lowers the sintering temperature by more than 100 °C with good relative density of 94.13%. The sintered samples were characterized in terms of density, apparent porosity, water absorption, crystal structure, micro-structure and microwave dielectric properties. Silver compatibility test is also performed for its use as electrode material in low temperature co-fired ceramic (LTCC) application. To check the performance of the prepared LTCC as substrate, a microstrip-fed aperture-coupled dual segment cylindrical dielectric resonator antenna (DS-CDRA) is designed using LMAP (x = 0.02) ceramic as substrate material and Barium Strontium Titanate with 10 wt% of PbO-BaO-B2O3-SiO2 glass (BSTG) and Teflon as the components of resonating material. The simulation study of the DS-CDRA is performed using the Ansys High Frequency Structure Simulator (HFSS) software. A conductive coating of silver is used on the substrate. The simulated and measured -10 dB reflection coefficient bandwidths of 910 MHz (9.07-9.98 GHz at resonant frequency of 9.49 GHz) and 1080 MHz (8.68-9.76 GHz at resonant frequency of 9.36 GHz), respectively are achieved. The measured results of the fabricated antenna are found in good agreement with the simulation results. The prepared material can find potential applications in radar and radio navigation as well as radio astronomy and military satellite communication.

Global distribution of particle phase state in atmospheric secondary organic aerosols

NASA Astrophysics Data System (ADS)

Shiraiwa, Manabu; Li, Ying; Tsimpidi, Alexandra P.; Karydis, Vlassis A.; Berkemeier, Thomas; Pandis, Spyros N.; Lelieveld, Jos; Koop, Thomas; Pöschl, Ulrich

2017-04-01

Secondary organic aerosols (SOA) are a large source of uncertainty in our current understanding of climate change and air pollution. The phase state of SOA is important for quantifying their effects on climate and air quality, but its global distribution is poorly characterized. We developed a method to estimate glass transition temperatures based on the molar mass and molecular O:C ratio of SOA components, and we used the global chemistry climate model EMAC with the organic aerosol module ORACLE to predict the phase state of atmospheric SOA. For the planetary boundary layer, global simulations indicate that SOA are mostly liquid in tropical and polar air with high relative humidity, semi-solid in the mid-latitudes and solid over dry lands. We find that in the middle and upper troposphere SOA should be mostly in a glassy solid phase state. Thus, slow diffusion of water, oxidants and organic molecules could kinetically limit gas-particle interactions of SOA in the free and upper troposphere, promote ice nucleation and facilitate long-range transport of reactive and toxic organic pollutants embedded in SOA.

Global distribution of particle phase state in atmospheric secondary organic aerosols.

PubMed

Shiraiwa, Manabu; Li, Ying; Tsimpidi, Alexandra P; Karydis, Vlassis A; Berkemeier, Thomas; Pandis, Spyros N; Lelieveld, Jos; Koop, Thomas; Pöschl, Ulrich

2017-04-21

Secondary organic aerosols (SOA) are a large source of uncertainty in our current understanding of climate change and air pollution. The phase state of SOA is important for quantifying their effects on climate and air quality, but its global distribution is poorly characterized. We developed a method to estimate glass transition temperatures based on the molar mass and molecular O:C ratio of SOA components, and we used the global chemistry climate model EMAC with the organic aerosol module ORACLE to predict the phase state of atmospheric SOA. For the planetary boundary layer, global simulations indicate that SOA are mostly liquid in tropical and polar air with high relative humidity, semi-solid in the mid-latitudes and solid over dry lands. We find that in the middle and upper troposphere SOA should be mostly in a glassy solid phase state. Thus, slow diffusion of water, oxidants and organic molecules could kinetically limit gas-particle interactions of SOA in the free and upper troposphere, promote ice nucleation and facilitate long-range transport of reactive and toxic organic pollutants embedded in SOA.

Global distribution of particle phase state in atmospheric secondary organic aerosols

PubMed Central

Shiraiwa, Manabu; Li, Ying; Tsimpidi, Alexandra P.; Karydis, Vlassis A.; Berkemeier, Thomas; Pandis, Spyros N.; Lelieveld, Jos; Koop, Thomas; Pöschl, Ulrich

2017-01-01

Secondary organic aerosols (SOA) are a large source of uncertainty in our current understanding of climate change and air pollution. The phase state of SOA is important for quantifying their effects on climate and air quality, but its global distribution is poorly characterized. We developed a method to estimate glass transition temperatures based on the molar mass and molecular O:C ratio of SOA components, and we used the global chemistry climate model EMAC with the organic aerosol module ORACLE to predict the phase state of atmospheric SOA. For the planetary boundary layer, global simulations indicate that SOA are mostly liquid in tropical and polar air with high relative humidity, semi-solid in the mid-latitudes and solid over dry lands. We find that in the middle and upper troposphere SOA should be mostly in a glassy solid phase state. Thus, slow diffusion of water, oxidants and organic molecules could kinetically limit gas–particle interactions of SOA in the free and upper troposphere, promote ice nucleation and facilitate long-range transport of reactive and toxic organic pollutants embedded in SOA. PMID:28429776

Fabrication and characterization of nano-Y2O3 and Al2O3 dispersed W-Ni alloys by mechanical alloying and pressureless conventional sintering

NASA Astrophysics Data System (ADS)

Talekar, V. R.; Patra, A.; Karak, S. K.

2018-03-01

Nano Y2O3 and Al2O3 dispersed W-Ni alloys with nominal composition of W89Ni10 (Y2O3)1 (alloy A), W89Ni10 (Al2O3)1 (alloy B) were mechanically alloyed for 10 h followed by compaction at 0.5 GPa pressure with 5 min of dwell time and conventional sintering at 1400°C with 2 h soaking time in Ar atmosphere with Ar flow rate of 100 ml/min. The microstructure of milled and sintered alloy was investigated using X-ray Diffraction (XRD), Scanning electron Microscopy (SEM), Energy dispersive spectroscopy (EDS) and Elemental mapping. Minimum crystallite size of 31.9 nm and maximum lattice strain, dislocation density of 0.23%, 9.12(1016/m2) respectively was found in alloy A at 10 h of milling. Uneven and coarse particles at 0 h of milling converted to elongated flake shape at 10 h of milling. Bimodal (fine and coarse) particle size distribution is revealed in both the alloys and minimum particle size of 0.69 μm is achieved in 10 h milled alloy A. Evidences of formation of intermetallic phases like Y2WO6, Y6WO12 and Y10W2O21 in sintered alloy A and Al2(WO4)3, NiAl10O16, NiAl2O4 and AlWO4 in sintered alloy B were revealed by XRD pattern and SEM micrograph. Minimum grain size of 1.50 μm was recorded in sintered alloy A. Both faceted and spherical W matrix is evident in both the alloys which suggests occurrence of both solid phase and liquid phase sintering. Maximum % relative sintered density and hardness of 85.29% and 5.13 GPa respectively was found in alloy A. Wear study at 20N force at 25 rpm for 15 min on ball on plate wear tester revealed that minimum wear depth (48.99 μm) and wear track width (272 μm) was found for alloy A as compared to alloy B.

Effect of Al(OH)3 on the sintering of UO2-Gd2O3 fuel pellets with addition of U3O8 from recycle

NASA Astrophysics Data System (ADS)

dos Santos, Lauro Roberto; Durazzo, Michelangelo; Urano de Carvalho, Elita Fontenele; Riella, Humberto Gracher

2017-09-01

The incorporation of gadolinium as burnable poison directly into nuclear fuel is important for reactivity compensation, which enables longer fuel cycles. The function of the burnable poison fuel is to control the neutron population in the reactor core during its startup and the beginning of the fuel burning cycle to extend the use of the fuel. The implementation of UO2-Gd2O3 poisoned fuel in Brazil has been proposed according to the future requirements established for the Angra-2 nuclear power plant. The UO2 powder used is produced from the Ammonium Uranyl Carbonate (AUC). The incorporation of Gd2O3 powder directly into the AUC-derived UO2 powder by dry mechanical blending is the most attractive process, because of its simplicity. Nevertheless, processing by this method leads to difficulties while obtaining sintered pellets with the minimum required density. The cause of the low densities is the bad sintering behavior of the UO2-Gd2O3 mixed fuel, which shows a blockage in the sintering process that hinders the densification. This effect has been overcome by microdoping of the fuel with small quantities of aluminum. The process for manufacturing the fuel inevitably generates uranium-rich scraps from various sources. This residue is reincorporated into the production process in the form of U3O8 powder additions. The addition of U3O8 also hinders densification in sintering. This study was carried out to investigate the influence of both aluminum and U3O8 additives on the density of fuel pellets after sintering. As the effects of these additives are counterposed, this work studied the combined effect thereof, seeking to find an applicable composition for the production process. The experimental results demonstrated the effectiveness of aluminum, in the form of Al(OH)3, as an additive to promote increase in the densification of the (U,Gd)O2 pellets during sintering, even with high additions of U3O8 recycled from the manufacturing process.

Piezoelectric Ceramics of the (1 − x)Bi0.50Na0.50TiO3–xBa0.90Ca0.10TiO3 Lead-Free Solid Solution: Chemical Shift of the Morphotropic Phase Boundary, a Case Study for x = 0.06

PubMed Central

Vivar-Ocampo, Rodrigo; Pardo, Lorena; Ávila, David; Morán, Emilio; González, Amador M.; Bucio, Lauro; Villafuerte-Castrejón, María-Elena

2017-01-01

Research and development of lead-free piezoelectric materials are still the hottest topics in the field of piezoelectricity. One of the most promising lead-free family of compounds to replace lead zirconate–titanate for actuators is that of Bi0.50Na0.50TiO3 (BNT) based solid solutions. The pseudo-binary (1 − x)Bi0.50Na0.50TiO3–xBa1 − yCayTiO3 system has been proposed for high temperature capacitors and not yet fully explored as piezoelectric material. In this work, the solid solution with x = 0.06 and y = 0.10 was obtained by two different synthesis routes: solid state and Pechini, aiming at using reduced temperatures, both in synthesis (<800 °C) and sintering (<1150 °C), while maintaining appropriated piezoelectric performance. Crystal structure, ceramic grain size, and morphology depend on the synthesis route and were analyzed by X-ray diffraction, together with scanning and transmission electron microscopy. The effects of processing and ceramic microstructure on the structural, dielectric, ferroelectric, and piezoelectric properties were discussed in terms of a shift of the Morphotropic Phase Boundary, chemically induced by the synthesis route. PMID:28773096

Piezoelectric Ceramics of the (1 - x)Bi0.50Na0.50TiO₃-xBa0.90Ca0.10TiO₃ Lead-Free Solid Solution: Chemical Shift of the Morphotropic Phase Boundary, a Case Study for x = 0.06.

PubMed

Vivar-Ocampo, Rodrigo; Pardo, Lorena; Ávila, David; Morán, Emilio; González, Amador M; Bucio, Lauro; Villafuerte-Castrejón, María-Elena

2017-07-01

Research and development of lead-free piezoelectric materials are still the hottest topics in the field of piezoelectricity. One of the most promising lead-free family of compounds to replace lead zirconate-titanate for actuators is that of Bi 0.50 Na 0.50 TiO₃ (BNT) based solid solutions. The pseudo-binary (1 - x )Bi 0.50 Na 0.50 TiO₃- x Ba 1 - y Ca y TiO₃ system has been proposed for high temperature capacitors and not yet fully explored as piezoelectric material. In this work, the solid solution with x = 0.06 and y = 0.10 was obtained by two different synthesis routes: solid state and Pechini, aiming at using reduced temperatures, both in synthesis (<800 °C) and sintering (<1150 °C), while maintaining appropriated piezoelectric performance. Crystal structure, ceramic grain size, and morphology depend on the synthesis route and were analyzed by X-ray diffraction, together with scanning and transmission electron microscopy. The effects of processing and ceramic microstructure on the structural, dielectric, ferroelectric, and piezoelectric properties were discussed in terms of a shift of the Morphotropic Phase Boundary, chemically induced by the synthesis route.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Du Hongliang; Zhou Wancheng; Luo Fa

The (1-x)(K{sub 0.5}Na{sub 0.5})NbO{sub 3}-x(Ba{sub 0.5}Sr{sub 0.5})TiO{sub 3} (KNN-BST) solid solution has been synthesized by conventional solid-state sintering in order to search for the new lead-free relaxor ferroelectrics for high temperature applications. The phase structure, dielectric properties, and relaxor behavior of the (1-x)KNN-xBST solid solution are systematically investigated. The phase structure of the (1-x)KNN-xBST solid solution gradually changes from pure perovskite phase with an orthorhombic symmetry to the tetragonal symmetry, then to the pseudocubic phase, and to the cubic phase with increasing addition of BST. The 0.90KNN-0.10BST solid solution shows a broad dielectric peak with permittivity maximum near 2500 andmore » low dielectric loss (<4%) in the temperature range of 100-250 deg. C. The result indicates that this material may have great potential for a variety of high temperature applications. The diffuse phase transition and the temperature of the maximum dielectric permittivity shifting toward higher temperature with increasing frequency, which are two typical characteristics for relaxor ferroelectrics, are observed in the (1-x)KNN-xBST solid solution. The dielectric relaxor behavior obeys a modified Curie-Weiss law and a Vogel-Fulcher relationship. The relaxor nature is attributed to the appearance of polar nanoregions owing to the formation of randon fields including local electric fields and elastic fields. These results confirm that the KNN-based relaxor ferroelectrics can be regarded as an alternative direction for the development of high temperature lead-free relaxor ferroelectrics.« less

The Impact of Condensed-Phase Viscosity on Multiphase Oxidation Kinetics Involving O3, NO3, and OH

NASA Astrophysics Data System (ADS)

Li, J.; Forrester, S. M.; Knopf, D. A.

2017-12-01

Organic aerosol (OA) particles are ubiquitous in the atmosphere and have a significant influence on air quality, human health, cloud formation processes and global climate. By now it is well-recognized that organic particulate species can be amorphous in nature, existing in liquid, semi-solid and solid (glassy) phase states. The phase state is modulated by particle composition and environmental conditions such as relative humidity and temperature. These modifications can influence particle viscosity and molecular diffusion and, therefore, impact the reactive uptake of gas-phase oxidants and radicals by the organic substrate. In this study, we determined the reactive uptake coefficients (γ) of O3 by canola oil, NO3 by levoglucosan (LEV) and a LEV/xylitol mixture, and OH by glucose/sulfuric acid mixtures and glucose/1,2,6-hexanetriol mixtures under dry conditions and for temperatures ranging from 293 K to 213 K. Uptake coefficients have been measured employing a chemical ionization mass spectrometer coupled to a temperature-controlled rotating-wall flow reactor. Glass transition temperatures (Tg) of applied substrates were estimated by the Gordon-Taylor equation. Phase states were qualitatively probed via poking experiment using a temperature-controlled cooling stage. Shattering of the substrates indicated the formation of a glassy state. Results show a significant impact of condensed phase state on reactive uptake kinetics whereby γ changed most profoundly around estimated Tg. For example, γ decreases from 6.5×10-4 to 1.9 ×10-5 for O3 uptake by canola oil and from 8.3×10-4 to 3.1×10-4 for NO3 uptake by the LEV/xylitol mixture, respectively. The decrease in γ will be discussed with regard to phase state, desorption lifetime, and Arrhenius temperature dependence of reaction rates. First results of OH uptakes at low temperatures are presented, together with a discussion of the relevant atmospheric implications.

High resolution laser micro sintering / melting using q-switched and high brilliant laser radiation

NASA Astrophysics Data System (ADS)

Exner, H.; Streek, A.

2015-03-01

Since the discovery of selective laser sintering/melting, numerous modifications have been made to upgrade or customize this technology for industrial purposes. Laser micro sintering (LMS) is one of those modifications: Powders with particles in the range of a few micrometers are used to obtain products with highly resolved structures. Pulses of a q-switched laser had been considered necessary in order to generate sinter layers from the micrometer scaled metal powders. LMS has been applied with powders from metals as well as from ceramic and cermet feedstock's to generate micro parts. Recent technological progress and the application of high brilliant continuous laser radiation have now allowed an efficient laser sintering/melting of micrometer scaled metal powders. Thereby it is remarkable that thin sinter layers are generated using high continuous laser power. The principles of the process, the state of the art in LMS concerning its advantages and limitations and furthermore the latest results of the recent development of this technology will be presented. Laser Micro Sintering / Laser Micro Melting (LMM) offer a vision for a new dimension of additive fabrication of miniature and precise parts also with application potential in all engineering fields.

Photoluminescent properties of Eu-doped ZnLiNbO4

NASA Astrophysics Data System (ADS)

Huang, Meng-Hsi; Lin, Ming-Hong; Fang, Te-Hua; Chang, Chia-Wei

2018-04-01

In this study, fluorescent Eu3+-doped ZnLiNbO4 materials were prepared via a vibrating milled solid-state reaction method. The objective was to develop new fluorescent oxide materials and study their fluorescent properties. The ZnLiNbO4 tetragonal spinel structure was formed with a single phase at a sintering temperature of 800 °C and with a regular shape at 1000 °C. The main exciton band was at 466 nm (7F0 → 5D2), and the main emission band was at 615 nm (5D0 → 7F2), which was an orange–red light band. The emission intensity was approximately 5% when the doping concentration reached 7%. The decay time was 2.96 ms.

Synthesis and study on the luminescence properties of cadmium borate phosphors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Annalakshmi, O.; Jose, M.T., E-mail: mtjosein@yahoo.co.in; Venkatraman, B.

2014-02-01

Highlights: • Cadmium borate synthesized by solid state sintering technique. • Neutron sensitivity of the material ten times that of TLD-600. • Gamma sensitivity is found to be twice that of TLD-100. • Gamma response is linear from 0.1 to 10{sup 3} mGy. - Abstract: Cadmium borate compound prepared through wet chemical reaction from the starting chemicals followed by high temperature solid state synthesis below the melting point to get the final TL phosphor powder. Phase purity and bond details of cadmium borate crystals are characterized using X-ray diffraction technique and infrared spectroscopy. Feasibility of these materials for radiation dosimetrymore » applications was studied after gamma and neutron irradiation. Gamma irradiation of undoped phosphors show a single peak around 185 °C whereas doping with gadolinium and silver, new more intense peak observed at 290 °C. Irradiation to thermal neutrons revealed single peak around 170 °C for all the phosphors. TL emission spectra and photoluminescence (PL) studies were also carried out on the phosphors. These borate materials are found to be highly sensitive to neutrons and hence can be used for neutron detection. Neutron sensitivity of the material is about ten times that of TLD-600.« less

Visible light photoreactivity from Carbon nitride bandgap states in Nb and Ti oxides

NASA Astrophysics Data System (ADS)

Lee, Hosik; Ohno, Takahisa; Icnsee Team

2011-03-01

Lamellar niobic and titanic solid acids (HNb3O8 , H2Ti4O9) are photocatalysts which can be used for environmental cleanup application and hydrogen production through water splitting. To increase their efficiency, bandgap adjustment which can induce visible light reactivity in addition to ultraviolet light has been one of hot issue in this kinds of photo-catalytic materials. Nitrogen-doping was one of the direction and its microscopic structures are disputed in this decade. In this work, we calculate the layered niobic and titanic solid acids structure and bandgap. Bandgap reduction by carbon nitride absorption are observed computationally. It is originated from localized nitrogen state which is consistent with previous experiments.

A Model of Solid State Gas Sensors

NASA Astrophysics Data System (ADS)

Woestman, J. T.; Brailsford, A. D.; Shane, M.; Logothetis, E. M.

1997-03-01

Solid state gas sensors are widely used to measure the concentrations of gases such as CO, CH_4, C_3H_6, H_2, C_3H8 and O2 The applications of these sensors range from air-to-fuel ratio control in combustion processes including those in automotive engines and industrial furnaces to leakage detection of inflammable and toxic gases in domestic and industrial environments. As the need increases to accurately measure smaller and smaller concentrations, problems such as poor selectivity, stability and response time limit the use of these sensors. In an effort to overcome some of these limitations, a theoretical model of the transient behavior of solid state gas sensors has been developed. In this presentation, a model for the transient response of an electrochemical gas sensor to gas mixtures containing O2 and one reducing species, such as CO, is discussed. This model accounts for the transport of the reactive species to the sampling electrode, the catalyzed oxidation/reduction reaction of these species and the generation of the resulting electrical signal. The model will be shown to reproduce the results of published steady state models and to agree with experimental steady state and transient data.

Production of coloured glass-ceramics from incinerator ash using thermal plasma technology.

PubMed

Cheng, T W; Huang, M Z; Tzeng, C C; Cheng, K B; Ueng, T H

2007-08-01

Incineration is a major treatment process for municipal solid waste in Taiwan. It is estimated that over 1.5 Mt of incinerator ash are produced annually. This study proposes using thermal plasma technology to treat incinerator ash. Sintered glass-ceramics were produced using quenched vitrified slag with colouring agents added. The experimental results showed that the major crystalline phases developed in the sintered glass-ceramics were gehlenite and wollastonite, but many other secondary phases also appeared depending on the colouring agents added. The physical/mechanical properties, chemical resistance and toxicity characteristic leaching procedure of the coloured glass-ceramics were satisfactory. The glass-ceramic products obtained from incinerator ash treated with thermal plasma technology have great potential for building applications.

Method and apparatus for making articles from particle based materials

DOEpatents

Moorhead, A.J.; Menchhofer, P.A.

1995-12-19

A method and apparatus are disclosed for the production of articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with the invention, a thermally settable slurry containing a relatively high concentration of the particles is conveyed through an elongate flow area having a desired cross-sectional configuration. The slurry is heated as it is advanced through the flow area causing the slurry to set or harden in a shape which conforms to the cross-sectional configuration of the flow area. The material discharges from the flow area as a self-supporting solid of near net final dimensions. The article may then be sintered to consolidate the particles and provide a high density product. 10 figs.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miller, D.J.; Pask, J.A.

The sintering of TiC-Ni particle compacts was studied with specific attention to effects of processing conditions. Densification was progressively inhibited with the increasing additions of free carbon to the system. These results are explained on the basis of changes in the eutectic reactions in the system, reduced solubility of TiC in the Ni-rich liquid, and decreased wetting of the solid by the liquid. Presintering hydrogen heat treatment reduced the carbon content of the TiC-Ni compacts and led to reduction in sintering rates and elevated temperatures of liquid-phase formation. Wetting experiments with hydrogen-treated materials showed a time-dependent wetting angle. These resultsmore » are discussed based on wetting theory and reactions predicted by the equilibrium ternary-phase diagram.« less

Effect of Mg(2+) doping on beta-alpha phase transition in tricalcium phosphate (TCP) bioceramics.

PubMed

Frasnelli, Matteo; Sglavo, Vincenzo M

2016-03-01

The beta to alpha transition in tricalcium phosphate (TCP) bioceramics containing different amount of magnesium was studied in the present work. Mg-doped TCP powder was obtained by solid-state reaction starting from pure calcium carbonate, ammonium phosphate dibasic and magnesium oxide powders. The β to α transformation temperature was identified by dilatometric and thermo-differential analyses. Small pellets produced by uniaxial pressing samples were employed to study the influence of Mg(2+) on the transition kinetic, after sintering at 1550°C and subsequent slow or fast cooling down to room temperature. The evolution of β- and α-TCP crystalline phases during each thermal treatment was determined by X-ray powder diffraction analysis combined with Rietveld method-based software An annealing treatment, suitable to reconvert metastable α phase to the more clinically suitable β phase, was also investigated. It is shown that the presence of magnesium within the TCP lattice strongly influences the kinetic of the β⇆α phase transition, promoting the spontaneous α→β reconversion even upon fast cooling, or slowing down the β→α transition during heating. Similarly, it allows the α→β transformation in TCP sintered components by optimized annealing treatment at 850°C. This work concerns the effect of Mg(2+) doping on the β→α phase reconstructive transition in tricalcium phosphate (TCP), one of the most important bio-resorbable materials for bone tissue regeneration. The transition occurs upon the sintering process and is has been shown to be strongly irreversible upon cooling, leading to technological issues such as poor mechanical properties and excessive solubility due to the presence of metastable α-phase. This paper points out the kinetic contribution of Mg(2+) on the spontaneous α→β reconversion also upon fast cooling (i.e. quenching). Moreover, an annealing treatment has been shown to be beneficial to remove the retained α-phase in sintered TCP components, the presence of Mg promoting the reconversion process. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

High surface area neodymium phosphate nano particles by modified aqueous sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sankar, Sasidharan; Warrier, Krishna Gopakumar, E-mail: wwarrierkgk@yahoo.co.in; Komban, Rajesh

2011-12-15

Graphical abstract: Synthesis of nano rod shaped neodymium phosphate particles with specific surface area as high as 107 m{sup 2} g{sup -1} and particles could be compacted and sintered at as low as 1300 Degree-Sign C to a density of 98.5% (theoretical) with an average grain size of {approx}1 {mu}m. Highlights: Black-Right-Pointing-Pointer Nano size neodymium phosphate is synthesized and characterized using a novel modified aqueous sol gel process. Black-Right-Pointing-Pointer Specific surface area above 100 m{sup 2} g{sup -1} achieved without the addition of any complexing agents. Black-Right-Pointing-Pointer High sintered density reported than the density obtained for powder synthesized through conventionalmore » solid state reaction. Black-Right-Pointing-Pointer The particles are nano sized and have rod shape morphology and are retained at higher temperatures. Black-Right-Pointing-Pointer An average grain size of {approx}1 {mu}m obtained for sintered NdPO{sub 4} after thermal etching at 1400 Degree-Sign C. -- Abstract: Synthesis of nano rod shaped neodymium phosphate (NdPO{sub 4}) particles with specific surface area as high as 107 m{sup 2}g{sup -1} and an average length of 50 nm with aspect ratio 5 was achieved using modified sol gel method. Crystallite size calculated from the X-ray diffraction data by applying Scherer equation was 5 nm for the precursor gel after calcination at 400 Degree-Sign C. NdPO{sub 4} was first precipitated from neodymium nitrate solution using phosphoric acid followed by peptization using dilute nitric acid and further gelation in ammonia atmosphere. The calcined gel powders were further characterized by surface area (Brunauer-Emmet-Teller nitrogen adsorption analysis), Transmission electron microscopy, scanning electron microscopy, UV-vis and FT-IR analysis. Transmission electron microscopy confirms the formation of rod like morphology from the sol, gel and the calcined particles in nano size range. These particles could be compacted and sintered at as low as 1300 Degree-Sign C to a density of 98.5% (theoretical) with an average grain size of {approx}1 {mu}m.« less

Synthesis and sintering of UN-UO 2 fuel composites

DOE PAGES

Jaques, Brian J.; Watkins, Jennifer; Croteau, Joseph R.; ...

2015-06-17

In this study, the design and development of an economical, accident tolerant fuel (ATF) for use in the current light water reactor (LWR) fleet is highly desirable for the future of nuclear power. Uranium mononitride has been identified as an alternative fuel with higher uranium density and thermal conductivity when compared to the benchmark, UO 2, which could also provide significant economic benefits. However, UN by itself reacts with water at reactor operating temperatures. In order to reduce its reactivity, the addition of UO 2 to UN has been suggested. In order to avoid carbon impurities, UN was synthesized frommore » elemental uranium using a hydride-dehydride-nitride thermal synthesis route prior to mixing with up to 10 wt% UO 2 in a planetary ball mill. UN and UN – UO 2 composite pellets were sintered in Ar – (0–1 at%) N 2 to study the effects of nitrogen concentration on the evolved phases and microstructure. UN and UN-UO 2 composite pellets were also sintered in Ar – 100 ppm N 2 to assess the effects of temperature (1700–2000 °C) on the final grain morphology and phase concentration.« less

A novel method for preparation of high dense tetragonal Li7La3Zr2O12

NASA Astrophysics Data System (ADS)

Zhao, Pengcheng; Wen, Yuehua; Cheng, Jie; Cao, Gaoping; Jin, Zhaoqing; Ming, Hai; Xu, Yan; Zhu, Xiayu

2017-03-01

For conventional preparation methods of Li7La3Zr2O12 (LLZO) solid state electrolytes, there is a stereotype that higher density always comes from higher pressure enforced upon the LLZO pellets. In this paper, a different way with an auto-consolidation mechanism is provided and discussed. No pressing operations are employed during the whole preparation process. Due to the surface tension of liquid melted Li2O at sintering temperature, LLZO particles could aggregate together freely and automatically. The preparation process for dense LLZO is greatly simplified. A dense tetragonal LLZO with high relative density about 93% has been prepared successfully by this auto-consolidation method. And there are no voids observed in the SEM images. At 30 °C, the total conductivity is about 5.67 × 10-5 S cm-1, which is the highest one for tetragonal LLZO in the reported issues, even two times higher than that prepared by hot-pressing method. The activation energy for total conductivity is ∼0.35 eV atom-1 at 30-120 °C, slightly lower than the previous reported values. This work sheds light on the understanding of the consolidation mechanism for solid electrolytes and suggests a reliable route to syhthesize cemanic solid electrolytes.

Effects of different compositions from magnetic and nonmagnetic dopants on structural and electrical properties of ZnO nanoparticles-based varistor ceramics

NASA Astrophysics Data System (ADS)

Sendi, Rabab Khalid

2018-03-01

In the current study, 20 nm zinc oxide (ZnO) nanoparticles were used to manufacture high-density ZnO discs doped with Mn and Sn via the conventional ceramic processing method, and their properties were characterized. Results show that the dopants were found to have significant effects on the ZnO varistors, especially on the shape and size of grains, which are significantly different for both dopants. The strong solid-state reaction in the varistor from the 20 nm ZnO powder during the sintering process may be attributed to the high surface area of the 20 nm ZnO nanoparticles. Although Mn and Sn do not affect the well-known peaks related to the wurtzite structure of ZnO ceramics, a few of the additional peaks could be formed at high doping content (≥2.0) due to the formation of other unknown phases during the sintering process. Both additives also significantly affect the electrical properties of the varistor, with a marked changed in the breakdown voltage from 415 V to 460 V for Sn and from 400 V to 950 V for Mn. Interestingly, the electrical behaviors of the varistors, such as breakdown voltage, nonlinear coefficient, and barrier height, are higher for Mn- than Sn-doping samples, and the opposite behaviors hold for hardness, leakage currents, and electrical conductivities. Results show that the magnetic moment and valence state of the two additive dopants are responsible for all demonstrated differences in the electrical characteristics between the two dopants.

Development of a ReaxFF reactive force field for ammonium nitrate and application to shock compression and thermal decomposition.

PubMed

Shan, Tzu-Ray; van Duin, Adri C T; Thompson, Aidan P

2014-02-27

We have developed a new ReaxFF reactive force field parametrization for ammonium nitrate. Starting with an existing nitramine/TATB ReaxFF parametrization, we optimized it to reproduce electronic structure calculations for dissociation barriers, heats of formation, and crystal structure properties of ammonium nitrate phases. We have used it to predict the isothermal pressure-volume curve and the unreacted principal Hugoniot states. The predicted isothermal pressure-volume curve for phase IV solid ammonium nitrate agreed with electronic structure calculations and experimental data within 10% error for the considered range of compression. The predicted unreacted principal Hugoniot states were approximately 17% stiffer than experimental measurements. We then simulated thermal decomposition during heating to 2500 K. Thermal decomposition pathways agreed with experimental findings.

Observation of a new surface mode on a fluid-saturated permeable solid

NASA Astrophysics Data System (ADS)

Nagy, Peter B.

1992-06-01

Almost ten years ago, S. Feng and D. L. Johnson predicted the presence of a new surface mode on a fluid/fluid-saturated porous solid interface with closed surface pores [J. Acoust. Soc. Am. 74, 906 (1983)]. We found that, due to surface tension, practically closed-pore boundary conditions can prevail at an interface between a nonwetting fluid (e.g., air) and a porous solid saturated with a wetting fluid (e.g., water or alcohol). Surface wave velocity and attenuation measurements were made on alcohol-saturated porous sintered glass at 100 kHz. The experimental results show clear evidence of the new ``slow'' surface mode predicted by Feng and Johnson.

Synthesis of solid solutions of perovskites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dambekalne, M.Y.; Antonova, M.K.; Perro, I.T.

The authors carry out thermographic studies, using a derivatograph, in order to understand the nature of the processes taking place during the synthesis of solid solutions of perovskites. Based on the detailed studies on the phase transformations occurring in the charges of the PSN-PMN solid solutions and on the selection of the optimum conditions for carrying out their synthesis, the authors obtained a powder containing a minimum quantity of the undesirable pyrochlore phase and by sintering it using the hot pressing method, they produced single phase ceramic specimens containing the perovskite phase alone with a density close to the theoreticalmore » value and showing zero apparent porosity and water absorption.« less

Metal Oxide Nanostructures and Their Gas Sensing Properties: A Review

PubMed Central

Sun, Yu-Feng; Liu, Shao-Bo; Meng, Fan-Li; Liu, Jin-Yun; Jin, Zhen; Kong, Ling-Tao; Liu, Jin-Huai

2012-01-01

Metal oxide gas sensors are predominant solid-state gas detecting devices for domestic, commercial and industrial applications, which have many advantages such as low cost, easy production, and compact size. However, the performance of such sensors is significantly influenced by the morphology and structure of sensing materials, resulting in a great obstacle for gas sensors based on bulk materials or dense films to achieve highly-sensitive properties. Lots of metal oxide nanostructures have been developed to improve the gas sensing properties such as sensitivity, selectivity, response speed, and so on. Here, we provide a brief overview of metal oxide nanostructures and their gas sensing properties from the aspects of particle size, morphology and doping. When the particle size of metal oxide is close to or less than double thickness of the space-charge layer, the sensitivity of the sensor will increase remarkably, which would be called “small size effect”, yet small size of metal oxide nanoparticles will be compactly sintered together during the film coating process which is disadvantage for gas diffusion in them. In view of those reasons, nanostructures with many kinds of shapes such as porous nanotubes, porous nanospheres and so on have been investigated, that not only possessed large surface area and relatively mass reactive sites, but also formed relatively loose film structures which is an advantage for gas diffusion. Besides, doping is also an effective method to decrease particle size and improve gas sensing properties. Therefore, the gas sensing properties of metal oxide nanostructures assembled by nanoparticles are reviewed in this article. The effect of doping is also summarized and finally the perspectives of metal oxide gas sensor are given. PMID:22736968

Metal oxide nanostructures and their gas sensing properties: a review.

PubMed

Sun, Yu-Feng; Liu, Shao-Bo; Meng, Fan-Li; Liu, Jin-Yun; Jin, Zhen; Kong, Ling-Tao; Liu, Jin-Huai

2012-01-01

Metal oxide gas sensors are predominant solid-state gas detecting devices for domestic, commercial and industrial applications, which have many advantages such as low cost, easy production, and compact size. However, the performance of such sensors is significantly influenced by the morphology and structure of sensing materials, resulting in a great obstacle for gas sensors based on bulk materials or dense films to achieve highly-sensitive properties. Lots of metal oxide nanostructures have been developed to improve the gas sensing properties such as sensitivity, selectivity, response speed, and so on. Here, we provide a brief overview of metal oxide nanostructures and their gas sensing properties from the aspects of particle size, morphology and doping. When the particle size of metal oxide is close to or less than double thickness of the space-charge layer, the sensitivity of the sensor will increase remarkably, which would be called "small size effect", yet small size of metal oxide nanoparticles will be compactly sintered together during the film coating process which is disadvantage for gas diffusion in them. In view of those reasons, nanostructures with many kinds of shapes such as porous nanotubes, porous nanospheres and so on have been investigated, that not only possessed large surface area and relatively mass reactive sites, but also formed relatively loose film structures which is an advantage for gas diffusion. Besides, doping is also an effective method to decrease particle size and improve gas sensing properties. Therefore, the gas sensing properties of metal oxide nanostructures assembled by nanoparticles are reviewed in this article. The effect of doping is also summarized and finally the perspectives of metal oxide gas sensor are given.

Coupling of HDPE/hydroxyapatite composites by silane-based methodologies.

PubMed

Sousa, R A; Reis, R L; Cunha, A M; Bevis, M J

2003-06-01

Several coupling treatments based on silane chemicals were investigated for the development of high density (HDPE)/hydroxyapatite (HA) composites. Two HA powders, sintered HA (HAs) and non sintered HA (HAns), were studied in combination with five silanes, namely y-methacryloxy propyltrimethoxy silane (MEMO), 3-(2-aminoethyl)aminopropyltrimethoxy silane (DAMO), vinyltrimethoxy silane (VTMO), 3-aminopropyltriethoxy silane (AMEO) and trimethoxypropyl silane (PTMO). The HA particles were treated by a dipping in method or by spraying with silane solutions. After drying, the treated powders were compounded with HDPE or HDPE with acrylic acid and/or organic peroxide and subsequently compression molded. The tensile test specimens obtained from the molded plates were tensile tested and their fracture surfaces were observed by scanning electron microscopy (SEM). For the sintered HA (HAs) composites, the most effective coupling treatments concerning stiffness are those based on MEMO and AMEO. The low influence of these coupling procedures on strength is believed to be associated to the low volume fraction and the relatively smooth surface of the used HA particles. For the non-sintered HA (HAns) composites, it was possible to improve significantly both the stiffness and the strength. Amino silanes demonstrated to be highly efficient concerning strength enhancement. The higher effectiveness of the coupling treatments for HAns filled composites is attributed to their higher particle surface area, smaller particle size distribution and expected higher chemical reactivity. For both cases, the improvement in mechanical performance after the coupling treatment is consistent with the enhancement in interfacial adhesion observed by SEM.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rager, Matthew S.; Aytug, Tolga; Veith, Gabriel M.

The developing field of printed electronics nanoparticle based inks such as CuO show great promise as a low-cost alternative to other metal-based counterparts (e.g., silver). In particular, CuO inks significantly eliminate the issue of particle oxidation, before and during the sintering process, that is prevalent in Cu-based formulations. We report here the scalable and low-thermal budget photonic fabrication of Cu interconnects employing a roll-to-roll compatible pulse-thermal-processing (PTP) technique that enables phase reduction and subsequent sintering of inkjet-printed CuO patterns onto flexible polymer templates. Detailed investigations of curing and sintering conditions were performed to understand the impact of PTP system conditionsmore » on the electrical performance of the Cu patterns. Specifically, the impact of energy and power of photonic pulses on print conductivity was systematically studied by varying the following key processing parameters: pulse intensity, duration and sequence. Through optimization of such parameters, highly conductive prints in < 1 s with resistivity values as low as 100 n m has been achieved. We also observed that the introduction of an initial ink-drying step in ambient atmosphere, after the printing and before sintering, leads to significant improvements in mechanical integrity and electrical performance of the printed Cu patterns. Moreover, the viability of CuO reactive inks, coupled with the PTP technology and pre ink-drying protocols, has also been demonstrated for the additive integration of a low-cost Cu temperature sensor onto a flexible polymer substrate.« less

Open-Source Selective Laser Sintering (OpenSLS) of Nylon and Biocompatible Polycaprolactone

PubMed Central

Paulsen, Samantha J.; Hwang, Daniel H.; Ta, Anderson H.; Yalacki, David R.; Schmidt, Tim; Miller, Jordan S.

2016-01-01

Selective Laser Sintering (SLS) is an additive manufacturing process that uses a laser to fuse powdered starting materials into solid 3D structures. Despite the potential for fabrication of complex, high-resolution structures with SLS using diverse starting materials (including biomaterials), prohibitive costs of commercial SLS systems have hindered the wide adoption of this technology in the scientific community. Here, we developed a low-cost, open-source SLS system (OpenSLS) and demonstrated its capacity to fabricate structures in nylon with sub-millimeter features and overhanging regions. Subsequently, we demonstrated fabrication of polycaprolactone (PCL) into macroporous structures such as a diamond lattice. Widespread interest in using PCL for bone tissue engineering suggests that PCL lattices are relevant model scaffold geometries for engineering bone. SLS of materials with large powder grain size (~500 μm) leads to part surfaces with high roughness, so we further introduced a simple vapor-smoothing technique to reduce the surface roughness of sintered PCL structures which further improves their elastic modulus and yield stress. Vapor-smoothed PCL can also be used for sacrificial templating of perfusable fluidic networks within orthogonal materials such as poly(dimethylsiloxane) silicone. Finally, we demonstrated that human mesenchymal stem cells were able to adhere, survive, and differentiate down an osteogenic lineage on sintered and smoothed PCL surfaces, suggesting that OpenSLS has the potential to produce PCL scaffolds useful for cell studies. OpenSLS provides the scientific community with an accessible platform for the study of laser sintering and the fabrication of complex geometries in diverse materials. PMID:26841023

Effects of Ceramic Density and Sintering Temperature on the Mechanical Properties of a Novel Polymer-Infiltrated Ceramic-Network Zirconia Dental Restorative (Filling) Material.

PubMed

Li, Weiyan; Sun, Jian

2018-05-10

BACKGROUND Polymer-infiltrated ceramic-network (PICN) dental material is a new and practical development in orthodontics. Sintering is the process of forming a stable solid mass from a powder by heating without melting. The aim of this study was to evaluate the effects of sintering temperature on the mechanical properties of a PICN zirconia dental material. MATERIAL AND METHODS A dense zirconia ceramic and four PICN zirconia dental materials, with varying porosities, were sintered at three different temperatures; 12 PICN zirconia dental materials based on these porous ceramics were prepared, as well as a pure polymer. After the specimen preparation, flexural strength and elastic modulus values were measured using the three-point bending test, and fracture toughness were determined by the single-edge notched beam (SENB) method. The Vickers hardness test method was used with an indentation strength (IS) test. Scanning electron microscopy (SEM) was used to examine the microstructure of the ceramic surface and the fracture surface. RESULTS Mechanical properties of the PICN dental materials, including flexural strength, elastic modulus, fracture toughness, and hardness, were more similar to the properties of natural teeth when compared with traditional dental ceramic materials, and were affected by the density and sintering temperature. SEM showed that the porous ceramic network became cohesive and that the length of cracks in the PICN dental material was reduced. CONCLUSIONS PICN zirconia dental materials were characterized by similar mechanical properties to natural dental tissues, but further studies are required continue to improve the similarities with natural human enamel and dentin.

Open-Source Selective Laser Sintering (OpenSLS) of Nylon and Biocompatible Polycaprolactone.

PubMed

Kinstlinger, Ian S; Bastian, Andreas; Paulsen, Samantha J; Hwang, Daniel H; Ta, Anderson H; Yalacki, David R; Schmidt, Tim; Miller, Jordan S

2016-01-01

Selective Laser Sintering (SLS) is an additive manufacturing process that uses a laser to fuse powdered starting materials into solid 3D structures. Despite the potential for fabrication of complex, high-resolution structures with SLS using diverse starting materials (including biomaterials), prohibitive costs of commercial SLS systems have hindered the wide adoption of this technology in the scientific community. Here, we developed a low-cost, open-source SLS system (OpenSLS) and demonstrated its capacity to fabricate structures in nylon with sub-millimeter features and overhanging regions. Subsequently, we demonstrated fabrication of polycaprolactone (PCL) into macroporous structures such as a diamond lattice. Widespread interest in using PCL for bone tissue engineering suggests that PCL lattices are relevant model scaffold geometries for engineering bone. SLS of materials with large powder grain size (~500 μm) leads to part surfaces with high roughness, so we further introduced a simple vapor-smoothing technique to reduce the surface roughness of sintered PCL structures which further improves their elastic modulus and yield stress. Vapor-smoothed PCL can also be used for sacrificial templating of perfusable fluidic networks within orthogonal materials such as poly(dimethylsiloxane) silicone. Finally, we demonstrated that human mesenchymal stem cells were able to adhere, survive, and differentiate down an osteogenic lineage on sintered and smoothed PCL surfaces, suggesting that OpenSLS has the potential to produce PCL scaffolds useful for cell studies. OpenSLS provides the scientific community with an accessible platform for the study of laser sintering and the fabrication of complex geometries in diverse materials.

Effects of Ceramic Density and Sintering Temperature on the Mechanical Properties of a Novel Polymer-Infiltrated Ceramic-Network Zirconia Dental Restorative (Filling) Material

PubMed Central

Li, Weiyan

2018-01-01

Background Polymer-infiltrated ceramic-network (PICN) dental material is a new and practical development in orthodontics. Sintering is the process of forming a stable solid mass from a powder by heating without melting. The aim of this study was to evaluate the effects of sintering temperature on the mechanical properties of a PICN zirconia dental material. Material/Methods A dense zirconia ceramic and four PICN zirconia dental materials, with varying porosities, were sintered at three different temperatures; 12 PICN zirconia dental materials based on these porous ceramics were prepared, as well as a pure polymer. After the specimen preparation, flexural strength and elastic modulus values were measured using the three-point bending test, and fracture toughness were determined by the single-edge notched beam (SENB) method. The Vickers hardness test method was used with an indentation strength (IS) test. Scanning electron microscopy (SEM) was used to examine the microstructure of the ceramic surface and the fracture surface. Results Mechanical properties of the PICN dental materials, including flexural strength, elastic modulus, fracture toughness, and hardness, were more similar to the properties of natural teeth when compared with traditional dental ceramic materials, and were affected by the density and sintering temperature. SEM showed that the porous ceramic network became cohesive and that the length of cracks in the PICN dental material was reduced. Conclusions PICN zirconia dental materials were characterized by similar mechanical properties to natural dental tissues, but further studies are required continue to improve the similarities with natural human enamel and dentin. PMID:29746449

Method of forming a relatively stable slip of silicon metal particles and yttrium containing particles

DOEpatents

Dickie, Ray A.; Mangels, John A.

1984-01-01

The method concerns forming a relatively stable slip of silicon metal particles and yttrium containing particles. In one embodiment, a casting slip of silicon metal particles is formed in water. Particles of a yttrium containing sintering aid are added to the casting slip. The yttrium containing sintering aid is a compound which has at least some solubility in water to form Y.sup.+3 ions which have a high potential for totally flocculating the silicon metal particles into a semiporous solid. A small amount of a fluoride salt is added to the casting slip which contains the yttrium containing sintering aid. The fluoride salt is one which will produce fluoride anions when dissolved in water. The small amount of the fluoride anions produced are effective to suppress the flocculation of the silicon metal particles by the Y.sup.+3 ions so that all particles remain in suspension in the casting slip and the casting slip has both an increased shelf life and can be used to cast articles having a relatively thick cross-section. The pH of the casting slip is maintained in a range from 7.5 to 9. Preferably, the fluoride salt used is one which is based on a monovalent cation such as sodium or ammonia. The steps of adding the yttrium containing sintering aid and the fluoride salt may be interchanged if desired, and the salt may be added to a solution containing the sintering aid prior to addition of the silicon metal particles.

Utilization of lignite power generation residues for the production of lightweight aggregates.

PubMed

Anagnostopoulos, Iason M; Stivanakis, Victor E

2009-04-15

A novel process is proposed for the utilization of lignite combustion solid residues in the production of inflammable lightweight aggregates (LWA). The process consists of two stages, pelletization and sintering, and carbon contained in BA was used as the process fuel. The main residues bottom ash (BA) and fly ash (FA) from Megalopolis power plant were characterized, mixed in different proportions and treated through pelletization and sintering process. Sintering benefits from combustion of BA carbon content and the product is a hardened porous cake. The energy required for achievement of high temperatures, in the range of 1250 degrees C, was offered by carbon combustion and CO(2) evolution is responsible for porous structure formation. Selected physical properties of sintered material relevant to use as lightweight aggregates were determined, including bulk density, porosity and water absorption. Bulk density varies from 0.83 to 0.91 g/cm(3), porosity varies from 60% to 64% and water absorption varies from 66% to 80%. LWA formed is used for the production of lightweight aggregate concrete (LWAC). Thermal conductivity coefficient varies from 0.25 to 0.37 W/mK (lower than maximum limit 0.43 W/mK) and compressive strength varies from 19 to 23 MPa (higher than minimum limit 17 MPa). The results indicate that sintering of lignite combustion residues is an efficient method of utilization of carbon containing BA and production of LWA for structural and insulating purposes. Carbon content of BA is a key factor in LWA production. Finally, this research work comprises the first proposed application for utilization of BA in Greece.

Preparation of UO2, ThO2 and (Th,U)O2 pellets from photochemically-prepared nano-powders

NASA Astrophysics Data System (ADS)

Pavelková, Tereza; Čuba, Václav; de Visser-Týnová, Eva; Ekberg, Christian; Persson, Ingmar

2016-02-01

Photochemically-induced preparation of nano-powders of crystalline uranium and/or thorium oxides and their subsequent pelletizing has been investigated. The preparative method was based on the photochemically induced formation of amorphous solid precursors in aqueous solution containing uranyl and/or thorium nitrate and ammonium formate. The EXAFS analyses of the precursors shown that photon irradiation of thorium containing solutions yields a compound with little long-range order but likely "ThO2 like" and the irradiation of uranium containing solutions yields the mixture of U(IV) and U(VI) compounds. The U-containing precursors were carbon free, thus allowing direct heat treatment in reducing atmosphere without pre-treatment in the air. Subsequent heat treatment of amorphous solid precursors at 300-550 °C yielded nano-crystalline UO2, ThO2 or solid (Th,U)O2 solutions with high purity, well-developed crystals with linear crystallite size <15 nm. The prepared nano-powders of crystalline oxides were pelletized without any binder (pressure 500 MPa), the green pellets were subsequently sintered at 1300 °C under an Ar:H2 (20:1) mixture (UO2 and (Th,U)O2 pellets) or at 1600 °C in ambient air (ThO2 pellets). The theoretical density of the sintered pellets varied from 91 to 97%.

Improvement of performance in low temperature solid oxide fuel cells operated on ethanol and air mixtures using Cu-ZnO-Al2O3 catalyst layer

NASA Astrophysics Data System (ADS)

Morales, M.; Espiell, F.; Segarra, M.

2015-10-01

Anode-supported single-chamber solid oxide fuel cells with and without Cu-ZnO-Al2O3 catalyst layers deposited on the anode support have been operated on ethanol and air mixtures. The cells consist of gadolinia-doped ceria electrolyte, Ni-doped ceria anode, and La0.6Sr0.4CoO3-δ-doped ceria cathode. Catalyst layers with different Cu-ZnO-Al2O3 ratios are deposited and sintered at several temperatures. Since the performance of single-chamber fuel cells strongly depends on catalytic properties of electrodes for partial oxidation of ethanol, the cells are electrochemically characterized as a function of the temperature, ethanol-air molar ratio and gas flow rate. In addition, catalytic activities of supported anode, catalytic layer-supported anode and cathode for partial oxidation of ethanol are analysed. Afterwards, the effect of composition and sintering temperature of catalyst layer on the cell performance are determined. The results indicate that the cell performance can be significantly enhanced using catalyst layers of 30:35:35 and 40:30:30 wt.% Cu-ZnO-Al2O3 sintered at 1100 °C, achieving power densities above 50 mW cm-2 under 0.45 ethanol-air ratio at temperatures as low as 450 °C. After testing for 15 h, all cells present a gradual loss of power density, without carbon deposition, which is mainly attributed to the partial re-oxidation of Ni at the anode.

Semiclassical law for the apparent viscosity of non-Newtonian fluids: An analogy between thixotropy of fluids and sintering of solids

NASA Astrophysics Data System (ADS)

Mezzasalma, Stefano A.

2000-08-01

A theory is presented to describe the apparent viscosity of thixotropic fluids as a function of the rate of shear. It represents the extension of a semiclassical approach that was previously formulated to deal with matter densification phenomena in solids starting from the state equation of the medium. In this context, the Debye expression for the Helmholtz free energy has been provided with a density of vibrational modes that accounts for atomic and microstructural changes occurring at the frequency scale of momentum transport (see diffusion). Working out the steady-state condition with respect to time gives an equation relating reduced apparent viscosity (η˜) and shear rate (γ˜) through the temperature value (θ*) that is energetically equivalent to the medium vibrations implied. Viscosity also turns out to depend on the Debye temperature θD (see φ˜θ*/θD) and an equivalent Gruneisen parameter (μ), defined with respect to viscosity variations. Increasing φ in pseudoplastic and dilatant media, respectively, increases and decreases η˜, which always increases with increasing μ. The analogy between dilatancy/sintering and pseudoplasticity/desintering is suggested, and a correspondence between matter and momentum transports is traced on the basis of the phononic spectrum properties. Application to experimental measurements are presented and discussed for aqueous monodispersions of polystyrene (PS) latex particles, aqueous glycerol solutions of partially hydrolyzed polyacrylamide (PHPAA) at different sodium chloride (NaCl) concentrations, polymethylmethacrylate (PMMA) suspensions in dioctylphthalate (DOP), and for a molecularly thin liquid film of octamethylciclotetrasiloxane (OMCTS). Best fit coefficients for φ and μ have been constrained to the Debye temperature and the effective low-shear viscosity (η0) according to their dependences upon the suspended volume fraction (φ), θD=θD(φ), and η0=η0(φ), and the agreement with experimental data is quite satisfactory in all cases here examined. It is then suggested that the viscous character of a liquid can be described in terms of a coupling between Brownian diffusion and phonon wave motion.

Exotic species with explicit noble metal-noble gas-noble metal linkages.

PubMed

Moreno, Norberto; Restrepo, Albeiro; Hadad, C Z

2018-02-14

We present a study of the isoelectronic Pt 2 Ng 2 F 4 and [Au 2 Ng 2 F 4 ] 2+ species with noble gas atoms (Ng = Kr, Xe, Rn) acting as links bridging the two noble metal atoms. The stability of the species is investigated using several thermodynamic, kinetic and reactivity indicators. The results are compared against [AuXe 4 ] 2+ , which is thermodynamically unstable in the gas phase but is stabilized in the solid state to the point that it has been experimentally detected as [AuXe 4 ](Sb 2 F 11 ) 2 (S. Seidel and K. Seppelt, Science, 2000, 290, 117-118). Our results indicate that improving upon [AuXe 4 ] 2+ , these exotic combinations between the a priori non-reactive noble metals and noble gases lead to metastable species, and, therefore, they have the possibility of existing in the solid state under adequate conditions. Our calculations include accurate energies and geometries at both the CCSD/SDDALL and MP2/SDDALL levels. We offer a detailed description of the nature of the bonding interactions using orbital and density-based analyses. The computational evidence suggests partially covalent and ionic interactions as the stabilization factors.

Production of Conidia by the Fungus Metarhizium anisopliae Using Solid-State Fermentation.

PubMed

Loera-Corral, Octavio; Porcayo-Loza, Javier; Montesinos-Matias, Roberto; Favela-Torres, Ernesto

2016-01-01

This chapter describes the production of conidia by Metarhizium anisopliae using solid-state fermentation. Before production of conidia, procedures for strains conservation, reactivation, and propagation are essential in order to provide genetic stability of the strains. The strain is conserved in freeze-dried vials and then reactivated through insect inoculation. Rice is used as a substrate for the conidia production in two different bioreactors: plastic bags and tubular bioreactor. The CO2 production in the tubular bioreactors is measured with a respirometer; this system allows calculating indirect growth parameters as lag time (tlag) (25-35 h), maximum rate of CO2 production (rCO2 max) (0.5-0.7 mg/gdm h), specific rate of CO2 production (μ) (0.10-0.15 1/h), and final CO2 production (CO2) (100-120 mg/gdm). Conidial yield per gram of dry substrate (gdm) should be above 1 × 10(9) conidia/gdm after 10 days of incubation. Germination and viability of conidia obtained after 10 days of incubation should be above 80 % and 75 %, respectively. Bioassays using of Tenebrio molitor as a host insect should yield a final mortality above 80 %.

Preparation and evaluation of thin-film sodium tungsten bronzes

NASA Technical Reports Server (NTRS)

Kautz, H. E.; Fielder, W. L.; Singer, J.; Fordyce, J. S.

1974-01-01

Thin films of sodium tungsten bronze (NaxWO3) were investigated as reversible sodium ion electrodes for solid electrolytes. The films were made by electron beam evaporation of the three phases, W metal, Na2WO4, and WO3, followed by sintering. The substrates were sodium beta alumina disks and glass slides. X-ray diffraction analyses of the films showed that sintering in dry nitrogen with prior exposure to air lead to mixed phases. Sintering in vacuum with no air exposure produced tetragonal I bronze with a nominal composition of Na0.31WO3, single phase within the limits of X-ray diffraction detectability. The films were uniform and adherent on sodium beta alumina substrates. The ac and dc conductivities of the beta alumina were measured with the sodium tungsten bronze films as electrodes. These experiments indicated that the tetragonal I bronze electrodes were not completely reversible. This may have resulted from sodium ion blocking within the bronze film or at the bronze beta alumina interface. Methods for attempting to make more completely reversible electrodes are suggested.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hanc, Emil; Zając, Wojciech, E-mail: wojciech.zajac@agh.edu.pl; Lu, Li

Ceramic oxides exhibiting high lithium-ion mobility at room temperature receive broad attention as candidate electrolytes for lithium batteries. Lithium-stuffed garnets from the Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} group seem to be especially promising because of their high ionic conductivity at room temperature and their electrochemical stability. In this work, we discuss factors that affect formation of the garnet in its bulk form or in the form of thick and thin films. We demonstrate that zinc oxide can be applied as a sintering aid that facilitate the formation of the highly conducting cubic Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} garnet phase inmore » a single-step sintering procedure. Based on our experience with the single-step sintering experiments, we successfully fabricated a thick-film membrane consisting of a garnet solid electrolyte using the tape casting technique. In order to reduce the thickness of the electrolyte even further we investigated the fabrication of a thin-film Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} electrolyte by means of the pulsed laser deposition technique.« less

Phase Evolution and Mechanical Properties of AlCoCrFeNiSi x High-Entropy Alloys Synthesized by Mechanical Alloying and Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Kumar, Anil; Swarnakar, Akhilesh Kumar; Chopkar, Manoj

2018-05-01

In the current investigation, AlCoCrFeNiSi x (x = 0, 0.3, 0.6 and 0.9 in atomic ratio) high-entropy alloy systems are prepared by mechanical alloying and subsequently consolidated by spark plasma sintering. The microstructural and mechanical properties were analyzed to understand the effect of Si addition in AlCoCrFeNi alloy. The x-ray diffraction analysis reveals the supersaturated solid solution of the body-centered cubic structure after 20 h of ball milling. However, the consolidation promotes the transformation of body-centered phases partially into the face-centered cubic structure and sigma phases. A recently proposed geometric model based on the atomic stress theory has been extended for the first time to classify single phase and multi-phases on the high-entropy alloys prepared by mechanical alloying and spark plasma sintering process. Improved microhardness and better wear resistance were achieved as the Si content increased from 0 to 0.9 in the present high-entropy alloy.

Engineering and environmental properties of thermally treated mixtures containing MSWI fly ash and low-cost additives.

PubMed

Polettini, A; Pomi, R; Trinci, L; Muntoni, A; Lo Mastro, S

2004-09-01

An experimental work was carried out to investigate the feasibility of application of a sintering process to mixtures composed of Municipal Solid Waste Incinerator (MSWI) fly ash and low-cost additives (waste from feldspar production and cullet). The proportions of the three constituents were varied to adjust the mixture compositions to within the optimal range for sintering. The material was compacted in cylindrical specimens and treated at 1100 and 1150 degrees C for 30 and 60 min. Engineering and environmental characteristics including weight loss, dimensional changes, density, open porosity, mechanical strength, chemical stability and leaching behavior were determined for the treated material, allowing the relationship between the degree of sintering and both mixture composition and treatment conditions to be singled out. Mineralogical analyses detected the presence of neo-formation minerals from the pyroxene group. Estimation of the extent of metal loss from the samples indicated that the potential for volatilization of species of Pb, Cd and Zn is still a matter of major concern when dealing with thermal treatment of incinerator ash.

On fabrication procedures of Li-ion conducting garnets

NASA Astrophysics Data System (ADS)

Hanc, Emil; Zając, Wojciech; Lu, Li; Yan, Binggong; Kotobuki, Masashi; Ziąbka, Magdalena; Molenda, Janina

2017-04-01

Ceramic oxides exhibiting high lithium-ion mobility at room temperature receive broad attention as candidate electrolytes for lithium batteries. Lithium-stuffed garnets from the Li7La3Zr2O12 group seem to be especially promising because of their high ionic conductivity at room temperature and their electrochemical stability. In this work, we discuss factors that affect formation of the garnet in its bulk form or in the form of thick and thin films. We demonstrate that zinc oxide can be applied as a sintering aid that facilitate the formation of the highly conducting cubic Li7La3Zr2O12 garnet phase in a single-step sintering procedure. Based on our experience with the single-step sintering experiments, we successfully fabricated a thick-film membrane consisting of a garnet solid electrolyte using the tape casting technique. In order to reduce the thickness of the electrolyte even further we investigated the fabrication of a thin-film Li7La3Zr2O12 electrolyte by means of the pulsed laser deposition technique.

Experimental and simulation studies on grain growth in TiC and WC-based cermets during liquid phase sintering

NASA Astrophysics Data System (ADS)

Shin, Soon-Gi

2000-06-01

The grain growth behaviors of TiC and WC particles in TiC-Ni, TiC-Mo2C-Ni, WC-Co and WC-VC-Co alloys during liquid phase sintering were investigated for different Ni or Co contents and compared with the results of Monte Carlo simulations. In the experimental study, TiC-Ni and WC-Co alloys had a maximum grain size at a certain liquid volume fraction, while the grain size in TiC-Mo2C-Ni and WC-VC-Co alloys increased monotonically with an increasing liquid volume fraction. These results mean that the grain growth of these alloys cannot be explained by the conventional mechanisms for Ostwald ripening, namely diffusion or reaction controlled processes. Monte Carlo simulations with different energy relationships between solidliquid interfaces predicted the effect of the liquid volume fraction on grain size similar to the experimental results. The contiguous boundaries between solid (carbide) particles appear to influence the grain growth behavior in TiC- and WC-based alloys during liquid phase sintering.

Hot pressing and lithification of gouge during the Mount St. Helens 2004-2008 eruption: insights from high temperature deformation experiments

NASA Astrophysics Data System (ADS)

Ryan, Amy G.; Russell, James K.; Heap, Michael J.

2017-04-01

We present results from an experimental program designed to investigate the timescales, conditions and mechanisms responsible for the densification and lithification of volcanic gouge at Mount St. Helens (MSH). From 2004-2008, MSH produced a series of lava domes/spines that were mantled by thick layers of gouge resulting from fracturing and cataclasis at the conduit-wall rock interface. The gouge comprises fine crystal-rich rock powder containing little to no glass. The erupted gouge carapace is texturally diverse, and varies from loose granular material to moderately indurated coherent rock to fine-grained cataclasite within tens of centimeters. The spatial association of these materials suggests that the originally unconsolidated conduit-fault gouge is densified and lithified during ascent to the surface. At present the conditions, timescales and mechanisms for lithification of the glass-poor materials are unknown. Here, we present results from a series of high-temperature (T) uniaxial deformation experiments performed on natural gouge collected from MSH (spine 5). The experiments are intended to (1) establish the feasibility of experimentally densifying/lithifying natural gouge materials at laboratory conditions approximating those within the MSH conduit, and to (2) constrain the effects of T, load and time on the extents, rates and mechanisms of densification. Our experimental conditions include T up to 800°C (T

Computational methods for reactive transport modeling: An extended law of mass-action, xLMA, method for multiphase equilibrium calculations

NASA Astrophysics Data System (ADS)

Leal, Allan M. M.; Kulik, Dmitrii A.; Kosakowski, Georg; Saar, Martin O.

2016-10-01

We present an extended law of mass-action (xLMA) method for multiphase equilibrium calculations and apply it in the context of reactive transport modeling. This extended LMA formulation differs from its conventional counterpart in that (i) it is directly derived from the Gibbs energy minimization (GEM) problem (i.e., the fundamental problem that describes the state of equilibrium of a chemical system under constant temperature and pressure); and (ii) it extends the conventional mass-action equations with Lagrange multipliers from the Gibbs energy minimization problem, which can be interpreted as stability indices of the chemical species. Accounting for these multipliers enables the method to determine all stable phases without presuming their types (e.g., aqueous, gaseous) or their presence in the equilibrium state. Therefore, the here proposed xLMA method inherits traits of Gibbs energy minimization algorithms that allow it to naturally detect the phases present in equilibrium, which can be single-component phases (e.g., pure solids or liquids) or non-ideal multi-component phases (e.g., aqueous, melts, gaseous, solid solutions, adsorption, or ion exchange). Moreover, our xLMA method requires no technique that tentatively adds or removes reactions based on phase stability indices (e.g., saturation indices for minerals), since the extended mass-action equations are valid even when their corresponding reactions involve unstable species. We successfully apply the proposed method to a reactive transport modeling problem in which we use PHREEQC and GEMS as alternative backends for the calculation of thermodynamic properties such as equilibrium constants of reactions, standard chemical potentials of species, and activity coefficients. Our tests show that our algorithm is efficient and robust for demanding applications, such as reactive transport modeling, where it converges within 1-3 iterations in most cases. The proposed xLMA method is implemented in Reaktoro, a unified open-source framework for modeling chemically reactive systems.

A micro-macro coupling approach of MD-SPH method for reactive energetic materials

NASA Astrophysics Data System (ADS)

Liu, Gui Rong; Wang, Guang Yu; Peng, Qing; De, Suvranu

2017-01-01

The simulation of reactive energetic materials has long been the interest of researchers because of the extensive applications of explosives. Much research has been done on the subject at macro scale in the past and research at micro scale has been initiated recently. Equation of state (EoS) is the relation between physical quantities (pressure, temperature, energy and volume) describing thermodynamic states of materials under a given set of conditions. It plays a significant role in determining the characteristics of energetic materials, including Chapman-Jouguet point and detonation velocity. Furthermore, EoS is the key to connect microscopic and macroscopic phenomenon when simulating the macro effects of an explosion. For instance, an ignition and growth model for high explosives uses two JWL EoSs, one for solid explosive and the other for gaseous products, which are often obtained from experiments that can be quite expensive and hazardous. Therefore, it is ideal to calculate the EoS of energetic materials through computational means. In this paper, the EoSs for both solid and gaseous products of β-HMX are calculated using molecular dynamics simulation with ReaxFF-d3, a reactive force field obtained from quantum mechanics. The microscopic simulation results are then compared with experiments and the continuum ignition and growth model. Good agreement is observed. Then, the EoSs obtained through micro-scale simulation is applied in a smoothed particle hydrodynamics (SPH) code to simulate the macro effects of explosions. Simulation results are compared with experiments.

Hydrothermal Cold Sintering

NASA Astrophysics Data System (ADS)

Kang, Xiaoyu

Solid state sintering transforms particle compact to a physically robust and dense polycrystalline monolith driven by reduction of surface energy and curvature. Since bulk diffusion is required for neck formation and pore elimination, sintering temperature about 2/3 of melting point is needed. It thus places limitations for materials synthesis and integration, and contributes to significant energy consumption in ceramic processing. Furthermore, since surface transport requires lower temperature than bulk processes, grain growth is often rapid and can be undesired for physical properties. For these reasons, several techniques have been developed including Liquid Phase Sintering (LPS), Hot Pressing (HP) and Field Assisted Sintering Technique (FAST), which introduce either viscous melt, external pressure or electric field to speed up densification rates at lower temperature. However, because of their inherent reliability on bulk diffusion, temperatures required are often too high for integrating polymers and non-noble metals. Reduction of sintering temperature below 400 °C would require a different densification mechanism that is based on surface transport with external forces to drive volume shrinkage. Densification method combining uniaxial pressure and solution under hydrothermal condition was first demonstrated by Kanahara's group at Kochi University in 1986 and was brought to our attention by the work of Kahari, etc, from University of Oulu on densification of Li2MoO 4 in 2015. This relatively new process showed promising ultra-low densification temperature below 300 °C, however little was known about its fundamental mechanism and scope of applications, which became the main focus of this dissertation. In this work, a uniaxial hydraulic press, a standard stainless steel 1/2 inch diameter die with heating band were utilized in densifying metal oxides. Applied pressure and sintering temperature were between 100 MPa and 700 MPa and from room temperature to 300 °C, respectively. Process variables were defined and effects of individual parameters were studied systematically through control variable method with Li2MoO4-water system. Crystalline structure, fractured surface morphology and chemical bonding information of the cold sintered pellets were studied with X-ray diffraction (XRD), field effect scanning electron microscopy (FE-SEM) and Raman spectroscopy, etc. Densification mechanism studies were conducted on ZnO. Through comparison experiments, it was found that the Zn2+ concentration in the solution is critical for densification, while dissolution of grains only serves as a means to the former. Through pressure dependent studies, a critical value was found, which correlated well with the hydrostatic pressure keeping liquid water from thermal expansion. These results confirmed establishment of hydrothermal condition that would be important for mass transport in densification. Densification rate variations with process time was estimated and similar time dependence to Kingery's model was found. The densification process was proposed to be consist of three consecutive stages, which are quick initial compaction, grain rearrangement and dissolution-reprecipitation events. Binary metal oxides with different acidities were subjected to cold sintering with various aqueous solutions in establishing a criteria for material selection. It was found that in general materials with high solubility at around neutral pH, high dissolution kinetics and similar free energy to their hydroxides or hydrates at ambient would be more likely for full densification with high phase purity. The anions in solution should also be wisely selected to avoid stable compound or complex formation. To extend the applicable material list for full densification, non-aqueous solvent of dimethyl sulfoxide (DMSO) based solution was studied for cold sintering. Both improvement of pellet density and suppression of hydroxide formation were achieved for MnO by using DMSO-HOAc solution. With this strategy, densification of other metal oxides with strong hydroxide formation may also be improved, for example oxides of alkaline earth and many transition metals. Finally, the author's previous work on Zn1-xMg xO thin films is included in Chapter 7.