Effect of sintering conditions on the electrical-transport properties of the SrZrO3-based protonic ceramic electrolyser membrane

NASA Astrophysics Data System (ADS)

Heras-Juaristi, Gemma; Pérez-Coll, Domingo; Mather, Glenn C.

2016-11-01

The effects of sintering temperature and addition of 4 mol.% ZnO as sintering additive on the crystal structure, microstructure and electrical properties of SrZr0.9Y0.1O3-δ are reported. The presence of ZnO as sintering aid brings about high densification at 1300 °C (relative density ∼97%); gas-tightness is not achieved for ZnO-free samples sintered below 1600 °C. Bulk conductivity (σB) is considerably higher in wet and dry O2 on doping with ZnO, but only slight variations of σB with sintering temperature are observed for the Zn-containing phases. Similarly, the apparent grain-boundary conductivities are much greater for the Zn-doped samples. The grain-boundary volume and accompanying resistances are much reduced on sintering at 1500 °C with ZnO addition in comparison to Zn-modified samples sintered below 1500 °C, with only minor changes in grain-boundary relaxation frequency observed. Conversely, in comparison to the undoped sample with sintering temperature of 1600 °C, there is an enormous improvement in the specific grain-boundary conductivity of two orders of magnitude for the ZnO-containing samples. Analysis on the basis of the core space-charge-layer model relates the enhancement of the grain-boundary transport to a higher concentration of charge carriers in the space-charge layer and associated lower potential barrier heights.

Two-Step Reactive Aid Sintering of BaZr0.8Y0.2O3- δ Proton-Conducting Ceramics

NASA Astrophysics Data System (ADS)

Wang, Siwei; Chen, Yan; Zhang, Lingling; Ren, Cong; Chen, Fanglin; Brinkman, Kyle S.

2015-12-01

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr0.8Y0.2O3- δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. In this paper, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO3 and B2O3-Li2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improved to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. The bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.

Two-Step Reactive Aid Sintering of BaZr 0.8Y 0.2O 3-δ Proton-Conducting Ceramics

DOE PAGES

Wang, Siwei; Chen, Yan; Zhang, Lingling; ...

2015-10-14

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. Here, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improvedmore » to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. Moreover, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less

Size-dependent disproportionation (in 2-20 nm regime) and hybrid Bond Valence derived interatomic potentials for BaTaO2N

NASA Astrophysics Data System (ADS)

Anbalagan, Kousika; Thomas, Tiju

2018-05-01

Interatomic potentials for complex materials (like ceramic systems) are important for realistic molecular dynamics (MD) simulations. Such simulations are relevant for understanding equilibrium, transport and dynamical properties of materials, especially in the nanoregime. Here we derive a hybrid interatomic potential (based on bond valence (BV) derived Morse and Coulomb terms), for modeling a complex ceramic, barium tantalum oxynitride (BaTaO2N). This material has been chosen due to its relevance for capacitive and photoactive applications. However, the material presents processing challenges such as the emergence of non-stoichiometric phases during processing, demonstrating complex processing-property correlations. This makes MD investigations of this material both scientifically and technologically relevant. The BV based hybrid potential presented here has been used for simulating sintering of BaTaO2N nanoparticles ( 2-20 nm) under different conditions (using the relevant canonical ensemble). Notably, we show that sintering of particles of diameter < 10 nm requires no external sintering aids such as the addition of barium sources (since stoichiometry is preserved during heat treatment in this size regime). Also, we observe that sintering of particles > 10 nm in size results in the formation of a cluster of tantalum and oxygen atoms at the interface of the BaTaO2N particles. This is in agreement with the experimental reports. The results presented here suggest that the potential proposed can be used to explore dynamical properties of BaTaO2N and related systems. This work will also open avenues for development of nanoscience-enabled aid-free sintering approaches to this and related materials.

Zirconia changes after grinding and regeneration firing.

PubMed

Hatanaka, Gabriel R; Polli, Gabriela S; Fais, Laiza M G; Reis, José Maurício Dos S N; Pinelli, Lígia A P

2017-07-01

Despite improvements in computer-aided design and computer-aided manufacturing (CAD-CAM) systems, grinding during either laboratory procedures or clinical adjustments is often needed to modify the shape of 3 mol(%) yttria-tetragonal zirconia polycrystal (3Y-TZP) restorations. However, the best way to achieve adjustment is unclear. The purpose of this in vitro study was to evaluate the microstructural and crystallographic phase changes, flexural strength, and Weibull modulus of a 3Y-TZP zirconia after grinding with or without water cooling and regeneration firing. Ninety-six bar-shaped specimens were obtained and divided as follows: as-sintered, control; as-sintered with regeneration firing; grinding without water cooling; grinding and regeneration firing with water cooling; and grinding and regeneration firing. Grinding (0.3 mm) was performed with a 150-μm diamond rotary instrument in a high-speed handpiece. For regeneration firing, the specimens were annealed at 1000°C for 30 minutes. The crystalline phases were evaluated by using x-ray powder diffraction. A 4-point bending test was conducted (10 kN; 0.5 mm/min). The Weibull modulus was used to analyze strength reliability. The microstructure was analyzed by scanning electron microscopy. Data from the flexural strength test were evaluated using the Kruskal-Wallis and Dunn tests (α=.05). Tetragonal-to-monoclinic phase transformation was identified in the ground specimens; R regeneration firing groups showed only the tetragonal phase. The median flexural strength of as-sintered specimens was 642.0; 699.3 MPa for as-sintered specimens with regeneration firing; 770.1 MPa for grinding and water-cooled specimens; 727.3 MPa for specimens produced using water-cooled grinding and regeneration firing; 859.9 MPa for those produced by grinding; and 764.6 for those produced by grinding and regeneration firing; with statistically higher values for the ground groups. The regenerative firing did not affect the flexural strength. Weibull modulus values ranged from 5.3 to 12.4. The SEM images showed semicircular cracks after grinding. Adjustments by grinding in 3Y-TZP frameworks should be performed with water cooling, and regeneration firing should be undertaken to obtain a more reliable material. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Pressureless sintering of whisker-toughened ceramic composites

DOEpatents

Tiegs, T.N.

1993-05-04

A pressureless sintering method is disclosed for use in the production of whisker-toughened ceramic composites wherein the sintered density of composites containing up to about 20 vol. % SiC whiskers is improved by reducing the average aspect ratio of the whiskers to from about 10 to about 20. Sintering aids further improve the density, permitting the production of composites containing 20 vol. % SiC with sintered densities of 94% or better of theoretical density by a pressureless sintering method.

Pressureless sintering of whiskered-toughened ceramic composites

DOEpatents

Tiegs, Terry N.

1994-01-01

A pressureless sintering method is disclosed for use in the production of whisker-toughened ceramic composites wherein the sintered density of composites containing up to about 20 vol. % SiC whiskers is improved by reducing the average aspect ratio of the whiskers to from about 10 to about 20. Sintering aids further improve the density, permitting the production of composites containing 20 vol. % SiC with sintered densities of 94% or better of theoretical density by a pressureless sintering method.

Pressureless sintering of whisker-toughened ceramic composites

DOEpatents

Tiegs, Terry N.

1993-01-01

A pressureless sintering method is disclosed for use in the production of whisker-toughened ceramic composites wherein the sintered density of composites containing up to about 20 vol. % SiC whiskers is improved by reducing the average aspect ratio of the whiskers to from about 10 to about 20. Sintering aids further improve the density, permitting the production of composites containing 20 vol. % SiC with sintered densities of 94% or better of theoretical density by a pressureless sintering method.

High energy product permanent magnet having improved intrinsic coercivity and method of making same

DOEpatents

Ramesh, Ramamoorthy; Thomas, Gareth

1990-01-01

A high energy rare earth-ferromagnetic metal permanent magnet is disclosed which is characterized by improved intrinsic coercivity and is made by forming a particulate mixture of a permanent magnet alloy comprising one or more rare earth elements and one or more ferromagnetic metals and forming a second particulate mixture of a sintering alloy consisting essentially of 92-98 wt. % of one or more rare earth elements selected from the class consisting of Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and mixtures of two or more of such rare earth elements, and 2-8 wt. % of one or more alloying metals selected from the class consisting of Al, Nb, Zr, V, Ta, Mo, and mixtures of two or more of such metals. The permanent magnet alloy particles and sintering aid alloy are mixed together and magnetically oriented by immersing the mixture in an axially aligned magnetic field while cold pressing the mixture. The compressed mixture is then sintered at a temperature above the melting point of the sintering aid and below the melting point of the permanent magnet alloy to thereby coat the particle surfaces of the permanent magnetic alloy particles with the sintering aid while inhibiting migration of the rare earth element in the sintering aid into the permanent magnet alloy particles to thereby raise the intrinsic coercivity of the permanent magnet alloy without substantially lowering the high energy of the permanent magnet alloy.

Pressureless sintering of whiskered-toughened ceramic composites

DOEpatents

Tiegs, T.N.

1994-12-27

A pressureless sintering method is disclosed for use in the production of whisker-toughened ceramic composites wherein the sintered density of composites containing up to about 20 vol. % SiC whiskers is improved by reducing the average aspect ratio of the whiskers to from about 10 to about 20. Sintering aids further improve the density, permitting the production of composites containing 20 vol. % SiC with sintered densities of 94% or better of theoretical density by a pressureless sintering method. 6 figures.

Is cell viability always directly related to corrosion resistance of stainless steels?

PubMed

Salahinejad, E; Ghaffari, M; Vashaee, D; Tayebi, L

2016-05-01

It has been frequently reported that cell viability on stainless steels is improved by increasing their corrosion resistance. The question that arises is whether human cell viability is always directly related to corrosion resistance in these biostable alloys. In this work, the microstructure and in vitro corrosion behavior of a new class of medical-grade stainless steels were correlated with adult human mesenchymal stem cell viability. The samples were produced by a powder metallurgy route, consisting of mechanical alloying and liquid-phase sintering with a sintering aid of a eutectic Mn-Si alloy at 1050 °C for 30 and 60 min, leading to nanostructures. In accordance with transmission electron microscopic studies, the additive particles for the sintering time of 30 min were not completely melted. Electrochemical impedance spectroscopic experiments suggested the higher corrosion resistance for the sample sintered for 60 min; however, a better cell viability on the surface of the less corrosion-resistant sample was unexpectedly found. This behavior is explained by considering the higher ion release rate of the Mn-Si additive material, as preferred sites to corrosion attack based on scanning electron microscopic observations, which is advantageous to the cells in vitro. In conclusion, cell viability is not always directly related to corrosion resistance in stainless steels. Typically, the introduction of biodegradable and biocompatible phases to biostable alloys, which are conventionally anticipated to be corrosion-resistant, can be advantageous to human cell responses similar to biodegradable metals. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Process for fabrication of large titanium diboride ceramic bodies

DOEpatents

Moorhead, Arthur J.; Bomar, E. S.; Becher, Paul F.

1989-01-01

A process for manufacturing large, fully dense, high purity TiB.sub.2 articles by pressing powders with a sintering aid at relatively low temperatures to reduce grain growth. The process requires stringent temperature and pressure applications in the hot-pressing step to ensure maximum removal of sintering aid and to avoid damage to the fabricated article or the die.

Amino Acids Aided Sintering for the Formation of Highly Porous FeAl Intermetallic Alloys

PubMed Central

Karczewski, Krzysztof; Stepniowski, Wojciech J.

2017-01-01

Fabrication of metallic foams by sintering metal powders mixed with thermally degradable compounds is of interest for numerous applications. Compounds releasing gaseous nitrogen, minimizing interactions between the formed gases and metallic foam by diluting other combustion products, were applied. Cysteine and phenylalanine, were used as gas releasing agents during the sintering of elemental Fe and Al powders in order to obtain metallic foams. Characterization was carried out by optical microscopy with image analysis, scanning electron microscopy with energy dispersive spectroscopy, and gas permeability tests. Porosity of the foams was up to 42 ± 3% and 46 ± 2% for sintering conducted with 5 wt % cysteine and phenylalanine, respectively. Chemical analyses of the formed foams revealed that the oxygen content was below 0.14 wt % and the carbon content was below 0.3 wt %. Therefore, no brittle phases could be formed that would spoil the mechanical stability of the FeAl intermetallic foams. The gas permeability tests revealed that only the foams formed in the presence of cysteine have enough interconnections between the pores, thanks to the improved air flow through the porous materials. The foams formed with cysteine can be applied as filters and industrial catalysts. PMID:28773106

Improvement of the stability of hydroxyapatite through glass ceramic reinforcement.

PubMed

Ha, Na Ra; Yang, Zheng Xun; Hwang, Kyu Hong; Kim, Tae Suk; Lee, Jong Kook

2010-05-01

Hydroxyapatite has achieved significant application in orthopedic and dental implants due to its excellent biocompatibility. Sintered hydroxyapatites showed significant dissolution, however, after their immersion in water or simulated body fluid (SBF). This grain boundary dissolution, even in pure hydroxyapatites, resulted in grain separation at the surfaces, and finally, in fracture. In this study, hydroxyapatite ceramics containing apatite-wollastonite (AW) or calcium silicate (SG) glass ceramics as additives were prepared to prevent the dissolution. AW and SG glass ceramics were added at 0-7 wt% and powder-compacted uniaxially followed by firing at moisture conditions. The glass phase was incorporated into the hydroxyapatite to act as a sintering aid, followed by crystallization, to improve the mechanical properties without reducing the biocompatibility. As seen in the results of the dissolution test, a significant amount of damage was reduced even after more than 14 days. TEM and SEM showed no decomposition of HA to the secondary phase, and the fracture toughness increased, becoming even higher than that of the commercial hydroxyapatite.

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.

Gadolinium doped ceria interlayers for Solid Oxide Fuel Cells cathodes: Enhanced reactivity with sintering aids (Li, Cu, Zn), and improved densification by infiltration

NASA Astrophysics Data System (ADS)

Nicollet, Clement; Waxin, Jenny; Dupeyron, Thomas; Flura, Aurélien; Heintz, Jean-Marc; Ouweltjes, Jan Pieter; Piccardo, Paolo; Rougier, Aline; Grenier, Jean-Claude; Bassat, Jean-Marc

2017-12-01

This paper reports the study of the densification of 20% Gd doped ceria (Ce0.8Gd0.2O1.9 (GDC)) interlayers in SOFC cathodes through two different routes: the well-known addition of sintering elements, and an innovative densification process by infiltration. First, Li, Cu, and Zn nitrates were added to GDC powders. The effect of these additives on the densification was studied by dilatometry on pellets, and show a large decrease of the sintering temperature from 1330 °C (pure GDC), down to 1080 °C, 950 °C, and 930 °C for Zn, Cu, and Li addition, respectively. However, this promising result does not apply to screen-printed layers, which are more porous than pellets and in which the shrinkage is constrained by the substrate. The second approach consists in preparing a pre-sintered GDC layer, which is subsequently infiltrated with Ce and Gd nitrates and sintered at 1250 °C to increase its density. Such an approach results in highly dense GDC interlayers. Using La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF) as electrode, the influence of the interlayers on the cathode performance was studied. The addition of sintering aids dramatically increases the cell resistances, most likely because the additives increase the reactivity between GDC and either Yttria Stabilized Zirconia (YSZ) or LSCF, thus losing the expected benefit related to the decrease of sintering temperatures. The interlayers prepared by infiltration do not induce additional resistances in the cell, which results in power densities of single cells 40-50% higher than those of cells prepared with commercial GDC interlayers, making this approach a valuable alternative to sintering aids.

Sintered silicon carbide molded body and method for its production

NASA Technical Reports Server (NTRS)

Omori, M.; Sendai, M.; Ohira, K.

1984-01-01

Sintered silicon carbide shapes are described. They are produced by using a composition containing an oxide of at least one element chosen from the group: Li, Be, Mg, Si, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Zn, Nb, Mo, Ba, Tc, Ta, W and Th as a supplement to known sintering aids.

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.

Effects of Dopant on the Dielectric Properties of CaZrO3 Ceramic Sintered in a Reducing Atmosphere

NASA Astrophysics Data System (ADS)

Lee, W. S.; Su, C. Y.; Lee, Y. C.; Lin, S. P.; Yang, Tony

2006-07-01

In this study, the influence of CaZrO3 doped with three dopants, SiO2, MnO, and Nb2O5, and then sintered in a reducing atmosphere on microstructure, phase formation, and electrical properties is investigated. SiO2 plays the role of sintering aid to enhance the density of CaZrO3 leading to better performance of electrical properties as a function of SiO2 content. MnO, and Nb2O5 were incorporated into the Zr-site of CaZrO3 to make stoichometric CaZrO3 into non-stoichiometric CaZrO3 with Zr excess resulting in the formation of a second phase, CaZr4O9, which has a lower dielectric constant (13) in comparison with that of the main phase of CaZrO3 (32). Thus, the dielectric constant of CaZrO3 doped with Nb2O5, or MnO is decreased markedly. In addition, Mn+2 incorporated into Zr-sites of CaZrO3 plays the role of acceptor, which compensates for the number of conduction electrons and contributes to better performance of electrical properties such as insulation resistance and \\tanδ. Conversely, Nb+5 incorporated into Zr-sites of CaZrO3 plays the role of donor and provides more conduction electrons, leading to poor performance of electrical properties.

Effect of Process Parameter on Barium Titanate Stannate (BTS) Materials Sintered at Low Sintering

NASA Astrophysics Data System (ADS)

Shukla, Alok; Bajpai, P. K.

2011-11-01

Ba(Ti1-xSnx)O3 solid solutions with (x = 0.15, 0.20, 0.30 and 0.40) are synthesized using conventional solid state reaction method. Formation of solid solutions in the range 0 ≤ x ≤0.40 is confirmed using X-ray diffraction technique. Single phase solid solutions with homogeneous grain distribution are observed at relatively low sintering by controlling process parameters viz. sintering time. Composition at optimized temperature (1150 °C) sintered by varying the sintering time, stabilize in cubic perovskite phase. The % experimental density increase with increasing the time of sintering instead of increasing sintering temperature. The lattice parameter increases by increasing the tin composition in the material. This demonstrates that process parameter optimization can lead to single phase at relatively lower sintering-a major advantage for the materials used as capacitor element in MLCC.

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

Wang, Siwei; Chen, Yan; Zhang, Lingling

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ(BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. In this paper, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering wasmore » improved to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. In conclusion, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less

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

Wang, Siwei; Chen, Yan; Zhang, Lingling

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. Here, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improvedmore » to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. Moreover, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less

Highly transparent Tb3Al5O12 magneto-optical ceramics sintered from co-precipitated powders with sintering aids

NASA Astrophysics Data System (ADS)

Dai, Jiawei; Pan, Yubai; Xie, Tengfei; Kou, Huamin; Li, Jiang

2018-04-01

Highly transparent terbium aluminum garnet (Tb3Al5O12, TAG) magneto-optical ceramics were fabricated from co-precipitated nanopowders with tetraethoxysilane (TEOS) as sintering aid by vacuum sintering combined with hot isostatic pressing (HIP) post-treatment. The ball milled TAG powder shows better dispersity than the as-synthesized powder, and its average particle size is about 80 nm. For the ceramic sample pre-sintered at 1720 °C for 20 h with HIP post-treated at 1700 °C for 3 h, the in-line transmittance exceeds 76% in the region of 400-1580nm (except the absorption band), reaching a maximum value of 81.8% at the wavelength of 1390 nm. The microstructure of the TAG ceramic is homogeneous and its average grain size is approximately 19.7 μm. The Verdet constant of the sample is calculated to be -182.7 rad·T-1·m-1 at room temperature.

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.

One step sintering of homogenized bauxite raw material and kinetic study

NASA Astrophysics Data System (ADS)

Gao, Chang-he; Jiang, Peng; Li, Yong; Sun, Jia-lin; Zhang, Jun-jie; Yang, Huan-ying

2016-10-01

A one-step sintering process of bauxite raw material from direct mining was completed, and the kinetics of this process was analyzed thoroughly. The results show that the sintering kinetics of bauxite raw material exhibits the liquid-phase sintering behavior. A small portion of impurities existed in the raw material act as a liquid phase. After X-ray diffraction analyses, scanning electron microscopy observations, and kinetics calculations, sintering temperature and heating duration were determined as the two major factors contributing to the sintering process and densification of bauxite ore. An elevated heating temperature and longer duration favor the densification process. The major obstacle for the densification of bauxite material is attributed to the formation of the enclosed blowhole during liquid-phase sintering.

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

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

Development of AlN and TiB2 Composites with Nb2O5, Y2O3 and ZrO2 as Sintering Aids

PubMed Central

González, José C.; Rodríguez, Miguel Á.; Figueroa, Ignacio A.; Villafuerte-Castrejón, María-Elena; Díaz, Gerardo C.

2017-01-01

The synthesis of AlN and TiB2 by spark plasma sintering (SPS) and the effect of Nb2O5, Y2O3 and ZrO2 additions on the mechanical properties and densification of the produced composites is reported and discussed. After the SPS process, dense AlN and TiB2 composites with Nb2O5, Y2O3 and ZrO2 were successfully prepared. X-ray diffraction analysis showed that in the AlN composites, the addition of Nb2O5 gives rise to Nb4N3 during sintering. The compound Y3Al5O12 (YAG) was observed as precipitate in the sample with Y2O3. X-ray diffraction analysis of the TiB2 composites showed TiB2 as a single phase in these materials. The maximum Vickers and toughness values were 14.19 ± 1.43 GPa and 27.52 ± 1.75 GPa for the AlN and TiB2 composites, respectively. PMID:28772681

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.

Powder metallurgy: Solid and liquid phase sintering of copper

NASA Technical Reports Server (NTRS)

Sheldon, Rex; Weiser, Martin W.

1993-01-01

Basic powder metallurgy (P/M) principles and techniques are presented in this laboratory experiment. A copper based system is used since it is relatively easy to work with and is commercially important. In addition to standard solid state sintering, small quantities of low melting metals such as tin, zinc, lead, and aluminum can be added to demonstrate liquid phase sintering and alloy formation. The Taguchi Method of experimental design was used to study the effect of particle size, pressing force, sintering temperature, and sintering time. These parameters can be easily changed to incorporate liquid phase sintering effects and some guidelines for such substitutions are presented. The experiment is typically carried out over a period of three weeks.

Sintered rare earth-iron Laves phase magnetostrictive alloy product and preparation thereof

DOEpatents

Malekzadeh, Manoochehr; Pickus, Milton R.

1979-01-01

A sintered rare earth-iron Laves phase magnetostrictive alloy product characterized by a grain oriented morphology. The grain oriented morphology is obtained by magnetically aligning powder particles of the magnetostrictive alloy prior to sintering. Specifically disclosed are grain oriented sintered compacts of Tb.sub.x Dy.sub.1-x Fe.sub.2 and their method of preparation. The present sintered products have enhanced magnetostrictive properties.

The influence of temperature induced phase transition on the energy storage density of anti-ferroelectric ceramics

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

Yi, Jinqiao; Zhang, Ling; Xie, Bing

2015-09-28

Anti-ferroelectric (AFE) composite ceramics of (Pb{sub 0.858}Ba{sub 0.1}La{sub 0.02}Y{sub 0.008})(Zr{sub 0.65}Sn{sub 0.3}Ti{sub 0.05})O{sub 3}-(Pb{sub 0.97}La{sub 0.02})(Zr{sub 0.9}Sn{sub 0.05} Ti{sub 0.05})O{sub 3} (PBLYZST-PLZST) were fabricated by the conventional solid-state sintering process (CS), the glass-aided sintering (GAS), and the spark plasma sintering (SPS), respectively. The influence of the temperature induced phase transition on the phase structure, hysteresis loops, and energy storage properties of the composite ceramics were investigated in detail. The measured results of X-ray diffraction demonstrate that the composite ceramics exhibit the perovskite phases and small amounts of non-functional pyrochlore phases. Compared with the CS process, the GAS and SPS processesmore » are proven more helpful to suppress the diffusion behaviors between the PBLYZST and PLZST phases according to the field emission scanning electron microscopy, thereby being able to improve the contribution of PBLYZST phase to the temperature stability of the orthogonal AFE phase. When the ambient temperature rises from 25 °C to 125 °C, CS and GAS samples have undergone a phase transition from orthorhombic AFE phase to tetragonal AFE phase, which results in a sharp decline in the energy storage density. However, the phase transition temperature of SPS samples is higher than 125 °C, and the energy storage density only slightly decreases due to the disorder of material microstructure caused by the high temperature. As a result, the SPS composite ceramics obtain a recoverable high energy storage density of 6.46 J/cm{sup 3} and the excellent temperature stability of the energy storage density of 1.16 × 10{sup −2} J/°C·cm{sup 3}, which is 1.29 × 10{sup −2} J/°C·cm{sup 3} lower than that of CS samples and about 0.43 times as that of GAS samples.« less

[Influence of MgO and TiO2 on mechanical properties of zirconia toughened alumina ceramics formed by gel-casting technique].

PubMed

Wang, Si-Qian; Wang, Wei; Du, Ruo-Xi; Zhang, Da-Feng; Liu, Chuan-Tong; Ma, Jian-Feng

2009-06-01

The objective of this study is to investigate the influence of mechanical properties and sintering performance by adding 5% weight percentage aids to nano-compound zirconia toughened alumina (ZTA) ceramics. Micrometer Al2O3 and nanometer ZrO2 (quality ratio 4:1) were used to get 55% volume percentage slurry. Magnesium oxide and titanium oxide were taken as aids which were 5% weight percentage of the Al2O3 and ZrO2 powder. Five groups (number 0, 1, 2, 3, 4 group) were divided according to different proportion of aids. After gel-casting, the porcelain pieces were sintered at 1150, 1200, 1300, 1400, 1450, 1500, 1600 degrees C for 2 hours. Static three-point flexure strength, line shrinkage, relative density were measured and scanning electron microscopy (SEM) was used to observe section. Number 1 (MgO 1%, TiO2 4%) group had the highest bending strength. It was (401.78+/-19.50) MPa after sintering at 1600 degrees C for 2 hours and was higher than 0 group (380.64+/-44.50) MPa. Bending strength became lower than 0 group when MgO was more than 2% or more than that weight percentage of ZTA powder. When MgO content was higher than 2% or more than that weight percentage, there was no difference in relative density raising rate between each sintering assistants groups. When the sintering temperature was higher than 1200 degrees C, all groups showed obvious line-shrinkage and the groups which contained sintering assistants were all was higher than 0 group. Adding MgO and TiO2 aids from 1% to 4% weight percentage of ZTA will promote fritting and increase ZTA nano-compound ceramics mechanical properties. Adding 2% MgO aids or more than that weight percent will has no obvious help to increase the relative density raising rate of ZTA nano-compound ceramics and will degrade the mechanical properties of ZTA nano-compound ceramics.

Effect of ZnO Nanoparticles on the Sintering Behavior and Physical Properties of Bi0.5(Na0.8K0.2)0.5TiO3 Lead-Free Ceramics

NASA Astrophysics Data System (ADS)

Vuong, Le Dai; Truong-Tho, Nguyen

2017-11-01

Sintered Bi0.5(Na0.8K0.2)0.5TiO3 + x wt.% ZnO nanoparticle (BNKT- xZnOn) ceramics have been fabricated by conventional annealing with the aid of ultrasound waves for preliminary milling. Because of the presence of the liquid Bi2O3-ZnO phase at the eutectic point of 738°C, the sintering temperature decreased from 1150°C to 1000°C, and the morphology phase boundary of BNKT- xZnOn ceramics can be clarified by two separated peaks at (002)T and (200)T of 2 θ in the x-ray diffraction (XRD) patterns. The improvement of ferroelectric properties has been obtained for BNZT-0.2 wt.% ZnOn ceramics by the increase of remanent polarization up to 20.4 μC/cm2 and a decrease of electric coercive field down to 14.2 kV/cm. The piezoelectric parameters of the ceramic included a piezoelectric charge constant of d 31 = 78 pC/N; electromechanical coupling factors k p = 0.31 and k t = 0.34, larger than the values of 42 pC/N, 0.12 and 0.13, respectively, were obtained for the BNKT ceramics.

New materials through a variety of sintering methods

NASA Astrophysics Data System (ADS)

Jaworska, L.; Cyboroń, J.; Cygan, S.; Laszkiewicz-Łukasik, J.; Podsiadło, M.; Novak, P.; Holovenko, Y.

2018-03-01

New sintering techniques make it possible to obtain materials with special properties that are impossible to obtain by conventional sintering techniques. This issue is especially important for ceramic materials for application under extreme conditions. Following the tendency to limit critical materials in manufacturing processes, the use of W, Si, B, Co, Cr should be limited, also. One of the cheapest and widely available materials is aluminum oxide, which shows differences in phase composition, grain size, hardness, strain and fracture toughness of the same type of powder, sintered via various methods. In this paper the alumina was sintered using the conventional free sintering process, microwave sintering, Spark Plasma Sintering (SPS), high pressure-high temperature method (HP-HT) and High Pressure Spark Plasma Sintering (HP SPS). Phase composition analysis, by X-ray diffraction of the alumina materials sintered using various methods, was carried out. For the conventional sintering method, compacts are composed of α-Al2O3 and θ-Al2O3. For compacts sintered using SPS, microwave and HP-HT methods, χ-Al2O3 and γ-Al2O3 phases were additionally present. Mechanical and physical properties of the obtained materials were compared between the methods of sintering. On the basis of images from scanning electron microscope quantitative analysis was performed to determine the degree of grain growth of alumina after sintering.

Liquid phase sintering of silicon carbide

DOEpatents

Cutler, R.A.; Virkar, A.V.; Hurford, A.C.

1989-05-09

Liquid phase sintering is used to densify silicon carbide based ceramics using a compound comprising a rare earth oxide and aluminum oxide to form liquids at temperatures in excess of 1,600 C. The resulting sintered ceramic body has a density greater than 95% of its theoretical density and hardness in excess of 23 GPa. Boron and carbon are not needed to promote densification and silicon carbide powder with an average particle size of greater than one micron can be densified via the liquid phase process. The sintered ceramic bodies made by the present invention are fine grained and have secondary phases resulting from the liquid phase. 4 figs.

Liquid phase sintering of silicon carbide

DOEpatents

Cutler, Raymond A.; Virkar, Anil V.; Hurford, Andrew C.

1989-01-01

Liquid phase sintering is used to densify silicon carbide based ceramics using a compound comprising a rare earth oxide and aluminum oxide to form liquids at temperatures in excess of 1600.degree. C. The resulting sintered ceramic body has a density greater than 95% of its theoretical density and hardness in excess of 23 GPa. Boron and carbon are not needed to promote densification and silicon carbide powder with an average particle size of greater than one micron can be densified via the liquid phase process. The sintered ceramic bodies made by the present invention are fine grained and have secondary phases resulting from the liquid phase.

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

High impact resistant ceramic composite

DOEpatents

Derkacy, J.A.

1991-07-16

A ceramic material and a method of forming a ceramic material which possesses a high impact resistance are disclosed. The material comprises: (a) a first continuous phase of [beta]-SiC; and (b) a second phase of about 25-40 vol % TiB[sub 2]. Al[sub 2]O[sub 3] is preferably used as a densification aid. The material is formed by hot-pressing the mixture at a temperature from greater than about 1800 C to less than the transition temperature of [beta]-SiC to [alpha]-SiC. The hot-pressing is performed at a pressure of about 2000 psi to about 4000 psi in an inert atmosphere for several hours and results in the formation of a two phase sintered ceramic composite material. 6 figures.

High impact resistant ceramic composite

DOEpatents

Derkacy, James A.

1991-07-16

A ceramic material and a method of forming a ceramic material which possesses a high impact resistance. The material comprises: (a) a first continuous phase of .beta.-SiC; and (b) a second phase of about 25-40 vol % TiB.sub.2. Al.sub.2 O.sub.3 is preferably used as a densification aid. The material is formed by hot-pressing the mixture at a temperature from greater than about 1800.degree. C. to less than the transition temperature of .beta.-SiC to .alpha.-SiC. The hot-pressing is performed at a pressure of about 2000 psi to about 4000 psi in an inert atmosphere for several hours and results in the formation of a two phase sintered ceramic composite material.

Taguchi Analysis on the Effect of Process Parameters on Densification During Spark Plasma Sintering of HfB2-20SiC (Preprint)

DTIC Science & Technology

2011-11-01

30 kN pressure and heating rate of 100 K/min. Introduction Boride , carbides and nitrides of the group IVB and VB transition metals are considered...10. Sciti D., Silvestroni L., Nygren M. Spark plasma sintering of Zr- and Hf- borides with decreasing amounts of MoSi2 as sintering aid Journal of

Sintering of Lead-Free Piezoelectric Sodium Potassium Niobate Ceramics

PubMed Central

Malič, Barbara; Koruza, Jurij; Hreščak, Jitka; Bernard, Janez; Wang, Ke; Fisher, John G.; Benčan, Andreja

2015-01-01

The potassium sodium niobate, K0.5Na0.5NbO3, solid solution (KNN) is considered as one of the most promising, environment-friendly, lead-free candidates to replace highly efficient, lead-based piezoelectrics. Since the first reports of KNN, it has been recognized that obtaining phase-pure materials with a high density and a uniform, fine-grained microstructure is a major challenge. For this reason the present paper reviews the different methods for consolidating KNN ceramics. The difficulties involved in the solid-state synthesis of KNN powder, i.e., obtaining phase purity, the stoichiometry of the perovskite phase, and the chemical homogeneity, are discussed. The solid-state sintering of stoichiometric KNN is characterized by poor densification and an extremely narrow sintering-temperature range, which is close to the solidus temperature. A study of the initial sintering stage revealed that coarsening of the microstructure without densification contributes to a reduction of the driving force for sintering. The influences of the (K + Na)/Nb molar ratio, the presence of a liquid phase, chemical modifications (doping, complex solid solutions) and different atmospheres (i.e., defect chemistry) on the sintering are discussed. Special sintering techniques, such as pressure-assisted sintering and spark-plasma sintering, can be effective methods for enhancing the density of KNN ceramics. The sintering behavior of KNN is compared to that of a representative piezoelectric lead zirconate titanate (PZT). PMID:28793702

Correction of facial and mandibular asymmetry using a computer aided design/computer aided manufacturing prefabricated titanium implant.

PubMed

Watson, Jason; Hatamleh, Muhanad; Alwahadni, Ahed; Srinivasan, Dilip

2014-05-01

Patients with significant craniofacial asymmetry may have functional problems associated with their occlusion and aesthetic concerns related to the imbalance in soft and hard tissue profiles. This report details a case of facial asymmetry secondary to left mandible angle deficiency due to undergoing previous radiotherapy. We describe the correction of the bony deformity using computer aided design/computer aided manufacturing custom-made titanium onlay using novel direct metal laser sintering. The direct metal laser sintering onlay proved a very accurate operative fit and showed a good aesthetic correction of the bony defect with no reported complications postoperatively. It is a useful low-morbidity technique, and there is no resorption or associated donor-site complications.

Accelerated sintering in phase-separating nanostructured alloys

PubMed Central

Park, Mansoo; Schuh, Christopher A.

2015-01-01

Sintering of powders is a common means of producing bulk materials when melt casting is impossible or does not achieve a desired microstructure, and has long been pursued for nanocrystalline materials in particular. Acceleration of sintering is desirable to lower processing temperatures and times, and thus to limit undesirable microstructure evolution. Here we show that markedly enhanced sintering is possible in some nanocrystalline alloys. In a nanostructured W–Cr alloy, sintering sets on at a very low temperature that is commensurate with phase separation to form a Cr-rich phase with a nanoscale arrangement that supports rapid diffusional transport. The method permits bulk full density specimens with nanoscale grains, produced during a sintering cycle involving no applied stress. We further show that such accelerated sintering can be evoked by design in other nanocrystalline alloys, opening the door to a variety of nanostructured bulk materials processed in arbitrary shapes from powder inputs. PMID:25901420

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).

METHOD OF JOINING CARBIDES TO BASE METALS

DOEpatents

Krikorian, N.H.; Farr, J.D.; Witteman, W.G.

1962-02-13

A method is described for joining a refractory metal carbide such as UC or ZrC to a refractory metal base such as Ta or Nb. The method comprises carburizing the surface of the metal base and then sintering the base and carbide at temperatures of about 2000 deg C in a non-oxidizing atmosphere, the base and carbide being held in contact during the sintering step. To reduce the sintering temperature and time, a sintering aid such as iron, nickel, or cobait is added to the carbide, not to exceed 5 wt%. (AEC)

Influence of processing parameters on microstructure and biocompatibility of surface laser sintered hydroxyapatite-SiO2 composites.

PubMed

Kivitz, E; Görke, R; Schilling, A F; Zhang, J; Heinrich, J G

2013-05-01

Silica-doped hydroxyapatite (HA) is a promising material concerning biocompatibility to natural bone, bioactivity and osteoconductive characteristics. HA exhibits phase transformations during sintering which are attendant to the change in volume and thermal strain. To avoid cracks during sintering, the exact knowledge of the phase transition temperatures is necessary. The sintering behavior of HA can be improved by adding amorphous silica with a low coefficient of thermal expansion. Therefore, the phase transformations in the system HA-SiO2 were analyzed by using differential scanning calorimetry followed by quantitative phase analysis by X-ray diffraction with the Riedveld method. The maximum sintering temperature without reversible phase transformation was defined as 1265°C. In laser surface sintered (LSS) samples, amorphous SiO2 , HA, and Si-α-TCP (or α-TCP) were detected. By comparison, only crystalline phases, such as cristobalite, HA, β-TCP, and Si-α-TCP (or α-TCP), were determined after furnace sintering. Scanning electron microscopy micrographs of furnace sintered and LSS samples show the differences in the resulting microstructures. Biocompatibility was determined by measuring cell activity of osteoblasts cultivated on four laser-sintered materials in the HA-SiO2 system in comparison to normal cell culture plastic. Cell proliferation was similar on all surfaces. The level of the cell activity on day 8 varied depending on the composition of the material and increased linearly as the amorphous SiO2 content rose. Taken together a laser-based method to develop novel biocompatible HA-SiO2 ceramics with adjustable properties and possible applications as orthopedic bioceramics are discussed. Copyright © 2012 Wiley Periodicals, Inc.

Investigation of the Nd-rich phases in the Nd-Fe-B system

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

Tang, W.; Zhou, S.; Wang, R.

1988-11-15

The crystal structures and the compositions of the Nd-rich phases in the Nd-Fe-B system have been investigated by means of transmission electron microscopy, x-ray diffraction, and Auger spectroscopy techniques. It has been observed that there are two kinds of Nd-rich phases with different structures and compositions. Most of the Nd-rich phases will undergo a phase transformation when the powder is sintered at high temperatures. This phase transformation is accompanied by the introduction of oxygen into the alloy which will change from a ternary system into a quaternary one. Both of the two Nd-rich phases are stable phases in this latermore » system. With the aid of the EDX and the Auger spectroscope, the compositions of the dhcp and the fcc Nd-rich phases have been determined. The Nd contents of the two phases are about 90 and 70 at. %, respectively, with the later phase containing about 15 at. % of oxygen.« less

Anisotropy of the ferromagnetic L10 phase in the Mn-Al-C alloys induced by high-pressure spark plasma sintering

NASA Astrophysics Data System (ADS)

Tyrman, Muriel; Ahmim, Smail; Pasko, Alexandre; Etgens, Victor; Mazaleyrat, Frédéric; Quetel-Weben, Simon; Perrière, Loïc; Guillot, Ivan

2018-05-01

The metastable τ-phase of MnAl equi-atomic compound belongs to a family of ferromagnetic alloys with L10 crystal structure. Stabilization of the phase by adding 2 at. % using manganese carbide (Mn23C6) enhances the magnetization in relation with the increase in lattice volume. It is thus a promising candidate for rare-earth-free permanent magnets. Coercivity of Mn-Al-C alloys being still weak, there is an interest to see to which extend sintering/transformation of the ɛ-phase by Spark Plasma Sintering (SPS) can increase the coercivity and the anisotropy. The structural and the magnetic properties were studied for samples sintered at 550 °C under uniaxial pressure of 100, 200, 300 and 400 MPa. Coercivity, remanence and anistotropy appears with the sintering pressure. The high pressure applied while sintering produces preferential orientation of the flake-shaped grains which influences the remanence.

Sintering and microstructure of silicon carbide ceramic with Y3Al5O12 added by sol-gel method*

PubMed Central

Guo, Xing-zhong; Yang, Hui

2005-01-01

Silicon carbide (SiC) ceramic with YAG (Y3Al5O12) additive added by sol-gel method was liquid-phase sintered at different sintering temperatures, and the sintering mechanism and microstructural characteristics of resulting silicon carbide ceramics were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and elemental distribution of surface (EDS). YAG (yttrium aluminum garnet) phase formed before the sintering and its uniform distribution in the SiC/YAG composite powder decreased the sintering temperature and improved the densification of SiC ceramic. The suitable sintering temperature was 1860 °C with the specimen sintered at this temperature having superior sintering and mechanical properties, smaller crystal size and fewer microstructure defects. Three characteristics of improved toughness of SiC ceramic with YAG added by sol-gel method were microstructural densification, main-crack deflection and crystal ‘bridging’. PMID:15682507

Selective laser sintering of single-phase powder Cr-V tool steel

NASA Astrophysics Data System (ADS)

Kovalev, A. I.; Mishina, V. P.; Wainstein, D. L.; Titov, V. I.; Moiseev, V. F.; Tolochko, N. K.

2002-10-01

Presented is positive experience from selective laser sintering (SLS) of cylindrical steel specimens (3.0% C, 3.0% Cr, 1.0% Si, 12.0% V, Fe balance) 30 mm long and 5 mm in diameter by rapid prototyping. It was demonstrated that monolithic steel material could be successfully fabricated by this technology. Differential thermal analysis (DTA), scanning electron microscopy (SEM), and x-ray diffractometry (XRD) were used to study the microstructure, phase, and chemical composition of the source material and obtained specimens. Low-melting cementite-based eutectic was found to provide the liquid phase sintering of powder tool steel. The porosity of the green sintered specimens did not exceed 5%. The mean hardness value of sintered specimens was 825 HV.

Effect of the application of surface treatments before and after sintering on the flexural strength, phase transformation and surface topography of zirconia.

PubMed

Kurtulmus-Yilmaz, Sevcan; Aktore, Huseyin

2018-05-01

To evaluate the effects of airborne-particle abrasion (APA) and Er,Cr:YSGG laser irradiation on 4-point-flexural strength, phase transformation and morphologic changes of zirconia ceramics treated at pre-sintered or post-sintered stage. Three hundred and forty-two bar shaped zirconia specimens were milled with different sizes according to the flexural strength test (n = 10), X-ray diffraction (XRD) (n = 4) and field emission scanning electron microscope (FE-SEM) (n = 4) analyses. For each test protocol, specimens were divided into 4 main groups whether the surface treatments applied before or after sintering and whether the specimens received heat treatment or not as pre-sintered, post-sintered no-heat and post-sintered heat-treated groups, and a group was served as control. Main groups were further divided into 6 equal subgroups according to surface treatment method applied (2 W-, 3 W-, 4 W-, 5 W-, 6 W-laser irradiations and APA). Surface treatments were applied to pre-sintered groups before sintering and to post-sintered groups after sintering. Post-sintered heat-treated groups were subjected to veneer ceramic firing simulation after surface treatments. Flexural strength and flexural modulus values were statistically analysed and monoclinic phase content was calculated. Weibull analysis was used to evaluate strength reliability and fractographic analysis was conducted. Highest flexural strength values were detected at post-sintered no-heat APA and 4W-laser groups (P < 0.05). Pre-sintered groups showed statistically lower flexural strength values. Heat treatment decreased the strength of the specimens. Monoclinic phase content was only detected at post-sintered no-heat groups and the highest amount was detected at APA group. Rougher surfaces and deeper irregularities were detected at FE-SEM images pre-sintered groups. Application of surface treatments at pre-sintered stage may be detrimental for zirconia ceramics in terms of flexural strength. Treating the surface of zirconia ceramic before sintering process is not recommended due to significant decrease in flexural strength values. 2 W-4 W Er,Cr:YSGG laser irradiations can be regarded as alternative surface treatment methods when zirconia restoration would be subjected to veneer ceramic firing procedures. Copyright © 2018 Elsevier Ltd. All rights reserved.

Scanning Electron Microscopy Analysis of the Adaptation of Single-Unit Screw-Retained Computer-Aided Design/Computer-Aided Manufacture Abutments After Mechanical Cycling.

PubMed

Markarian, Roberto Adrian; Galles, Deborah Pedroso; Gomes França, Fabiana Mantovani

To measure the microgap between dental implants and custom abutments fabricated using different computer-aided design/computer-aided manufacture (CAD/CAM) methods before and after mechanical cycling. CAD software (Dental System, 3Shape) was used to design a custom abutment for a single-unit, screw-retained crown compatible with a 4.1-mm external hexagon dental implant. The resulting stereolithography file was sent for manufacturing using four CAD/CAM methods (n = 40): milling and sintering of zirconium dioxide (ZO group), cobalt-chromium (Co-Cr) sintered via selective laser melting (SLM group), fully sintered machined Co-Cr alloy (MM group), and machined and sintered agglutinated Co-Cr alloy powder (AM group). Prefabricated titanium abutments (TI group) were used as controls. Each abutment was placed on a dental implant measuring 4.1× 11 mm (SA411, SIN) inserted into an aluminum block. Measurements were taken using scanning electron microscopy (SEM) (×4,000) on four regions of the implant-abutment interface (IAI) and at a relative distance of 90 degrees from each other. The specimens were mechanically aged (1 million cycles, 2 Hz, 100 N, 37°C) and the IAI width was measured again using the same approach. Data were analyzed using two-way analysis of variance, followed by the Tukey test. After mechanical cycling, the best adaptation results were obtained from the TI (2.29 ± 1.13 μm), AM (3.58 ± 1.80 μm), and MM (1.89 ± 0.98 μm) groups. A significantly worse adaptation outcome was observed for the SLM (18.40 ± 20.78 μm) and ZO (10.42 ± 0.80 μm) groups. Mechanical cycling had a marked effect only on the AM specimens, which significantly increased the microgap at the IAI. Custom abutments fabricated using fully sintered machined Co-Cr alloy and machined and sintered agglutinated Co-Cr alloy powder demonstrated the best adaptation results at the IAI, similar to those obtained with commercial prefabricated titanium abutments after mechanical cycling. The adaptation of custom abutments made by means of SLM or milling and sintering of zirconium dioxide were worse both before and after mechanical cycling.

Magnetic properties of ball-milled SrFe12O19 particles consolidated by Spark-Plasma Sintering

PubMed Central

Stingaciu, Marian; Topole, Martin; McGuiness, Paul; Christensen, Mogens

2015-01-01

The room-temperature magnetic properties of ball-milled strontium hexaferrite particles consolidated by spark-plasma sintering are strongly influenced by the milling time. Scanning electron microscopy revealed the ball-milled SrFe12O19 particles to have sizes varying over several hundred nanometers. X-Ray powder-diffraction studies performed on the ball-milled particles before sintering clearly demonstrate the occurrence of a pronounced amorphization process. During sintering at 950 oC, re-crystallization takes place, even for short sintering times of only 2 minutes and transformation of the amorphous phase into a secondary phase is unavoidable. The concentration of this secondary phase increases with increasing ball-milling time. The remanence and maximum magnetization values at 1T are weakly influenced, while the coercivity drops dramatically from 2340 Oe to 1100 Oe for the consolidated sample containing the largest amount of secondary phase. PMID:26369360

Method of manufacture of single phase ceramic superconductors

DOEpatents

Singh, J.P.; Poeppel, R.B.; Goretta, K.C.; Chen, N.

1995-03-28

A ceramic superconductor is produced by close control of oxygen partial pressure during sintering of the material. The resulting microstructure of YBa{sub 2}Cu{sub 3}O{sub x} indicates that sintering kinetics are enhanced at reduced p(O{sub 2}) and that because of second phase precipitates, grain growth is prevented. The density of specimens sintered at 910 C increased from 79 to 94% theoretical when p(O{sub 2}) was decreased from 0.1 to 0.0001 MPa. The increase in density with decrease in p(O{sub 2}) derives from enhanced sintering kinetics, due to increased defect concentration and decreased activation energy of the rate-controlling species undergoing diffusion. Sintering at 910 C resulted in a fine-grain microstructure, with an average grain size of about 4 {mu}m. Post sintering annealing in a region of stability for the desired phase converts the second phases and limits grain growth. The method of pinning grain boundaries by small scale decompositive products and then annealing to convert its product to the desired phase can be used for other complex asides. Such a microstructure results in reduced microcracking, strengths as high as 230 MPa and high critical current density capacity. 25 figures.

Method of manufacture of single phase ceramic superconductors

DOEpatents

Singh, Jitrenda P.; Poeppel, Roger B.; Goretta, Kenneth C.; Chen, Nan

1995-01-01

A ceramic superconductor is produced by close control of oxygen partial pressure during sintering of the material. The resulting microstructure of YBa.sub.2 Cu.sub.3 O.sub.x indicates that sintering kinetics are enhanced at reduced p(O.sub.2) and that because of second phase precipitates, grain growth is prevented. The density of specimens sintered at 910.degree. C. increased from 79 to 94% theoretical when p(O.sub.2) was decreased from 0.1 to 0.0001 MPa. The increase in density with decrease in p(O.sub.2) derives from enhanced sintering kinetics, due to increased defect concentration and decreased activation energy of the rate-controlling species undergoing diffusion. Sintering at 910.degree. C resulted in a fine-grain microstructure, with an average grain size of about 4 .mu.m. Post sintering annealing in a region of stability for the desired phase converts the second phases and limits grain growth. The method of pinning grain boundaries by small scale decompositive products and then annealing to convert its product to the desired phase can be used for other complex asides. Such a microstructure results in reduced microcracking, strengths as high as 230 MPa and high critical current density capacity.

Development of Processing Parameters for Organic Binders Using Selective Laser Sintering

NASA Technical Reports Server (NTRS)

Mobasher, Amir A.

2003-01-01

This document describes rapid prototyping, its relation to Computer Aided Design (CAD), and the application of these techniques to choosing parameters for Selective Laser Sintering (SLS). The document reviews the parameters selected by its author for his project, the SLS machine used, and its software.

Ir-based refractory superalloys by pulse electric current sintering (PECS) process (II prealloyed powder)

NASA Astrophysics Data System (ADS)

Huang, C.; Yamabe-Mitarai, Y.; Harada, H.

2002-02-01

Five prealloyed powder samples prepared from binary Ir-based refractory superalloys were sintered at 1800 °C for 4 h by Pulse Electric Current Sintering (PECS). No metal loss was observed during sintering. The relative densities of the sintered specimens all exceeded 90% T.D. The best one was Ir-13% Hf with the density of 97.82% T.D. Phases detected in sintered samples were in accordance with the phase diagram as expected. Fractured surfaces were observed in two samples (Ir-13% Hf and Ir-15% Zr). Some improvements obtained by using prealloyed powders instead of elemental powders, which were investigated in the previous studies, were presented.

[Effect of repeated sintering and variations in thickness on the color and microstructure of dental lithium disilicate-based glass ceramic veneers].

PubMed

Cui, Huang; Jia, Yu; Shaofeng, Meng; Biyun, Gao

2017-08-01

Objective The aim of this study is to evaluate the effect of repeated sintering and variation in thickness on the color and microstructure of dental lithium disilicate-based glass ceramic veneers. Methods A total of 24 computer aided design and computer aided manufacturing (CAD/CAM) veneers was fabricated using the IPS e.max-CAD LS2 and then randomly divided into four groups (S0, S1, S2, S3; n=6). Each group was sintered 0, 1, 2, 3 times individually according to the manufacturer's recommendation. The color parameters (L, C, H, a, b values) of all the specimens were measured by a Vita easyshade dental colorimeter. The results were statistically analyzed using the SAS 9.1.3 software for MANOVA and LSD. Subsequently, the microstructures of the intersecting surfaces of the specimens were observed by scanning electron microscopy (SEM). Results After repeated sintering, the L value significantly decreased (P<0.05). For the C and b values, statistical differences were observed among the groups except between S2 and S3. SEM results showed that the interlocking microstructures of rod-shaped Li₂Si₂O₅ crystals became more compact when the number of sintering times was increased. Conclusion Repeated sintering exhibited significant influence on the color of the IPS e.max-CAD LS2 veneers.

SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB{sub 2}

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

Sulima, Iwona, E-mail: isulima@up.krakow.pl

Steel-8TiB{sub 2} composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB{sub 2} particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size ofmore » materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB{sub 2} composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB{sub 2} composites. •New phases of different size and morphology were identified.« less

Sintering, properties and fabrication of Si3N4 + Y2O3 based ceramics

NASA Technical Reports Server (NTRS)

Quackenbush, C. L.; Smith, J. T.; Neil, J. T.; French, K. W.

1983-01-01

Pure silicon nitride shows a remarkable resistance to sintering without the use of densification additives. The present investigation is concerned with results which show the effect of chemical content on sinterability, taking into account the composition, raw material impurities, and processing contaminants. Aspects of sintering are discussed along with strength characteristics, and oxidation relations. Attention is given to phase field I and II materials, phase field III and IV materials, tungsten carbide and oxidation at 600 C, and studies involving shape fabrication by injection molding. It was found that in sintering Si3N4 + Y2O3 an increase in the amount of Y2O3 and, in particular, the addition of Al2O3 enhances the fluidity of the liquid phase.

Sintering of micro-trusses created by extrusion-3D-printing of lunar regolith inks

NASA Astrophysics Data System (ADS)

Taylor, Shannon L.; Jakus, Adam E.; Koube, Katie D.; Ibeh, Amaka J.; Geisendorfer, Nicholas R.; Shah, Ramille N.; Dunand, David C.

2018-02-01

The development of in situ fabrication methods for the infrastructure required to support human life on the Moon is necessary due to the prohibitive cost of transporting large quantities of materials from the Earth. Cellular structures, consisting of a regular network (truss) of micro-struts with ∼500 μm diameters, suitable for bricks, blocks, panels, and other load-bearing structural elements for habitats and other infrastructure are created by direct-extrusion 3D-printing of liquid inks containing JSC-1A lunar regolith simulant powders, followed by sintering. The effects of sintering time, temperature, and atmosphere (air or hydrogen) on the microstructures, mechanical properties, and magnetic properties of the sintered lunar regolith micro-trusses are investigated. The air-sintered micro-trusses have higher relative densities, linear shrinkages, and peak compressive strengths, due to the improved sintering of the struts within the micro-trusses achieved by a liquid or glassy phase. Whereas the hydrogen-sintered micro-trusses show no liquid-phase sintering or glassy phase, they contain metallic iron 0.1-2 μm particles from the reduction of ilmenite, which allows them to be lifted with magnets.

Structural characterization of biomedical Co-Cr-Mo components produced by direct metal laser sintering.

PubMed

Barucca, G; Santecchia, E; Majni, G; Girardin, E; Bassoli, E; Denti, L; Gatto, A; Iuliano, L; Moskalewicz, T; Mengucci, P

2015-03-01

Direct metal laser sintering (DMLS) is a technique to manufacture complex functional mechanical parts from a computer-aided design (CAD) model. Usually, the mechanical components produced by this procedure show higher residual porosity and poorer mechanical properties than those obtained by conventional manufacturing techniques. In this work, a Co-Cr-Mo alloy produced by DMLS with a composition suitable for biomedical applications was submitted to hardness measurements and structural characterization. The alloy showed a hardness value remarkably higher than those commonly obtained for the same cast or wrought alloys. In order to clarify the origin of this unexpected result, the sample microstructure was investigated by X-ray diffraction (XRD), electron microscopy (SEM and TEM) and energy dispersive microanalysis (EDX). For the first time, a homogeneous microstructure comprised of an intricate network of thin ε (hcp)-lamellae distributed inside a γ (fcc) phase was observed. The ε-lamellae grown on the {111}γ planes limit the dislocation slip inside the γ (fcc) phase, causing the measured hardness increase. The results suggest possible innovative applications of the DMLS technique to the production of mechanical parts in the medical and dental fields. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

Order parameter aided efficient phase space exploration under extreme conditions

NASA Astrophysics Data System (ADS)

Samanta, Amit

Physical processes in nature exhibit disparate time-scales, for example time scales associated with processes like phase transitions, various manifestations of creep, sintering of particles etc. are often much higher than time the system spends in the metastable states. The transition times associated with such events are also orders of magnitude higher than time-scales associated with vibration of atoms. Thus, an atomistic simulation of such transition events is a challenging task. Consequently, efficient exploration of configuration space and identification of metastable structures in condensed phase systems is challenging. In this talk I will illustrate how we can define a set of coarse-grained variables or order parameters and use these to systematically and efficiently steer a system containing thousands or millions of atoms over different parts of the configuration. This order parameter aided sampling can be used to identify metastable states, transition pathways and understand the mechanistic details of complex transition processes. I will illustrate how this sampling scheme can be used to study phase transition pathways and phase boundaries in prototypical materials, like SiO2 and Cu under high-pressure conditions. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

Fracture behavior of metal-ceramic fixed dental prostheses with frameworks from cast or a newly developed sintered cobalt-chromium alloy.

PubMed

Krug, Klaus-Peter; Knauber, Andreas W; Nothdurft, Frank P

2015-03-01

The aim of this study was to investigate the fracture behavior of metal-ceramic bridges with frameworks from cobalt-chromium-molybdenum (CoCrMo), which are manufactured using conventional casting or a new computer-aided design/computer-aided manufacturing (CAD/CAM) milling and sintering technique. A total of 32 metal-ceramic fixed dental prostheses (FDPs), which are based on a nonprecious metal framework, was produced using a conventional casting process (n = 16) or a new CAD/CAM milling and sintering process (n = 16). Eight unveneered frameworks were manufactured using each of the techniques. After thermal and mechanical aging of half of the restorations, all samples were subjected to a static loading test in a universal testing machine, in which acoustic emission monitoring was performed. Three different critical forces were revealed: the fracture force (F max), the force at the first reduction in force (F decr1), and the force at the critical acoustic event (F acoust1). With the exception of the veneered restorations with cast or sintered metal frameworks without artificial aging, which presented a statistically significant but slightly different F max, no statistically significant differences between cast and CAD/CAM sintered and milled FDPs were detected. Thermal and mechanical loading did not significantly affect the resulting forces. Cast and CAD/CAM milled and sintered metal-ceramic bridges were determined to be comparable with respect to the fracture behavior. FDPs based on CAD/CAM milled and sintered frameworks may be an applicable and less technique-sensitive alternative to frameworks that are based on conventionally cast frameworks.

Rare earth elements in sinters from the geothermal waters (hot springs) on the Tibetan Plateau, China

NASA Astrophysics Data System (ADS)

Feng, Jin-Liang; Zhao, Zhen-Hong; Chen, Feng; Hu, Hai-Ping

2014-10-01

The mineralogical and geochemical composition of sinters from the geothermal areas on the Tibetan Plateau was determined. They occur as siliceous, salty and calcareous sinters but biogenic siliceous sinters were also found. The analyses indicate that there are no distinct inter -element relationships between individual rare earth elements (REEs) and other elements. Formed from the same geothermal water, the mineralogical and chemical composition of the sinters is influenced by their genesis and formation conditions. The REE distributions depend on the origin of the sinters. Fe-Mn phases in sinters tend to scavenge more REEs from geothermal water. Neither the REE fractionation nor the Ce anomaly seems to be associated with Fe-Mn phases in the sinters. The fourth tetrads of some sinters display weak W-type (concave) effects. In contrast, the third tetrads present large effects in some sinters due to positive Gd anomalies. The origin of the positive Eu anomalies in some sinters seems to be caused by preferential dissolution of feldspars during water-rock interaction. The complexing ligands in geothermal water may contribute significantly to the fractionation of REEs in sinters. The dominant CO32- and HCO3- complexing in geothermal water favors enrichment of heavy REEs in calcareous sinters.

Experimental sintering of ash at conduit conditions and implications for the longevity of tuffisites

NASA Astrophysics Data System (ADS)

Gardner, James E.; Wadsworth, Fabian B.; Llewellin, Edward W.; Watkins, James M.; Coumans, Jason P.

2018-03-01

Escape of gas from magma in the conduit plays a crucial role in mitigating explosivity. Tuffisite veins—ash-filled cracks that form in and around volcanic conduits—represent important gas escape pathways. Sintering of the ash infill decreases its porosity, eventually forming dense glass that is impermeable to gas. We present an experimental investigation of surface tension-driven sintering and associated densification of rhyolitic ash under shallow conduit conditions. Suites of isothermal (700-800 °C) and isobaric H2O pressure (20 and 40 MPa) experiments were run for durations of 5-90 min. Obsidian powders with two different size distributions were used: 1-1600 μm (mean size = 89 μm), and 63-400 μm (mean size = 185 μm). All samples evolved similarly through four textural phases: phase 1—loose and cohesion-less particles; phase 2—particles sintered at contacts and surrounded by fully connected tortuous pore space of up to 40% porosity; phase 3—continuous matrix of partially coalesced particles that contain both isolated spherical vesicles and connected networks of larger, contorted vesicles; phase 4—dense glass with 2-5% fully isolated vesicles that are mainly spherical. Textures evolve faster at higher temperature and higher H2O pressure. Coarse samples sinter more slowly and contain fewer, larger vesicles when fully sintered. We quantify the sintering progress by measuring porosity as a function of experimental run-time, and find an excellent collapse of data when run-time is normalized by the sintering timescale {λ}_s=η \\overline{R}/σ , where η is melt viscosity, \\overline{R} is mean particle radius, and σ is melt-gas surface tension. Because timescales of diffusive H2O equilibration are generally fast compared to those of sintering, the relevant melt viscosity is calculated from the solubility H2O content at experimental temperature and pressure. We use our results to develop a framework for estimating ash sintering rates under shallow conduit conditions, and predict that sintering of ash to dense glass can seal tuffisites in minutes to hours, depending on pressure (i.e., depth), temperature, and ash size.

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.

Modeling the mechanical behavior of ceramic and heterophase structures manufactured using selective laser sintering and spark plasma sintering

NASA Astrophysics Data System (ADS)

Skripnyak, Vladimir A.; Skripnyak, Evgeniya G.; Skripnyak, Vladimir V.; Vaganova, Irina K.

A model for predicting mechanical properties of ultra-high temperature ceramics and composites manufactured by selective laser sintering (SLS) and spark plasma sintering (SPS) under shock loading is presented. The model takes into account the porous structure, the specific volume and average sizes of phases, and the temperature of sintering. Residual stresses in ceramic composites reinforced with particles of refractory borides, carbides and nitrides after SLS or SPS were calculated. It is shown that the spall strength of diboride-zirconium matrix composites can be increased by the decreasing of porosity and the introduction of inclusions of specially selected refractory strengthening phases.

Synthesis and characterization of a model dual-phase system using the spark plasma sintering technique

NASA Astrophysics Data System (ADS)

Teimouri, M.; Godfrey, A.

2017-07-01

Samples of a model dual-phase system, consisting of copper and AISI-420 martensitic steel have been synthesized using spark plasma sintering, with the objective of developing a microstructural analogue for dual-phase steels, in which the volume fraction and size of each phase can be controlled independently. Microstructural investigation of the samples, including fractography of samples deformed in tension until failure, show that densification is strongly temperature dependent. Samples sintered at temperatures of 900 °C or above at a pressure of 60 MPa show a density of more than 98%. The best mechanical properties, in terms of ultimate tensile strength and ductility is found in samples sintered at a temperature of 1000 °C, where a density of nearly 99% is achieved.

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.

Role of Y2O3, CaO, MgO additives on structural and microstructural behavior of zirconia/mullite aggregates

NASA Astrophysics Data System (ADS)

Mishra, D. K.; Prusty, Sasmita; Mohapatra, B. K.; Singh, S. K.; Behera, S. N.

2012-07-01

Zirconia mullite (MUZ), Y2O3-MUZ, CaO-MUZ and MgO-MUZ composites, synthesized through plasma fusion technique, are becoming important due to their commercial scale of production within five minutes of plasma treatment from sillimanite, zircon and alumina mixture. The X-ray diffraction studies reveal the monoclinic zirconia phase in MUZ composite whereas mixed monoclinic, tetragonal and cubic phases of zirconia have been observed in Y2O3, CaO, MgO added MUZ composites. The Y2O3, CaO and MgO additives act as sintering aids to favour the transformation and stabilisation of tetragonal and cubic zirconia phases at room temperature. These additives also play a key role in the development of various forms of microstructure to achieve dense MUZ composites.

Low-Temperature Sintering of AlN Ceramics by Sm2O3-Y2O3-CaO Sintering Additives Formed via Decomposition of Nitrate Solutions

NASA Astrophysics Data System (ADS)

Zhan, Jun; Cao, Ye; Zhang, Hao; Guo, Jun; Zhang, Jianhua; Geng, Chunlei; Shi, Changdong; Cui, Song; Tang, Wenming

2017-01-01

The Sm, Y and Ca anhydrous nitrates were mixed with the AlN powder in ethanol and then decomposed into the Sm2O3-Y2O3-CaO sintering additives via calcining. Low-temperature sintering of the AlN ceramics was carried out at temperature range from 1675 to 1750 °C. Effects of the composition and adding amount of the sintering additives on the phases, microstructures and properties of the AlN ceramics were investigated. During sintering the AlN ceramics, main secondary phases of CaYAl3O7 and CaSmAl3O7 form. The relative density, bending strength and thermal conductivity of the AlN ceramics increase with the increase in the rare-earth oxides in them. The thermal conductivity of the sintered AlN ceramics is also greatly affected by the distribution of the secondary phases. As sintered at 1750 °C, the AlN ceramics by adding the sintering additives of 2 wt.% Sm2O3, 2 wt.% Y2O3 and 1 wt.% CaO formed via decomposition of their nitrates is fully dense and have the optimal bending strength and thermal conductivity of 402.1 MPa and 153.7 W/(m K), respectively.

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.

Mesoscale Thermodynamically motivated Statistical Mechanics based Kinetic Model for Sintering monoliths

NASA Astrophysics Data System (ADS)

Mohan, Nisha

Modeling the evolution of microstructure during sintering is a persistent challenge in ceramics science, although needed as the microstructure impacts properties of an engineered material. Bridging the gap between microscopic and continuum models, kinetic Monte Carlo (kMC) methods provide a stochastic approach towards sintering and microstructure evolution. These kMC models work at the mesoscale, with length and time-scales between those of atomistic and continuum approaches. We develop a sintering/compacting model for the two-phase sintering of boron nitride ceramics and allotropes alike. Our formulation includes mechanisms for phase transformation between h-BN and c-BN and takes into account thermodynamics of pressure and temperature on interaction energies and mechanism rates. In addition to replicating the micro-structure evolution observed in experiments, it also captures the phase diagram of Boron Nitride materials. Results have been analyzed in terms of phase diagrams and crystal growth. It also serves with insights to guide the choice of additives and conditions for the sintering process.While detailed time and spatial resolutions are lost in any MC, the progression of stochastic events still captures plausible local energy minima and long-time temporal developments. DARPA.

Mineral Phases and Release Behaviors of As in the Process of Sintering Residues Containing As at High Temperature

PubMed Central

Wang, Xingrun; Zhang, Fengsong; Nong, Zexi

2014-01-01

To investigate the effect of sintering temperature and sintering time on arsenic volatility and arsenic leaching in the sinter, we carried out experimental works and studied the structural changes of mineral phases and microstructure observation of the sinter at different sintering temperatures. Raw materials were shaped under the pressure of 10 MPa and sintered at 1000~1350°C for 45 min with air flow rate of 2000 mL/min. The results showed that different sintering temperatures and different sintering times had little impact on the volatilization of arsenic, and the arsenic fixed rate remained above 90%; however, both factors greatly influenced the leaching concentration of arsenic. Considering the product's environmental safety, the best sintering temperature was 1200°C and the best sintering time was 45 min. When sintering temperature was lower than 1000°C, FeAsS was oxidized into calcium, aluminum, and iron arsenide, mainly Ca3(AsO4)2 and AlAsO4, and the arsenic leaching was high. When it increased to 1200°C, arsenic was surrounded by a glass matrix and became chemically bonded inside the matrix, which lead to significantly lower arsenic leaching. PMID:24723798

Degradation resistance of 3Y-TZP ceramics sintered using spark plasma sintering

NASA Astrophysics Data System (ADS)

Chintapalli, R.; Marro, F. G.; Valle, J. A.; Yan, H.; Reece, M. J.; Anglada, M.

2009-09-01

Commercially available tetragonal zirconia powder doped with 3 mol% of yttria has been sintered using spark plasma sintering (SPS) and has been investigated for its resistance to hydrothermal degradation. Samples were sintered at 1100, 1150, 1175 and 1600 °C at constant pressure of 100 MPa and soaking for 5 minutes, and the grain sizes obtained were 65, 90, 120 and 800 nm, respectively. Samples sintered conventionally with a grain size of 300 nm were also compared with samples sintered using SPS. Finely polished samples were subjected to artificial degradation at 131 °C for 60 hours in vapour in auto clave under a pressure of 2 bars. The XRD studies show no phase transformation in samples with low density and small grain size (<200 nm), but significant phase transformation is seen in dense samples with larger grain size (>300 nm). Results are discussed in terms of present theories of hydrothermal degradation.

Solution-derived sodalite made with Si- and Ge-ethoxide precursors for immobilizing electrorefiner salt

NASA Astrophysics Data System (ADS)

Riley, Brian J.; Lepry, William C.; Crum, Jarrod V.

2016-01-01

Chlorosodalite has the general form of Na8(AlSiO4)6Cl2 and this paper describes experiments conducted to synthesize sodalite with a solution-based approach to immobilize a simulated spent electrorefiner salt solution containing a mixture of alkali, alkaline earth, and lanthanide chlorides. The reactants used were the salt solution, NaAlO2, and either Si(OC2H5)4 or Ge(OC2H5)4. Additionally, seven different glass sintering aids (at loadings of 5 mass%) were evaluated as sintering aids for consolidating the as-made powders using a cold-press-and-sinter technique. This process of using alkoxide additives for the Group IV component can be used to produce large quantities of sodalite at near-room temperature as compared to a method where colloidal silica was used as the silica source. However, the small particle sizes inhibited densification during heat treatments.

Method for heat treating and sintering metal oxides with microwave radiation

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Meek, Thomas T.

1989-01-01

A method for microwave sintering materials, primarily metal oxides, is described. Metal oxides do not normally absorb microwave radiation at temperatures ranging from about room temperature to several hundred degrees centrigrade are sintered with microwave radiation without the use of the heretofore required sintering aids. This sintering is achieved by enclosing a compact of the oxide material in a housing or capsule formed of a oxide which has microwave coupling properties at room temprature up to at least the microwave coupling temperature of the oxide material forming the compact. The heating of the housing effects the initial heating of the oxide material forming the compact by heat transference and then functions as a thermal insulator for the encased oxide material after the oxide material reaches a sufficient temperature to adequately absorb or couple with microwave radiation for heating thereof to sintering temperature.

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).

The Effects of Spark-Plasma Sintering (SPS) on the Microstructure and Mechanical Properties of BaTiO3/3Y-TZP Composites

PubMed Central

Li, Jing; Cui, Bencang; Wang, Huining; Lin, Yuanhua; Deng, Xuliang; Li, Ming; Nan, Cewen

2016-01-01

Composite ceramics BaTiO3/3Y-TZP containing 0 mol %, 3 mol %, 5 mol %, 7 mol %, and 10 mol % BaTiO3 have been prepared by conventional sintering and spark-plasma sintering (SPS), respectively. Analysis of the XRD patterns and Raman spectra reveal that the phase composition of t-ZrO2, m-ZrO2, and BaTiO3 has been obtained. Our results indicate that SPS can be effective for the decrease in grain size and porosity compared with conventional sintering, which results in a lower concentration of m-ZrO2 and residual stress. Therefore, the fracture toughness is enhanced by the BaTiO3 phase through the SPS technique, while the behavior was impaired by the piezoelectric second phase through conventional sintering. PMID:28773445

Sintering of catalytic nanoparticles: particle migration or Ostwald ripening?

PubMed

Hansen, Thomas W; Delariva, Andrew T; Challa, Sivakumar R; Datye, Abhaya K

2013-08-20

Metal nanoparticles contain the active sites in heterogeneous catalysts, which are important for many industrial applications including the production of clean fuels, chemicals and pharmaceuticals, and the cleanup of exhaust from automobiles and stationary power plants. Sintering, or thermal deactivation, is an important mechanism for the loss of catalyst activity. This is especially true for high temperature catalytic processes, such as steam reforming, automotive exhaust treatment, or catalytic combustion. With dwindling supplies of precious metals and increasing demand, fundamental understanding of catalyst sintering is very important for achieving clean energy and a clean environment, and for efficient chemical conversion processes with atom selectivity. Scientists have proposed two mechanisms for sintering of nanoparticles: particle migration and coalescence (PMC) and Ostwald ripening (OR). PMC involves the mobility of particles in a Brownian-like motion on the support surface, with subsequent coalescence leading to nanoparticle growth. In contrast, OR involves the migration of adatoms or mobile molecular species, driven by differences in free energy and local adatom concentrations on the support surface. In this Account, we divide the process of sintering into three phases. Phase I involves rapid loss in catalyst activity (or surface area), phase II is where sintering slows down, and phase III is where the catalyst may reach a stable performance. Much of the previous work is based on inferences from catalysts that were observed before and after long term treatments. While the general phenomena can be captured correctly, the mechanisms cannot be determined. Advancements in the techniques of in situ TEM allow us to observe catalysts at elevated temperatures under working conditions. We review recent evidence obtained via in situ methods to determine the relative importance of PMC and OR in each of these phases of catalyst sintering. The evidence suggests that, in phase I, OR is responsible for the rapid loss of activity that occurs when particles are very small. Surprisingly, very little PMC is observed in this phase. Instead, the rapid loss of activity is caused by the disappearance of the smallest particles. These findings are in good agreement with representative atomistic simulations of sintering. In phase II, sintering slows down since the smallest particles have disappeared. We now see a combination of PMC and OR, but do not fully understand the relative contribution of each of these processes to the overall rates of sintering. In phase III, the particles have grown large and other parasitic phenomena, such as support restructuring, can become important, especially at high temperatures. Examining the evolution of particle size and surface area with time, we do not see a stable or equilibrium state, especially for catalysts operating at elevated temperatures. In conclusion, the recent literature, especially on in situ studies, shows that OR is the dominant process causing the growth of nanoparticle size. Consequently, this leads to the loss of surface area and activity. While particle migration could be controlled through suitable structuring of catalyst supports, it is more difficult to control the mobility of atomically dispersed species. These insights into the mechanisms of sintering could help to develop sinter-resistant catalysts, with the ultimate goal of designing catalysts that are self-healing.

Low-Temperature Sintering Behavior (≤ 400°C) of Micro-sized Silver Particles Decorated by Silver Nanoparticles Through Surface Iodination

NASA Astrophysics Data System (ADS)

Zhou, Jian; Tang, Hongbo

2018-05-01

This paper introduces a facile and effective route to decorate micro-sized silver particle surfaces with Ag/AgI nanoclusters through a wet chemical reaction at room temperature using iodine and ethanol as reactant and solvent, respectively. Photosensitivity of AgI is utilized in the route, and AgI decomposes into Ag upon contact with sunshine, forming Ag/AgI nanoclusters. The modified micro-sized Ag particles showed sinterability even at 200°C and formed rigid electrical conductive networks at 350°C. Moreover, sintered film containing the modified Ag particles reached the best conductivity, 9.35 mΩ/sq, after sintering at 350°C for 20 min, while the film with untreated control Ag particles obtained its best conductivity at 400°C. The excellent sinterability should be attributed to the nanoclusters which served as a sintering aid during the heating process. However, increase of sintering temperature and time destroyed densification and conductivity of the sintered film containing the modified particles.

Structural and magnetic properties of Ga-substituted Co 2 ‑W hexaferrites

NASA Astrophysics Data System (ADS)

Mahmood, Sami H.; Al Sheyab, Qusai; Bsoul, Ibrahim; Mohsen, Osama; Awadallah, Ahmad

2018-05-01

Precursor powders of BaMg2-xCoxFe16O27 with (x = 0.0, 1.0, and 2.0) were prepared using high-energy ball milling, and the effects of chemical composition and sintering temperature on the structural and magnetic properties were investigated using x-ray diffractometer (XRD), scanning electron microscopy (SEM), and vibrating sample magnetometry (VSM). XRD patterns of the prepared samples indicated that crystallization of pure BaW hexaferrite phase was achieved at sintering temperature of 1300{\\deg} C, while BaM and cubic spinel phase intermediate phases were obtained at lower sintering temperatures of 1100{\\deg} C and 1200{\\deg} C. SEM images revealed improvement of the crystallization of the structural phases, and growth of the particle size with increasing the sintering temperature. The magnetic data of the samples sintered at 1300{\\deg} C revealed an increase of the saturation magnetization from 59.44 emu/g to 72.56 emu/g with increasing Co concentration (x) from 0.0 to 2.0. The coercive field Hc decreased from 0.07 kOe at x = 0.0, to 0.03 kOe at x = 1.0, and then increases to 0.09 kOe at x = 2.0. The thermomagnetic curves of the samples sintered at 1300{\\deg} C confirmed the existence of the W-type phase, and revealed spin reorientation transitions above room temperature.

The influence of Ca/P ratio on the properties of hydroxyapatite bioceramics

NASA Astrophysics Data System (ADS)

Ramesh, S.; Tan, C. Y.; Hamdi, M.; Sopyan, I.; Teng, W. D.

2007-07-01

The paper reports on the effect of Ca/P ratio (1.57, 1.67 and 1.87) on the densification behaviour of nanocrystalline hydroxyapatite (HA) prepared by a chemical precipitation method. Green compacts were prepared and sintered at temperatures ranging from 1000°C to 1350°C. The sintered samples were characterized to determine the HA phase stability, bulk density, hardness, fracture toughness and Young's modulus. XRD analysis revealed that the phase stability was not disrupted throughout the sintering regime employed for HA having Ca/P ratio of 1.57 and 1.67. However, secondary phases were observed for HA having a Ca/P ratio of 1.87 when sintered at high temperatures. In general, regardless of Ca/P ratio, the HA bodies achieved > 95% relative density when sintered at 1100°C-1250°C. The results indicated that the stoichiometric HA (Ca/P ratio = 1.67) exhibited the overall best properties, with the highest hardness of 7.23 GPa and fracture toughness of 1.28 MPam1/2 being attained when sintered at 1000°C-1050°C.

Behavior of New Zealand Ironsand During Iron Ore Sintering

NASA Astrophysics Data System (ADS)

Wang, Zhe; Pinson, David; Chew, Sheng; Rogers, Harold; Monaghan, Brian J.; Pownceby, Mark I.; Webster, Nathan A. S.; Zhang, Guangqing

2016-02-01

A New Zealand ironsand sample was characterized by scanning electron microscopy (SEM), X-ray fluorescence spectroscopy, qualitative and quantitative X-ray diffraction, and electron probe microanalysis. The titanomagnetite-rich ironsand was added into an industrial sinter blend in the proportion of 5 wt pct, and the mixture was uniaxially pressed into cylindrical tablets and sintered in a tube furnace under flowing gas with various oxygen potentials and temperatures to develop knowledge and understanding of the behavior of titanium during sintering. An industrial sinter with the addition of 3 wt pct ironsand was also examined. Both the laboratory and industrial sinters were characterized by optical and SEM. Various morphologies of relict ironsand particles were present in the industrial sinter due to the heterogeneity of sintering conditions, which could be well simulated by the bench-scale sintering experiments. The assimilation of ironsand during sintering in a reducing atmosphere started with the diffusion of calcium into the lattice of the ironsand matrix, and a reaction zone was formed near the boundary within individual ironsand particles where a perovskite phase was generated. With increasing sintering temperature, in a reducing atmosphere, ironsand particles underwent further assimilation and most of the titanium moved from the ironsand particles into a glass phase. In comparison, more titanium remained in the original ironsand particles when sintered in air. Ironsand particles are more resistant to assimilation in an oxidizing atmosphere.

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.

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.

Lightweight Aluminum/Nano composites for Automotive Drive Train Applications

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

Chelluri, Bhanumathi; Knoth, Edward A.; Schumaker, Edward J.

2012-12-14

During Phase I, we successfully processed air atomized aluminum powders via Dynamic Magnetic Compaction (DMC) pressing and subsequent sintering to produce parts with properties similar to wrought aluminum. We have also showed for the first time that aluminum powders can be processed without lubes via press and sintering to 100 % density. This will preclude a delube cycle in sintering and promote environmentally friendly P/M processing. Processing aluminum powders via press and sintering with minimum shrinkage will enable net shape fabrication. Aluminum powders processed via a conventional powder metallurgy process produce too large a shrinkage. Because of this, sinter partsmore » have to be machined into specific net shape. This results in increased scrap and cost. Fully sintered aluminum alloy under this Phase I project has shown good particle-to-particle bonding and mechanical properties. We have also shown the feasibility of preparing nano composite powders and processing via pressing and sintering. This was accomplished by dispersing nano silicon carbide (SiC) powders into aluminum matrix comprising micron-sized powders (<100 microns) using a proprietary process. These composite powders of Al with nano SiC were processed using DMC press and sinter process to sinter density of 85-90%. The process optimization along with sintering needs to be carried out to produce full density composites.« less

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

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

Thömmes, A., E-mail: thoemmes.alexander@gmail.com; Shevtsova, L. I., E-mail: edeliya2010@mail.ru; Laptev, I. S., E-mail: ilya-laptev-nstu@mail.ru

2015-10-27

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

Improved Tubulars for Better Economics in Deep Gas Well Drilling Using Microwave Technology

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

Dinesh Agrawal

2006-09-30

The main objective of the entire research program has been to improve the rate-of-penetration in deep hostile environments by improving the life cycle and performance of coiled-tubing, an important component of a deep well drilling system for oil and gas exploration, by utilizing the latest developments in the microwave materials technology. Based on the results of the Phase I and insurmountable difficulties faced in the extrusion and de-waxing processes, the approach of achieving the goals of the program was slightly changed in the Phase II in which an approach of microwave sintering combined with Cold Isostatic Press (CIP) and joiningmore » (by induction or microwave) has been adopted. This process can be developed into a semicontinuous sintering process if the CIP can produce parts fast enough to match the microwave sintering rates. The main objective of the Phase II research program is to demonstrate the potential to economically manufacture microwave processed coiled tubing with improved performance for extended useful life under hostile coiled tubing drilling conditions. After the completion of the Phase II, it is concluded that scale up and sintering of a thin wall common O.D. size tubing that is widely used in the market is still to be proved and further experimentation and refinement of the sintering process is needed in Phase III. Actual manufacturing capability of microwave sintered, industrial quality, full length tubing will most likely require several million dollars of investment.« less

Improved Tubulars for Better Economics in Deep Gas Well Drilling using Microwave Technology

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

Dinesh Agrawal; Paul Gigl; Mark Hunt

2007-07-31

The main objective of the entire research program has been to improve the rate-of-penetration in deep hostile environments by improving the life cycle and performance of coiled-tubing, an important component of a deep well drilling system for oil and gas exploration, by utilizing the latest developments in the microwave materials technology. Based on the results of the Phase I and insurmountable difficulties faced in the extrusion and de-waxing processes, the approach of achieving the goals of the program was slightly changed in the Phase II in which an approach of microwave sintering combined with Cold Isostatic Press (CIP) and joiningmore » (by induction or microwave) has been adopted. This process can be developed into a semicontinuous sintering process if the CIP can produce parts fast enough to match the microwave sintering rates. The main objective of the Phase II research program is to demonstrate the potential to economically manufacture microwave processed coiled tubing with improved performance for extended useful life under hostile coiled tubing drilling conditions. After the completion of the Phase II, it is concluded that scale up and sintering of a thin wall common O.D. size tubing that is widely used in the market is still to be proved and further experimentation and refinement of the sintering process is needed in Phase III. Actual manufacturing capability of microwave sintered, industrial quality, full length tubing will most likely require several million dollars of investment.« less

Phase stability, porosity distribution and microstructural evolution of amorphous Al{sub 50}Ti{sub 50} powders consolidated by electrical resistance sintering

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

Urban, P., E-mail: purban@us.es; Montes, J. M.; Cintas, J.

2015-03-30

The effect of intensity and duration of the electrical resistance sintering process on the phase stability, porosity distribution and microstructural evolution of Al{sub 50}Ti{sub 50} amorphous powders is studied. The phase transformations during the consolidation process were determined by X-ray diffraction. The porosity distribution was observed by optical and scanning electron microscopy. The amorphous phase is partially transformed to the crystalline phase during the sintering process, and formation of AlTi and AlTi{sub 3} intermetallic compounds occurs for temperatures higher than 300 °C. Finally, it is observed that the compacts core have lower porosity and a higher tendency to the amorphous-crystallinemore » phase transformation than the periphery.« less

Liquid phase sintered ceramic bone scaffolds by combined laser and furnace.

PubMed

Feng, Pei; Deng, Youwen; Duan, Songlin; Gao, Chengde; Shuai, Cijun; Peng, Shuping

2014-08-21

Fabrication of mechanically competent bioactive scaffolds is a great challenge in bone tissue engineering. In this paper, β-tricalcium phosphate (β-TCP) scaffolds were successfully fabricated by selective laser sintering combined with furnace sintering. Bioglass 45S5 was introduced in the process as liquid phase in order to improve the mechanical and biological properties. The results showed that sintering of β-TCP with the bioglass revealed some features of liquid phase sintering. The optimum amount of 45S5 was 5 wt %. At this point, the scaffolds were densified without defects. The fracture toughness, compressive strength and stiffness were 1.67 MPam1/2, 21.32 MPa and 264.32 MPa, respectively. Bone like apatite layer was formed and the stimulation for apatite formation was increased with increase in 45S5 content after soaking in simulated body fluid, which indicated that 45S5 could improve the bioactivity. Furthermore, MG-63 cells adhered and spread well, and proliferated with increase in the culture time.

[Influences of R2O-Al2O3-B2O3-SiO2 system glass and superfine alpha-Al2O3 on the sintering and phase transition of hydroxyapatite ceramics].

PubMed

Wang, Zhiqiang; Chen, Xiaoxu; Cai, Yingji; Lü, Bingling

2003-06-01

The effects of R2O-Al2O3-B2O3-SiO2 system glass and superfine alpha-Al2O3 on the sintering and phase transition of hydroxyapatite (HAP) ceramics were assessed. The results showed that alpha-Al2O3 impeded the sintering of HAP and raised the sintering temperature. When glass and alpha-Al2O3 were used together to reinforce HAP ceramics, better results could be obtained; the bending strength of multiphase HAP ceramics approached 106 MPa when 10% (wt) alpha-Al2O3 and 20%(wt) glass were used and sintered at 1200 for 1 h.

Comparing Sliding-Wear Characteristics of the Electro-Pressure Sintered and Wrought Cobalt

NASA Astrophysics Data System (ADS)

Lee, J. E.; Kim, Y. S.; Kim, T. W.

Dry sliding wear tests of hot-pressure sintered and wrought cobalt were carried out to compare their wear characteristics. Cobalt powders with average size of 1.5µm were electro-pressure sintered to make sintered-cobalt disk wear specimens. A vacuum-induction melted cobalt ingot was hot-rolled at 800°C to a plate, from which wrought-cobalt disk specimens were machined. The specimens were heat treated at various temperatures to vary grain size and phase fraction. Wear tests of the cobalt specimens were carried out using a pin-on-disk wear tester against a glass (83% SiO2) bead at 100N with the constant sliding speed and distance of 0.36m/s and 600m, respectively. Worn surfaces, their cross sections, and wear debris were examined by an SEM. The wear of the cobalt was found to be strongly influenced by the strain-induced phase transformation of ɛ-Co (hcp) to α-Co (fcc). The sintered cobalt had smaller uniform grain size and showed higher wear rate than the wrought cobalt. The higher wear rate of the sintered cobalt was explained by the more active deformation-induced phase transformation than in the wrought cobalt with larger irregular grains.

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.

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.

Evolution of Photometric and Polarimetric Phase Curves of Fine-Grained Water Ice Particles due to Grain Sintering

NASA Astrophysics Data System (ADS)

Jost, B.; Cerubini, R.; Poch, O.; Pommerol, A.; Thomas, N.

2018-06-01

Laboratory photometric and polarimetric phase curves of micrometer-sized water ice particles to elucidate the effect of grain sintering on scattering properties relevant for the analysis of potential plume deposition sites on icy satellites.

Effect of sintering temperature on the electrolysis of TiO2

NASA Astrophysics Data System (ADS)

Li, Ze-quan; Ru, Li-yue; Bai, Cheng-guang; Zhang, Na; Wang, Hai-hua

2012-07-01

The effects of sintering temperature on the microstructure and the conductivity of TiO2 cathodes were studied by examining the phase composition, microstructure, and element contents of the sintered cathodes and the cathodic products using X-ray diffraction and scanning electronic microscopy-energy dispersive spectrometry. The oxygen vacancy, conductivity, average pore diameter, and specific surface area of the sintered cathodes were detected by X-ray photoelectron spectroscopy, four-point probe, and ASPA 2010. The results showed that TiO2 phase transformations occurred, and oxygen vacancies formed with the increase of sintering temperature. The cathodic conductivity improved, but the average pore diameter and the effective response area of the TiO2 cathode were reduced when the sintering temperature increased. These phenomena could weaken the contact between reaction ions and electrons and also had the same effect on the cathodes and the molten salt. Moreover, they were disadvantageous to ion migration, so a lower sintering temperature was favorable for the microstructure of electrolysis. Consequently, the cathodic conductivity may be improved, but the microstructure became compact with the increase of sintering temperature. The cathodic products at different temperatures indicated that the cathodic conductivity was more important for electrolysis.

Optimization of the sintering atmosphere for high-density hydroxyapatite–carbon nanotube composites

PubMed Central

White, Ashley A.; Kinloch, Ian A.; Windle, Alan H.; Best, Serena M.

2010-01-01

Hydroxyapatite–carbon nanotube (HA–CNT) composites have the potential for improved mechanical properties over HA for use in bone graft applications. Finding an appropriate sintering atmosphere for this composite presents a dilemma, as HA requires water in the sintering atmosphere to remain phase pure and well hydroxylated, yet CNTs oxidize at the high temperatures required for sintering. The purpose of this study was to optimize the atmosphere for sintering these composites. While the reaction between carbon and water to form carbon monoxide and hydrogen at high temperatures (known as the ‘water–gas reaction’) would seem to present a problem for sintering these composites, Le Chatelier's principle suggests this reaction can be suppressed by increasing the concentration of carbon monoxide and hydrogen relative to the concentration of carbon and water, so as to retain the CNTs and keep the HA's structure intact. Eight sintering atmospheres were investigated, including standard atmospheres (such as air and wet Ar), as well as atmospheres based on the water–gas reaction. It was found that sintering in an atmosphere of carbon monoxide and hydrogen, with a small amount of water added, resulted in an optimal combination of phase purity, hydroxylation, CNT retention and density. PMID:20573629

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.

Hexagonal OsB 2: Sintering, microstructure and mechanical properties

DOE PAGES

Xie, Zhilin; Lugovy, Mykola; Orlovskaya, Nina; ...

2015-02-07

In this study, the metastable high pressure ReB 2-type hexagonal OsB 2 bulk ceramics was produced by spark plasma sintering. The phase composition, microstructure, and mechanical behavior of the sintered OsB 2 were studied by X-ray diffraction, optical microscopy, TEM, SEM, EDS, and nanoindentation. The produced ceramics was rather porous and contained a mixture of hexagonal (~80 wt.%) and orthorhombic (~20 wt.%) phases as identified by X-ray diffraction and EBSD analysis. Two boron-rich phases, which do not contain Os, were also identified by TEM and SEM/EDS analysis. Nanoindentation measurements yielded a hardness of 31 ± 9 GPa and Young’s modulusmore » of 574 ± 112 GPa, indicating that the material is rather hard and very stiff; but, it is very prone to crack formation and propagation, which is indicative of a very brittle nature of this material. Improvements in the sintering regime are required in order to produce dense, homogeneous and single phase hexagonal OsB 2 bulk ceramics.« less

Evaluation of marginal/internal fit of chrome-cobalt crowns: Direct laser metal sintering versus computer-aided design and computer-aided manufacturing.

PubMed

Gunsoy, S; Ulusoy, M

2016-01-01

The purpose of this study was to evaluate the internal and marginal fit of chrome cobalt (Co-Cr) crowns were fabricated with laser sintering, computer-aided design (CAD) and computer-aided manufacturing, and conventional methods. Polyamide master and working models were designed and fabricated. The models were initially designed with a software application for three-dimensional (3D) CAD (Maya, Autodesk Inc.). All models were fabricated models were produced by a 3D printer (EOSINT P380 SLS, EOS). 128 1-unit Co-Cr fixed dental prostheses were fabricated with four different techniques: Conventional lost wax method, milled wax with lost-wax method (MWLW), direct laser metal sintering (DLMS), and milled Co-Cr (MCo-Cr). The cement film thickness of the marginal and internal gaps was measured by an observer using a stereomicroscope after taking digital photos in ×24. Best fit rates according to mean and standard deviations of all measurements was in DLMS both in premolar (65.84) and molar (58.38) models in μm. A significant difference was found DLMS and the rest of fabrication techniques (P < 0.05). No significant difference was found between MCo-CR and MWLW in all fabrication techniques both in premolar and molar models (P > 0.05). DMLS was best fitting fabrication techniques for single crown based on the results.The best fit was found in marginal; the larger gap was found in occlusal.All groups were within the clinically acceptable misfit range.

Boron Carbide: Stabilization of Highly-Loaded Aqueous Suspensions, Pressureless Sintering, and Room Temperature Injection Molding

NASA Astrophysics Data System (ADS)

Diaz-Cano, Andres

Boron carbide (B4C) is the third hardest material after diamond and cubic boron nitride. It's unique combination of properties makes B4C a highly valuable material. With hardness values around 35 MPa, a high melting point, 2450°C, density of 2.52 g/cm3, and high chemical inertness, boron carbide is used in severe wear components, like cutting tools and sandblasting nozzles, nuclear reactors' control rots, and finally and most common application, armor. Production of complex-shaped ceramic component is complex and represents many challenges. Present research presents a new and novel approach to produce complex-shaped B4C components. Proposed approach allows forming to be done at room temperatures and under very low forming pressures. Additives and binder concentrations are kept as low as possible, around 5Vol%, while ceramics loadings are maximized above 50Vol%. Given that proposed approach uses water as the main solvent, pieces drying is simple and environmentally safe. Optimized formulation allows rheological properties to be tailored and adjust to multiple processing approaches, including, injection molding, casting, and additive manufacturing. Boron carbide samples then were pressureless sintered. Due to the high covalent character of boron carbide, multiples sintering aids and techniques have been proposed in order to achieve high levels of densification. However, is not possible to define a clear sintering methodology based on literature. Thus, present research developed a comprehensive study on the effect of multiple sintering aids on the densification of boron carbide when pressureless sintered. Relative densities above 90% were achieved with values above 30MPa in hardness. Current research allows extending the uses and application of boron carbide, and other ceramic systems, by providing a new approach to produce complex-shaped components with competitive properties.

Effect of sintering time on structural, microstructural and chemical composition of Ni-doped lanthanum gallate perovskites

NASA Astrophysics Data System (ADS)

Colomer, M. T.; Kilner, J. A.

2015-08-01

This work reports the effect of two different sintering times, 6 and 48 h on the structural, microstructural, and chemical features of Ni-doped La0.90Sr0.10GaO3.00-δ. Independently of the sintering time, La0.90Sr0.10Ga1-xNixO3.00-δ (where x=0.10, and 0.20 (mol)) presents a rhombohedral symmetry with a lattice volume that decreases when NiO dopant increases. Besides the perovskite, LaSrGa3.00O7.00 (nominal composition) is present as second phase in all cases. When the samples are doped with NiO, the peaks of this second phase are shifted with respect to the peaks of the pure phase. These shifts suggest that this second phase could admit some Ni ions in its structure. According to the XRD patterns, the amount of the latter phase is larger when sintering time is increased. Electron probe microanalysis (EPMA) indicated that the matrix of the samples sintered for 6 h is constituted by a perovskite with an experimental composition very close to the nominal one. However, when the samples are sintered for 48 h the matrix of each sample is constituted by two perovskites; both with compositional deviations with respect to their nominal one. In particular, a significant Sr depletion compensated by a La increment in the A site is observed. Those compositional deviations could be mainly due to the diffusion of the cations in the bulk and/or from the bulk to the surface of the samples. That diffusion can favour the formation, not only, of a second perovskite with a different composition in relation with the first one formed, but also, the formation of second phases. In addition, a very slight broadening of Bragg peaks of the perovskites sintered for 48 h is observed by XRD and can be related to the presence of two different perovskites in each sample according to EPMA results. By BSEM and EPMA analyses La4.00Ga2.00O9.00 (nominal composition) is also observed as second phase when samples are treated for 48 h.

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.

Processing and nanostructure influences on mechanical properties of thermoelectric materials

NASA Astrophysics Data System (ADS)

Schmidt, Robert David

Thermoelectric (TE) materials are materials that can generate an electric current from a thermal gradient, with possible service in recovery of waste heat such as engine exhaust. Significant progress has been made in improving TE conversion efficiency, typically reported according to the figure of merit, ZT, with several recent papers publishing ZT values above 2. Furthermore, cost reductions may be made by the use of lower cost elements such as Mg, Si, Sn, Pb, Se and S in TE materials, while achieving ZT values between 1.3 and 1.8. To be used in a device, the thermoelectric material must be able to withstand the applied thermal and mechanical forces without failure. However, these materials are brittle, with low fracture toughness typically less than 1.5 MPa-m1/2, and often less than 0.5 MPa-m1/2. For comparison, window glass is approximately 0.75 MPa-m1/2. They have been optimized with nanoprecipitates, nanoparticles, doping, alterations in stoichiometry, powder processing and other techniques, all of which may alter the mechanical properties. In this study, the effect of SiC nanoparticle additions in Mg2Si, SnTe and Ag nanoparticle additions in the skutterudite Ba0.3Co 4Sb12 on the elastic moduli, hardness and fracture toughness are measured. Large changes (˜20%) in the elastic moduli in SnTe 1+x as a function of x at 0 and 0.016 are shown. The effect on mechanical properties of doping and precipitates of CdS or ZnS in a PbS or PbSe matrix have been reported. Changes in sintering behavior of the skutterudite with the Ag nanoparticle additions were explored. Possible liquid phase sintering, with associated benefits in lower processing temperature, faster densification and lower cost, has been shown. A technique has been proposed for determining additional liquid phase sintering aids in other TE materials. The effects of porosity, grain size, powder processing method, and sintering method were explored with YbAl3 and Ba0.3Co4Sb 12, with the porosity dependence of the elastic moduli reported. Only one other TE material has the porosity dependence of the elastic moduli previously reported in the literature, lead-antimony-silver-tellurium (LAST), and the effect of different powder processing and sintering methods has never been reported previously on TE materials.

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 sintering temperature on micro structural and impedance spectroscopic properties of Ni0.5Zn0.5Fe2O4 nano ferrite

NASA Astrophysics Data System (ADS)

Venkatesh, Davuluri; Ramesh, K. V.; Sastry, C. V. S. S.

2017-07-01

Ni-Zn nanoferrite Ni0.5Zn0.5Fe2O4 is prepared by citrate gel auto combustion method and sintered at various temperatures 800, 900, 1000, 1100 and 1200°C. The room temperature x-ray diffraction conforms that the single phase spinel structure is formed. Crystallite size and density were increased with increasing of sintering temperature. From Raman spectroscopy all sintered samples are single phase with cubic spinel structure belong to Fd3m space group. From surface morphology studies it is clearly observed that the particle size increased with increasing of sintering temperature. Impedance spectroscopy revel that increasing of conductivity is due to grain resistance is decreased with increasing of sintering temperature. Cole-Cole plots are studied from impedance data. The electrical modulus analysis shows that non-Debye nature of Ni0.5Zn0.5Fe2O4 ferrite.

Strength and fatigue properties of three-step sintered dense nanocrystal hydroxyapatite bioceramics

NASA Astrophysics Data System (ADS)

Guo, Wen-Guang; Qiu, Zhi-Ye; Cui, Han; Wang, Chang-Ming; Zhang, Xiao-Jun; Lee, In-Seop; Dong, Yu-Qi; Cui, Fu-Zhai

2013-06-01

Dense hydroxyapatite (HA) ceramic is a promising material for hard tissue repair due to its unique physical properties and biologic properties. However, the brittleness and low compressive strength of traditional HA ceramics limited their applications, because previous sintering methods produced HA ceramics with crystal sizes greater than nanometer range. In this study, nano-sized HA powder was employed to fabricate dense nanocrystal HA ceramic by high pressure molding, and followed by a three-step sintering process. The phase composition, microstructure, crystal dimension and crystal shape of the sintered ceramic were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Mechanical properties of the HA ceramic were tested, and cytocompatibility was evaluated. The phase of the sintered ceramic was pure HA, and the crystal size was about 200 nm. The compressive strength and elastic modulus of the HA ceramic were comparable to human cortical bone, especially the good fatigue strength overcame brittleness of traditional sintered HA ceramics. Cell attachment experiment also demonstrated that the ceramics had a good cytocompatibility.

Effects of intergranular phase on the coercivity for MnBi magnets prepared by spark plasma sintering

NASA Astrophysics Data System (ADS)

Cao, J.; Huang, Y. L.; Hou, Y. H.; Zhang, G. Q.; Shi, Z. Q.; Zhong, Z. C.; Liu, Z. W.

2018-05-01

MnBi magnets with a high content of low temperature phase (LTP) and excellent magnetic properties were prepared by spark plasma sintering (SPS) using ball milling powders as precursors without magnetic purification. A complicated intergranular phase, which contains Mn phase, Bi phase, MnO phase, and even amorphous phase in MnBi magnets, was characterized and reported systematically. It was found that the formation of intergranular phase which was contributed by ball milling precursors and sintering mechanism, jointly, had important influence on the magnetic properties. The appropriate content of intergranular phase was beneficial in improving the coercivity due to the strong magnetic isolation effects. The optimum magnetic properties with Mr=26.0 emu/g, Hci= 7.11 kOe and (BH)max=1.53 MGOe at room temperature, and a maximum value Hci= 25.37 kOe at 550 K can be obtained. Strongly favorable magnetic properties make SPSed MnBi magnets an attractive candidate material for small permanent magnets used in high-temperature applications.

The effect of air-abrasion and heat treatment on the fracture behavior of Y-TZP.

PubMed

Passos, Sheila P; Linke, Bernie; Major, Paul W; Nychka, John A

2015-09-01

This study evaluated how the flexural strength and fracture behavior of a zirconia-based ceramic (Y-TZP) were affected by pre- and post-sintering mechanical and thermal treatments. Treatments included sandblasting with different particle size and type (30μm SiO2; 50 and 110μm Al2O3) and thermal conditioning. Two hundred bar-shaped specimens of pre-sintered Y-TZP ceramic (Lava Frame, 3M) were prepared (specimen dimensions: 25mm length×4mm width×0.7mm thickness) and divided into three groups (before sintering, after sintering and after sintering with heating treatment). The before sintering group specimens were airborne-particle abraded prior to dense sintering. Specimens from the after sintering group were airborne-particle abraded after sintering. The after sintering with heating treatment group specimens were submitted to a heating procedure after airborne-particle abrasion. The controls were the specimens that were sintered and not treated with any conditioning procedures. The specimens from all experimental conditions were analyzed by SEM, CLSM and XRD. All specimens were tested in four-point bending. Data were statistically analyzed using one-way ANOVA and Post Hoc tests (α=0.05). A Weibull analysis was used to analyze the strength reliability. Sandblasting pre-sintered zirconia before sintering significantly decreased the flexural strength, except when the smallest blasting particles were used (30μm SiO2). Phase transformation (t-m) was observed after sandblasting and reverse transformation (m-t) was observed after heating. Sandblasting with 30μm SiO2 and 50μm Al2O3 allowed lower phase transformation. However, 30mm SiO2 presented better reliability. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

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.

Isothermal reduction kinetics and mineral phase of chromium-bearing vanadium-titanium sinter reduced with CO gas at 873-1273 K

NASA Astrophysics Data System (ADS)

Yang, Song-tao; Zhou, Mi; Jiang, Tao; Xue, Xiang-xin

2018-02-01

Reduction of chromium-bearing vanadium-titanium sinter (CVTS) was studied under simulated conditions of a blast furnace, and thermodynamics and kinetics were theoretically analyzed. Reduction kinetics of CVTS at different temperatures was evaluated using a shrinking unreacted core model. The microstructure, mineral phase, and variation of the sinter during reduction were observed by X-ray diffraction, scanning electron microscopy, and metallographic microscopy. Results indicate that porosity of CVTS increased with temperature. Meanwhile, the reduction degree of the sinter improved with the reduction rate. Reduction of the sinter was controlled by a chemical reaction at the initial stage and inner diffusion at the final stage. Activation energies measured 29.22-99.69 kJ/mol. Phase transformations in CVTS reduction are as follows: Fe2O3→Fe3O4→FeO→Fe; Fe2TiO5→Fe2TiO4→FeTiO3; FeO·V2O3→V2O3; FeO·Cr2O3→Cr2O3.

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.

Yttria catalyzed microstructural modifications in oxide dispersion strengthened V-4Cr-4Ti alloys synthesized by field assisted sintering technique

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran; Verma, Shailendra Kumar; Dash, Biswaranjan; Agrawal, Priyanka; Subramanian, Karthikeyan

2017-08-01

The present work deals with synthesis, characterisation and elevated temperature mechanical property evaluation of V-4Cr-4Ti and oxide (yttria = 0.3, 0.6 and 0.9 at%) dispersion strengthened V-4Cr-4Ti alloy processed by mechanical alloying and field-assisted sintering, under optimal conditions. Microstructural parameters of both powder and sintered samples were deduced by X-ray diffraction (XRD) and further confirmed with high resolution transmission electron microscopy. Powder diffraction and electron microscopy study show that ball milling of starting elemental powders (V-4Cr-4Ti) with and without yttria addition has resulted in single phase α-V (V-4Cr-4Ti) alloy. Wherein, XRD and electron microscopy images of sintered samples have revealed phase separation (viz., Cr-V and Ti-V) and domain size reduction, with yttria addition. The reasons behind phase separation and domain size reduction with yttria addition during sintering are extensively discussed. Microhardness and high temperature compression tests were done on sintered samples. Yttria addition (0.3 and 0.6 at.%) increases the elevated temperature compressive strength and strain hardening exponent of α-V alloys. High temperature compression test of 0.9 at% yttria dispersed α-V alloy reveals a glassy behaviour.

Enhanced Densification of PM Steels by Liquid Phase Sintering with Boron-Containing Master Alloy

NASA Astrophysics Data System (ADS)

Vattur Sundaram, Maheswaran; Surreddi, Kumar Babu; Hryha, Eduard; Veiga, Angela; Berg, Sigurd; Castro, Fransisco; Nyborg, Lars

2018-01-01

Reaching high density in PM steels is important for high-performance applications. In this study, liquid phase sintering of PM steels by adding gas-atomized Ni-Mn-B master alloy was investigated for enhancing the density levels of Fe- and Mo- prealloyed steel powder compacts. The results indicated that liquid formation occurs in two stages, beginning with the master alloy melting (LP-1) below and eutectic phase formation (LP-2) above 1373 K (1100 °C). Mo and C addition revealed a significant influence on the LP-2 temperatures and hence on the final densification behavior and mechanical properties. Microstructural embrittlement occurs with the formation of continuous boride networks along the grain boundaries, and its severity increases with carbon addition, especially for 2.5 wt pct of master alloy content. Sintering behavior, along with liquid generation, microstructural characteristics, and mechanical testing revealed that the reduced master alloy content from 2.5 to 1.5 wt pct (reaching overall boron content from 0.2 to 0.12 wt pct) was necessary for obtaining good ductility with better mechanical properties. Sintering with Ni-Mn-B master alloy enables the sintering activation by liquid phase formation in two stages to attain high density in PM steels suitable for high-performance applications.

Estimation of Sintering Kinetics of Oxidized Magnetite Pellet Using Optical Dilatometer

NASA Astrophysics Data System (ADS)

Sandeep Kumar, T. K.; Viswanathan, Neelakantan Nurni; Ahmed, Hesham M.; Andersson, Charlotte; Björkman, Bo

2015-04-01

The quality of magnetite pellet is primarily determined by the physico-chemical changes the pellet undergoes as it makes excursion through the gaseous and thermal environment in the induration furnace. Among these physico-chemical processes, the oxidation of magnetite phase and the sintering of oxidized magnetite (hematite) and magnetite (non-oxidized) phases are vital. Rates of these processes not only depend on the thermal and gaseous environment the pellet gets exposed in the induration reactor but also interdependent on each other. Therefore, a systematic study should involve understanding these processes in isolation to the extent possible and quantify them seeking the physics. With this motivation, the present paper focusses on investigating the sintering kinetics of oxidized magnetite pellet. For the current investigation, sintering experiments were carried out on pellets containing more than 95 pct magnetite concentrate from LKAB's mine, dried and oxidized to completion at sufficiently low temperature to avoid sintering. The sintering behavior of this oxidized pellet is quantified through shrinkage captured by Optical Dilatometer. The extent of sintering characterized by sintering ratio found to follow a power law with time i.e., Kt n . The rate constant K for sintering was determined for different temperatures from isothermal experiments. The rate constant, K, varies with temperature as and the activation energy ( Q) and reaction rate constant ( K') are estimated. Further, the sintering kinetic equation was also extended to a non-isothermal environment and validated using laboratory experiments.

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

Synthesis of Nanocrystalline CaWO4 as Low-Temperature Co-fired Ceramic Material: Processing, Structural and Physical Properties

NASA Astrophysics Data System (ADS)

Vidya, S.; Solomon, Sam; Thomas, J. K.

2013-01-01

Nanocrystalline scheelite CaWO4, a promising material for low-temperature co-fired ceramic (LTCC) applications, has been successfully synthesized through a single-step autoignition combustion route. Structural analysis of the sample was performed by powder x-ray diffraction (XRD), Fourier-transform infrared spectroscopy, and Raman spectroscopy. The XRD analysis revealed that the as-prepared sample was single phase with scheelite tetragonal structure. The basic optical properties and optical constants of the CaWO4 nanopowder were studied using ultraviolet (UV)-visible absorption spectroscopy, which showed that the material was a wide-bandgap semiconductor with bandgap of 4.7 eV at room temperature. The sample showed poor transmittance in the ultraviolet region but maximum transmission in the visible/near-infrared regions. The photoluminescence spectra recorded at different temperatures showed intense emission in the green region. The particle size estimated from transmission electron microscopy was 23 nm. The feasibility of CaWO4 for LTCC applications was studied from its sintering behavior. The sample was sintered at a relatively low temperature of 810°C to high density, without using any sintering aid. The surface morphology of the sintered sample was analyzed by scanning electron microscopy. The dielectric constant and loss factor of the sample measured at 5 MHz were found to be 10.50 and 1.56 × 10-3 at room temperature. The temperature coefficient of the dielectric constant was -88.71 ppm/°C. The experimental results obtained in this work demonstrate the potential of nano-CaWO4 as a low-temperature co-fired ceramic as well as an excellent luminescent material.

IMPROVED TUBULARS FOR BETTER ECONOMICS IN DEEP GAS WELL DRILLING USING MICROWAVE TECHNOLOGY

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

Dinesh Agrawal; Paul Gigl; Mahlon Dennis

2005-03-01

The main objective of the research program has been to improve the rate-of-penetration in deep hostile environments by improving the life cycle and performance of coiled-tubing, an important component of a deep well drilling system for oil and gas exploration, by utilizing the latest developments in the microwave materials technology. Originally, it was proposed to accomplish this by developing an efficient and economically viable continuous microwave process to sinter continuously formed/extruded steel powder for the manufacture of seamless coiled tubing and other tubular products. However, based on the results and faced with insurmountable difficulties in the extrusion and de-waxing processes,more » the approach of achieving the goals of the program has been slightly changed. In the continuation proposal an approach of microwave sintering combined with Cold Isostatic Press (CIP) and joining (by induction or microwave) is adopted. This process can be developed into a semi-continuous sintering process if the CIP can produce parts fast enough to match the microwave sintering rates. Originally, the entire program was spread over three phases with the following goals: Phase I: Demonstration of the feasibility concept of continuous microwave sintering process for tubular steel products. Phase II: Design, building and testing of a prototype microwave system which shall be combined with a continuous extruder for steel tubular objects. Phase III: Execution of the plan for commercialization of the technology by one of the industrial partners. However, since some of the goals of the phase I were not completed, an extension of nine months was granted and we continued extrusion experiments, designed and built semicontinuous microwave sintering unit.« less

Phase study and surface morphology of beta-alumina

NASA Astrophysics Data System (ADS)

Tak, S. K.

2018-05-01

Beta alumina ceramic is well known as a polycrystalline ceramic material. The characteristic crystal structure of beta-alumina makes it useful as a separator in sodium sulphur batteries and other electrochemical devices requiring the passage of sodium ions. β"-alumina powders for this study were prepared by zeta process. The pellets were sintered at different microwave power levels and power schedule to optimize the sintering conditions to obtain preferred β" phase with improved microstructure. Phase identification was studied by X-ray diffraction (XRD). XRD analysis shows increase in β'' phase as the sintering temperature was increased from 1400°C to 1600°C. Surface morphology of the pellets was carried out by Scanning Electron microscopy (SEM). SEM studies revealed the formation and growth of platelet grains with interconnected porosity.

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.

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.

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.

Synthesis, analysis and processing of novel materials in the yttrium oxide-aluminum oxide system

NASA Astrophysics Data System (ADS)

Marchal, Julien Claudius

In the current work, liquid feed flame spray pyrolysis (LF-FSP) was used to create three novel nanopowders in the Y2O3-Al 2O3 system: alpha-Al2O3, YAG (garnet Y3Al5O12) and hexagonal Y3Al 5O12. For example, LF-FSP combustion of metalloorganic yttrium and aluminum precursors in a 3/5 ratio forms hexagonal Y3Al5O 12, a newly discovered crystalline phase detailed in this work. The resulting 15-35 nm average particle size, single crystal nanopowders were characterized by TGA-DTA, XRD, HR-TEM, electron diffraction and FTIR. The data was used to establish a model for the crystal structure of this new phase (hexagonal, with crystal parameter of a = 0.736 nm, c = 1.052) consisting of a superlattice of substituted hexagonal YAlO3. YAG has been extensively investigated for its applications as scintillators, phosphors and as a laser host. Fully dispersible, unaggregated single crystal YAG nanopowders with average particle sizes of 35-50 nm were obtained from hexagonal Y3Al5O12 after annealing at 850°C-1200°C (for 2h-8d). The resulting YAG nanopowder was processed into green bodies using cold isostatic pressing after adding binders. 99%+ dense monoliths were obtained after sintering at 1400°C in vacuum (6-8 h), while maintaining grain sizes < 500 nm. The ability to sinter while keeping sub-micron grains differs from present techniques (where translucency is obtained through exaggerated grain growth to 5-10 microns) reported in the literature for sintering polycrystalline YAG, and is the first step for improving polycrystalline YAG laser host optical properties. LF-FSP processing of transition Al2O3 nanopowders converts them to single crystal alpha-Al2O3 nanopowders, previously thought impossible to obtain. The alpha-Al2O 3 nanopowders thus obtained, consist of unaggregated 30-40 nm single particles. These nanopowders were characterized by XRD, HR-TEM, SEM, DLS, FTIR. Green bodies of alpha-Al2O3 nanopowders were sintered to 99% density without sintering aids at 1400°C (6-8 h). After HIPing at 1400°C and 138 MPa, the pellets exhibited some transparency. LF-FSP thus allows synthesis of large quantities of previously unavailable alpha-Al 2O3 nanopowders necessary for developing nanograined alpha-Al 2O3 ceramic monoliths for transparent armors, polycrystalline laser hosts and prosthetic implants. Most importantly, it demonstrates the use of LF-FSP to modify the crystalline phase of nanopowders, without causing aggregation.

Bentonite-Clay Waste Form for the Immobilization of Cesium and Strontium from Fuel Processing Waste Streams

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

Kaminski, Michael D.; Mertz, Carol J.

2016-01-01

The physical properties of a surrogate waste form containing cesium, strontium, rubidium, and barium sintered into bentonite clay were evaluated for several simulant feed streams: chlorinated cobalt dicarbollide/polyethylene glycol (CCD-PEG) strip solution, nitrate salt, and chloride salt feeds. We sintered bentonite clay samples with a loading of 30 mass% of cesium, strontium, rubidium, and barium to a density of approximately 3 g/cm 3. Sintering temperatures of up to 1000°C did not result in volatility of cesium. Instead, there was an increase in crystallinity of the waste form upon sintering to 1000ºC for chloride- and nitrate-salt loaded clays. The nitrate saltmore » feed produced various cesium pollucite phases, while the chloride salt feed did not produce these familiar phases. In fact, many of the x-ray diffraction peaks could not be matched to known phases. Assemblages of silicates were formed that incorporated the Sr, Rb, and Ba ions. Gas evolution during sintering to 1000°C was significant (35% weight loss for the CCD-PEG waste-loaded clay), with significant water being evolved at approximately 600°C.« less

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

Concentrated solar energy used for sintering magnesium titanates for electronic applications

NASA Astrophysics Data System (ADS)

Apostol, Irina; Rodríguez, Jose; Cañadas, Inmaculada; Galindo, Jose; Mendez, Senen Lanceros; de Abreu Martins, Pedro Libȃnio; Cunha, Luis; Saravanan, Kandasamy Venkata

2018-04-01

Solar energy is an important renewable source of energy with many advantages: it is unlimited, clean and free. The main objective of this work was to sinter magnesium titanate ceramics in a solar furnace using concentrated solar energy, which is a novel and original process. The direct conversion of solar power into high temperature makes this process simple, feasible and ecologically viable/environmentally sustainable. We performed the solar sintering experiments at Plataforma Solar de Almeria-CIEMAT, Spain. This process takes place in a vertical axis solar furnace (SF5-5 kW) hosting a mobile flat mirror heliostat, a fixed parabolic mirror concentrator, an attenuator and a test table the concentrator focus. We sintered (MgO)0.63(TiO2)0.37, (MgO)0.49(TiO2)0.51, (MgO)0.50(TiO2)0.50 ceramics samples in air at about 1100 °C for a duration of 16 min, 1 h, 2 h and 3 h in the solar furnace. The MgO/TiO2 ratio and the dwell time was varied in order to obtain phase pure MgTiO3 ceramic. We obtained a pure MgTiO3 geikielite phase by solar sintering of (MgO)0.63(TiO2)0.37 samples at 1100 °C (16 min-3 h). Samples of (MgO)0.63(TiO2)0.37, solar sintered at 1100 °C for 3 h, resulted in well-sintered, non-porous samples with good density (3.46 g/cm3). The sintered samples were analyzed by XRD for phase determination. The grain and surface morphology was observed using SEM. Electrical measurements were carried out on solar sintered samples. The effect of processing parameters on microstructure and dielectric properties were investigated and is presented.

Joining of porous silicon carbide bodies

DOEpatents

Bates, Carl H.; Couhig, John T.; Pelletier, Paul J.

1990-05-01

A method of joining two porous bodies of silicon carbide is disclosed. It entails utilizing an aqueous slip of a similar silicon carbide as was used to form the porous bodies, including the sintering aids, and a binder to initially join the porous bodies together. Then the composite structure is subjected to cold isostatic pressing to form a joint having good handling strength. Then the composite structure is subjected to pressureless sintering to form the final strong bond. Optionally, after the sintering the structure is subjected to hot isostatic pressing to further improve the joint and densify the structure. The result is a composite structure in which the joint is almost indistinguishable from the silicon carbide pieces which it joins.

Improved performance of silicon nitride-based high temperature ceramics

NASA Technical Reports Server (NTRS)

Ashbrook, R. L.

1977-01-01

Recent progress in the production of Si3N4 based ceramics is reviewed: (1) high temperature strength and toughness of hot pressed Si3N4 were improved by using high purity powder and a stabilized ZrO2 additive, (2) impact resistance of hot pressed Si3N4 was increased by the use of a crushable energy absorbing layer, (3) the oxidation resistance and strength of reaction sintered Si3N4 were increased by impregnating reaction sintered silicon nitride with solutions that oxidize to Al2O3 or ZrO2, (4) beta prime SiA1ON compositions and sintering aids were developed for improved oxidation resistance or improved high temperature strength.

Embrittling Components in Sintered Steels: Comparison of Phosphorus and Boron

NASA Astrophysics Data System (ADS)

Danninger, Herbert; Vassileva, Vassilka; Gierl-Mayer, Christian

2017-12-01

In ferrous powder metallurgy, both boron and phosphorus have been known to be sintering activators for a long time. However, the use has been widely different: while P is a standard additive to sintered iron and steels, boron has been frequently studied, but its use in practice is very limited. Both additives are also known to be potentially embrittling, though in a different way. In the present study the differences between the effects of both elements are shown: while P activates sintering up to a certain threshold, in part by stabilizing ferrite, in part by forming a transient liquid phase, boron is the classical additive enhancing persistent liquid phase, being virtually insoluble in the iron matrix. The consequence is that sintered steels can tolerate quite a proportion of phosphorus, depending on composition and sintering process; boron however is strongly embrittling in particular in combination with carbon, which requires establishing a precisely defined content that enhances sintering but is not yet embrittling. The fracture mode of embrittled materials is also different: while with Fe-P the classical intergranular fracture is observed, with boron a much more rugged fracture surface appears, indicating some failure through the eutectic interparticle network but mostly transgranular cleavage. If carbon is added, in both cases transgranular cleavage dominates even in the severely embrittled specimens, indicating that no more the grain boundaries and sintering necks are the weakest links in the systems.

Fabrication of Ce3+ doped Gd3Ga3Al2O12 ceramics by reactive sintering method

NASA Astrophysics Data System (ADS)

Ye, Yong; Liu, Peng; Yan, Dongyue; Xu, Xiaodong; Zhang, Jian

2017-09-01

Ce3+ doped Gd3Ga3Al2O12 (Ce:GGAG) ceramics were fabricated by solid state reactive sintering method in this study. The ceramics were pre-sintered in normal muffle furnace in air at various temperature range from 1410 °C to 1550 °C for 10 h and post-treated by hot isostatic press at 1400 °C/2 h in 200 MPa Ar. The phase and microstructure evolution of Ce: GGAG samples during the densification process were investigated by X-ray diffraction and scanning electron microscope. Pure GGAG phase appeared with the temperature increased to 1200 °C. The fully dense and translucent GGAG ceramics were fabricated by pre-sintering at 1450 °C and followed by HIP treatment.

Preparation of Ti3Al intermetallic compound by spark plasma sintering

NASA Astrophysics Data System (ADS)

Ito, Tsutomu; Fukui, Takahiro

2018-04-01

Sintered compacts of single phase Ti3Al intermetallic compound, which have excellent potential as refractory materials, were prepared by spark plasma sintering (SPS). A raw powder of Ti3Al intermetallic compound with an average powder diameter of 176 ± 56 μm was used in this study; this large powder diameter is disadvantageous for sintering because of the small surface area. The samples were prepared at sintering temperatures (Ts) of 1088, 1203, and 1323 K, sintering stresses (σs) of 16, 32, and 48 MPa, and a sintering time (ts) of 10 min. The calculated relative densities based on the apparent density of Ti3Al provided by the supplier were approximately 100% under all sintering conditions. From the experimental results, it was evident that SPS is an effective technique for dense sintering of Ti3Al intermetallic compounds in a short time interval. In this report, the sintering characteristics of Ti3Al intermetallic compacts are briefly discussed and compared with those of pure titanium compacts.

Characteristics of products generated by selective sintering and stereolithography rapid prototyping processes

NASA Technical Reports Server (NTRS)

Cariapa, Vikram

1993-01-01

The trend in the modern global economy towards free market policies has motivated companies to use rapid prototyping technologies to not only reduce product development cycle time but also to maintain their competitive edge. A rapid prototyping technology is one which combines computer aided design with computer controlled tracking of focussed high energy source (eg. lasers, heat) on modern ceramic powders, metallic powders, plastics or photosensitive liquid resins in order to produce prototypes or models. At present, except for the process of shape melting, most rapid prototyping processes generate products that are only dimensionally similar to those of the desired end product. There is an urgent need, therefore, to enhance the understanding of the characteristics of these processes in order to realize their potential for production. Currently, the commercial market is dominated by four rapid prototyping processes, namely selective laser sintering, stereolithography, fused deposition modelling and laminated object manufacturing. This phase of the research has focussed on the selective laser sintering and stereolithography rapid prototyping processes. A theoretical model for these processes is under development. Different rapid prototyping sites supplied test specimens (based on ASTM 638-84, Type I) that have been measured and tested to provide a data base on surface finish, dimensional variation and ultimate tensile strength. Further plans call for developing and verifying the theoretical models by carefully designed experiments. This will be a joint effort between NASA and other prototyping centers to generate a larger database, thus encouraging more widespread usage by product designers.

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.

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.

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.

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

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

Greenquist, Ian; Tonks, Michael

2016-10-01

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

Sintering, thermal stability and mechanical properties of ZrO2-WC composites obtained by pulsed electric current sintering

NASA Astrophysics Data System (ADS)

Huang, Shuigen; Vanmeensel, Kim; van der Biest, Omer; Vleugels, Jozef

2011-03-01

ZrO2-WC composites exhibit comparable mechanical properties as traditional WC-Co materials, which provides an opportunity to partially replace WC-Co for some applications. In this study, 2 mol.% Y2O3 stabilized ZrO2 composites with 40 vol.% WC were consolidated in the 1150°C-1850°C range under a pressure of 60 MPa by pulsed electric current sintering (PECS). The densification behavior, microstructure and phase constitution of the composites were investigated to clarify the role of the sintering temperature on the grain growth, mechanical properties and thermal stability of ZrO2 and WC components. Analysis results indicated that the composites sintered at 1350°C and 1450°C exhibited the highest tetragonal ZrO2 phase transformability, maximum toughness, and hardness and an optimal flexural strength. Chemical reaction of ZrO2 and C, originating from the graphite die, was detected in the composite PECS for 20 min at 1850°C in vacuum.

Conventional and two step sintering of PZT-PCN ceramics

NASA Astrophysics Data System (ADS)

Keshavarzi, Mostafa; Rahmani, Hooman; Nemati, Ali; Hashemi, Mahdieh

2018-02-01

In this study, PZT-PCN ceramic was made via sol-gel seeding method and effects of conventional sintering (CS) as well as two-step sintering (TSS) were investigated on microstructure, phase formation, density, dielectric and piezoelectric properties. First, high quality powder was achieved by seeding method in which the mixture of Co3O4 and Nb2O5 powder was added to the prepared PZT sol to form PZT-PCN gel. After drying and calcination, pyrochlore free PZT-PCN powder was synthesized. Second, CS and TSS were applied to achieve dense ceramic. The optimum temperature used for 2 h of conventional sintering was obtained at 1150 °C; finally, undesired ZrO2 phase formed in CS procedure was removed successfully with TSS procedure and dielectric and piezoelectric properties were improved compared to the CS procedure. The best electrical properties obtained for the sample sintered by TSS in the initial temperature of T 1 = 1200 °C and secondary temperature of T 2 = 1000 °C for 12 h.

Microstructural and Mechanical Characterization of Ti-12Mo-6Zr Biomaterials Fabricated by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Daoush, Walid Mohamed Rashad Mohamed; Park, Hee Sup; Inam, Fawad; Lim, Byung Kyu; Hong, Soon Hyung

2015-03-01

Ti-12Mo-6Zr/Al2O3 (titanium biomaterial) was prepared by a powder metallurgy route using Spark Plasma Sintering (SPS). Ti, Mo, and Zr powders were mixed by wet milling with different content of alumina nanoparticles (up to 5 wt pct) as an oxide dispersion strengthening phase. Composite powder mixtures were SPSed at 1273 K (1000 °C) followed by heat treatment and quenching. Composite powders, sintered materials, and heat-treated materials were examined using optical and high-resolution electronic microscopy (scanning and transmission) and X-ray diffraction to characterize particle size, surface morphology, and phase identifications for each composition. All sintered materials were evaluated by measuring density, Vickers hardness, and tensile properties. Fully dense sintered materials were produced by SPS and mechanical properties were found to be improved by subsequent heat treatment. The tensile properties as well as the hardness were increased by increasing the content of Al2O3 nanoparticles in the Ti-12Mo-6Zr matrix.

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

Ozturk, Fahrettin; Toros, Serkan; Evis, Zafer

In this study, the diametral strength test of sintered hydroxyapatite was simulated by the finite element software, ABAQUS/Standard. Stress distributions on diametral test sample were determined. The effect of sintering temperature on stress distribution of hydroxyapatite was studied. It was concluded that high sintering temperatures did not reduce the stress on hydroxyapatite. It had a negative effect on stress distribution of hydroxyapatite after 1300 deg. C. In addition to the porosity, other factors (sintering temperature, presence of phases and the degree of crystallinity) affect the diametral strength of the hydroxyapatite.

Effect of the Sintering Temperature on the Formation of Ferroelectric Properties of a Lead Zirconate-Titanate Ceramic

NASA Astrophysics Data System (ADS)

Barabanova, E. V.; Topchiev, A. A.; Malyshkina, O. V.

2018-04-01

Effect of the sintering temperature on the formation of the microstructure, the domain structure, and the ferroelectric properties of a lead zirconate-titanate Pb(Ti x Zr1 - x )O3 piezoelectric ceramics has been studied. It is shown that the ferroelectric phase forms at a sintering temperature of 860°C. At higher sintering temperatures, the main effect on the properties is due to a unit cell deformation and free charge carriers.

The effects of surface finish and grain size on the strength of sintered silicon carbide

NASA Technical Reports Server (NTRS)

You, Y. H.; Kim, Y. W.; Lee, J. G.; Kim, C. H.

1985-01-01

The effects of surface treatment and microstructure, especially abnormal grain growth, on the strength of sintered SiC were studied. The surfaces of sintered SiC were treated with 400, 800 and 1200 grit diamond wheels. Grain growth was induced by increasing the sintering times at 2050 C. The beta to alpha transformation occurred during the sintering of beta-phase starting materials and was often accompanied by abnormal grain growth. The overall strength distributions were established using Weibull statistics. The strength of the sintered SiC is limited by extrinsic surface flaws in normal-sintered specimens. The finer the surface finish and grain size, the higher the strength. But the strength of abnormal sintering specimens is limited by the abnormally grown large tabular grains. The Weibull modulus increases with decreasing grain size and decreasing grit size for grinding.

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.

Accuracy evaluation of metal copings fabricated by computer-aided milling and direct metal laser sintering systems

PubMed Central

Lee, Wan-Sun; Kim, Woong-Chul

2015-01-01

PURPOSE To assess the marginal and internal gaps of the copings fabricated by computer-aided milling and direct metal laser sintering (DMLS) systems in comparison to casting method. MATERIALS AND METHODS Ten metal copings were fabricated by casting, computer-aided milling, and DMLS. Seven mesiodistal and labiolingual positions were then measured, and each of these were divided into the categories; marginal gap (MG), cervical gap (CG), axial wall at internal gap (AG), and incisal edge at internal gap (IG). Evaluation was performed by a silicone replica technique. A digital microscope was used for measurement of silicone layer. Statistical analyses included one-way and repeated measure ANOVA to test the difference between the fabrication methods and categories of measured points (α=.05), respectively. RESULTS The mean gap differed significantly with fabrication methods (P<.001). Casting produced the narrowest gap in each of the four measured positions, whereas CG, AG, and IG proved narrower in computer-aided milling than in DMLS. Thus, with the exception of MG, all positions exhibited a significant difference between computer-aided milling and DMLS (P<.05). CONCLUSION Although the gap was found to vary with fabrication methods, the marginal and internal gaps of the copings fabricated by computer-aided milling and DMLS fell within the range of clinical acceptance (<120 µm). However, the statistically significant difference to conventional casting indicates that the gaps in computer-aided milling and DMLS fabricated restorations still need to be further reduced. PMID:25932310

Accuracy evaluation of metal copings fabricated by computer-aided milling and direct metal laser sintering systems.

PubMed

Park, Jong-Kyoung; Lee, Wan-Sun; Kim, Hae-Young; Kim, Woong-Chul; Kim, Ji-Hwan

2015-04-01

To assess the marginal and internal gaps of the copings fabricated by computer-aided milling and direct metal laser sintering (DMLS) systems in comparison to casting method. Ten metal copings were fabricated by casting, computer-aided milling, and DMLS. Seven mesiodistal and labiolingual positions were then measured, and each of these were divided into the categories; marginal gap (MG), cervical gap (CG), axial wall at internal gap (AG), and incisal edge at internal gap (IG). Evaluation was performed by a silicone replica technique. A digital microscope was used for measurement of silicone layer. Statistical analyses included one-way and repeated measure ANOVA to test the difference between the fabrication methods and categories of measured points (α=.05), respectively. The mean gap differed significantly with fabrication methods (P<.001). Casting produced the narrowest gap in each of the four measured positions, whereas CG, AG, and IG proved narrower in computer-aided milling than in DMLS. Thus, with the exception of MG, all positions exhibited a significant difference between computer-aided milling and DMLS (P<.05). Although the gap was found to vary with fabrication methods, the marginal and internal gaps of the copings fabricated by computer-aided milling and DMLS fell within the range of clinical acceptance (<120 µm). However, the statistically significant difference to conventional casting indicates that the gaps in computer-aided milling and DMLS fabricated restorations still need to be further reduced.

Synthesis of Silicon Nitride and Silicon Carbide Nanocomposites through High Energy Milling of Waste Silica Fume for Structural Applications

NASA Astrophysics Data System (ADS)

Suri, Jyothi

Nanocomposites have been widely used in a multitude of applications in electronics and structural components because of their improved mechanical, electrical, and magnetic properties. Silicon nitride/Silicon carbide (Si 3N4/SiC) nanocomposites have been studied intensively for low and high temperature structural applications, such as turbine and automobile engine components, ball bearings, turbochargers, as well as energy applications due to their superior wear resistance, high temperature strength, high oxidation resistance and good creep resistance. Silica fume is the waste material produced during the manufacture of silicon and ferro-silicon alloys, and contains 94 to 97 wt.% SiO2. In the present dissertation, the feasibility of using waste silica fume as the raw material was investigated to synthesize (I) advanced nanocomposites of Si3N4/SiC, and (2) porous silicon carbide (SiC) for membrane applications. The processing approach used to convert the waste material to advanced ceramic materials was based on a novel process called, integrated mechanical and thermal activation process (IMTA) process. In the first part of the dissertation, the effect of parameters such as carbothermic nitridation and reduction temperature and the graphite concentration in the starting silica fume plus graphite mixture, were explored to synthesize nanocomposite powders with tailored amounts of Si3N4 and SiC phases. An effective way to synthesize carbon-free Si3N 4/SiC composite powders was studied to provide a clear pathway and fundamental understanding of the reaction mechanisms. Si3N4/SiC nanocomposite powders were then sintered using two different approaches, based on liquid phase sintering and spark plasma sintering processes, with Al 2O3 and Y2O3 as the sintering aids. The nanocomposites were investigated for their densification behavior, microstructure, and mechanical properties. Si3N4/SiC nanocomposites thus obtained were found to possess superior mechanical properties at much lower costs. The second part of the work has comprised of the successful fabrication of bilayered SiC membranes with a graded porosity, consisting of porous nano-SiC layer on the surface of a porous coarse-grained SiC support layer. The effect of different particle sizes of SiC in the support layers was systematically studied. Also, the effects of sintering temperature were investigated to control the pore size, particle size and overall density of the bi-layered SiC membrane.

Investigation of Sintering Temperature on Attrition Resistance of Highly Porous Diatomite Based Material

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

Garderen, Noemie van; Clemens, Frank J.; Scharf, Dagobert

2010-05-30

Highly porous diatomite based granulates with a diameter of 500 mum have been produced by an extrusion method. In order to investigate the relation between microstructure, phase composition and attrition resistance of the final product, the granulates were sintered between 800 and 1300 deg. C. Mean pore size of the granulates was evaluated by Hg-porosimetry. An increase of the pore size is observed in the range of 3.6 nm to 40 mum with increasing sintering temperature. Higher mean pore radii of 1.6 mum and 5.7 mum obtained by sintering at 800 and 1300 deg. C respectively. X-ray diffraction shows thatmore » mullite phase appears at 1100 deg. C due to the presence of clay. At 1100 deg. C diatomite (amorphous silicate) started to transform into alpha-cristobalite. Attrition resistance was determined by evaluating the amount of ground material passed through a sieve with a predefined mesh size. It was observed that a material sintered at high temperature leads to an increase of attrition resistance due to the decrease of total porosities and phase transformation. Due to the reason that attrition resistance significantly increased by sintering the granulates at higher temperature, a so called attrition resistance index was determined in order to compare all the different attrition resistance values. This attrition resistance index was determined by using the exponential component of the equation obtained from attrition resistance curves. It permits comparison of the attrition behaviour without a time influence.« less

Microwave sintering of nanopowder ZnNb2O6: Densification, microstructure and microwave dielectric properties

NASA Astrophysics Data System (ADS)

Bafrooei, H. Barzegar; Nassaj, E. Taheri; Hu, C. F.; Huang, Q.; Ebadzadeh, T.

2014-12-01

High density ZnNb2O6 ceramics were successfully fabricated by microwave sintering of ZnO-Nb2O5 and ZnNb2O6 nanopowders. Phase formation, microstructure and microwave electrical properties of the microwave sintered (MS) and microwave reaction sintered (MRS) specimens were examined using X-ray diffraction, field emission scanning electron microscopy and microwave dielectric properties measurement. Specimens were sintered in a temperature range from 950 to 1075 °C for 30 min at an interval of 25 °C using a microwave furnace operated at 2.45 GHz frequency, 3 kW power. XRD pattern revealed the formation of pure columbite phase of ZnNb2O6. The SEM micrographs show grain growth and reduction in porosity of specimens with the increase in sintering temperature. Good combination of microwave dielectric properties (εr~23.6, Qf~64,300 GHz and τf~-66 ppm/°C and εr~24, Qf~75,800 GHz and τf~-64 ppm/°C) was obtained for MS- and MRS-prepared samples at 1000 °C and 1050 °C for 30 min, respectively.

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.

Magnetic and magneto elastic properties of cobalt ferrite ceramic compacted through cold isostatic pressing

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

Indla, Srinivas; Das, Dibakar, E-mail: ddse@uohyd.ernet.in; Chelvane, Arout

2016-05-06

Nano crystalline CoFe{sub 2}O{sub 4} powder was prepared by combustion synthesis method. As synthesized powder was calcined at an appropriate condition to remove the impurities and to promote phase formation. Phase pure CoFe{sub 2}O{sub 4} powder was pressed into cylindrical rod at an applied pressure of 200 MPa using a cold isostatic pressing. Sintering of the green compact at 1350°c for 12 hrs resulted in sintered cylindrical rod with ~85% of the theoretical density. Single phase cubic spinel structure was observed in the powder x-ray diffraction pattern of the sintered pellet. Scanning electron micrographs (SEM) of the as sintered pelletmore » revealed the microstructure to be composed of ferrite grains of average size ~4 µm. Saturation magnetization of 72 emu/g and coercivity of 355 Oe were observed for cobalt ferrite sample. The magnetostriction was measured on a circular disc (12 mm diameter and 12 mm length) with the strain gauge (350 Ω) mounted on the flat surface of the circular disc. Magnetostriciton of 180 ppm and strain derivative of 1 × 10{sup −9} m/A were observed for the sintered CoFe{sub 2}O{sub 4} sample.« less

Enhanced Sintering of TiNi Shape Memory Foams under Mg Vapor Atmosphere

NASA Astrophysics Data System (ADS)

Aydoğmuş, Tarik; Bor, Şakir

2012-12-01

TiNi alloy foams are promising candidates for biomaterials to be used as artificial orthopedic implant materials for bone replacement applications in biomedical sector. However, certain problems exist in their processing routes, such as formation of unwanted secondary intermetallic phases leading to brittleness and deterioration of shape memory and superelasticity characteristics; and the contamination during processing resulting in oxides and carbonitrides which affect mechanical properties negatively. Moreover, the eutectic reaction present in Ti-Ni binary system at 1391 K (1118 °C) prevents employment of higher sintering temperatures (and higher mechanical properties) even when equiatomic prealloyed powders are used because of Ni enrichment of TiNi matrix as a result of oxidation. It is essential to prevent oxidation of TiNi powders during processing for high-temperature (>1391 K i.e., 1118 °C) sintering practices. In the current study, magnesium powders were used as space holder material to produce TiNi foams with the porosities in the range of 40 to 65 pct. It has been found that magnesium prevents secondary phase formation and contamination. It also prevents liquid phase formation while enabling employment of higher sintering temperatures by two-step sintering processing: holding the sample at 1373 K (1100 °C) for 30 minutes, and subsequently sintering at temperatures higher than the eutectic temperature, 1391 K (1118 °C). By this procedure, magnesium may allow sintering up to temperatures close to the melting point of TiNi. TiNi foams produced with porosities in the range of 40 to 55 pct were found to be acceptable as implant materials in the light of their favorable mechanical properties.

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.

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.

Sintering of Pt nanoparticles via volatile PtO 2: Simulation and comparison with experiments

DOE PAGES

Plessow, Philipp N.; Abild-Pedersen, Frank

2016-09-23

It is a longstanding question whether sintering of platinum under oxidizing conditions is mediated by surface migration of Pt species or through the gas phase, by PtO 2(g). Clearly, a rational approach to avoid sintering requires understanding the underlying mechanism. A basic theory for the simulation of ripening through the vapor phase has been derived by Wynblatt and Gjostein. Recent modeling efforts, however, have focused entirely on surface-mediated ripening. In this work, we explicitly model ripening through PtO 2(g) and study how oxygen pressure, temperature, and shape of the particle size distribution affect sintering. On the basis of the availablemore » data on α-quartz, adsorption of monomeric Pt species on the support is extremely weak and has therefore not been explicitly simulated, while this may be important for more strongly interacting supports. Our simulations clearly show that ripening through the gas phase is predicted to be relevant. Assuming clean Pt particles, sintering is generally overestimated. This can be remedied by explicitly including oxygen coverage effects that lower both surface free energies and the sticking coefficient of PtO 2(g). Additionally, mass-transport limitations in the gas phase may play a role. Using a parameterization that accounts for these effects, we can quantitatively reproduce a number of experiments from the literature, including pressure and temperature dependence. Lastly, this substantiates the hypothesis of ripening via PtO 2(g) as an alternative to surface-mediated ripening.« less

Influence of Alkali Resistant (Ar) Fibreglass in Porcelain Clay for Manufacturing Vitrified Clay Pipes

NASA Astrophysics Data System (ADS)

Ikhmal Hanapi, Muhammad; Ahmad, Sufizar; Taib, Hariati; Ismail, Al Emran; Nasrull Abdol Rahman, Mohd; Salleh, Salihatun Md; Sadikin, Azmahani; Mahzan, Shahruddin

2017-10-01

The aim of this work is to determine the characteristics of porcelain ceramic with influence of milled Alkali Resistant (AR) fiberglass for manufacturing vitrified clay pipes. In this study, raw materials consist of porcelain clay and AR fiberglass were refined into powders less than 90μm. Subsequently, these samples were compacted into cylindrical pellet for chemical analysis using X-Ray Fluorescence (XRF). The ceramic sample was produced by mixing different weight percentage of AR glass to porcelain ceramic with 3 wt%, 6 wt%, 9 wt% and 12 wt%. Subsequently, the sample was compacted with 3 ton of pressure load and sintered at 900 °C, 1000 °C, 1100 °C and 1200 °C. The phase identification by using X-Ray Diffraction (XRD) and microstructural analysis were performed for the sintered sample. Chemical analysis revealed that the significant element for all raw material are SiO2, Al2O3, Na2O and K2O. Phase identification analysis shown that sample sintered at 1000 °C produces quartz (SiO2), berlinite (AlPO4), albite (NaAlSi3O8) and calcium-magnesium-aluminum-silicate (CaMgAlSiO). The formation of primary mullite was observed in sample sintered at 1100 °C. The image of microstructural morphology denoted that the formation of glassy phase with decreasing amount of void when sintering temperature and addition of AR glass were increased, which correspond well to phase identification analysis.

Interfacial reactions and wetting in Al-Mg sintered by powder metallurgy process

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

Faisal, Heny, E-mail: faisal@physics.its.ac.id; Darminto,; Triwikantoro,

2016-04-19

Was conducted to analyze the effect of temperature variation on the bonding interface sintered composite Al-Mg and analyze the effect of variations of the density and hardness sinter. Research carried out by the base material powders of Al, Mg powder and solvent n-butanol. The method used in this study is a powder metallurgy, with a composition of 60% volume fraction of Al - 40% Mg. Al-Mg mixing with n-butanol for 1 hour at 500 rpm. Then the emphasis (cold comression) with a size of 1.4 cm in diameter dies and height of 2.8 cm, is pressed with a force of 20 MPa and heldmore » for 15 minutes. After the sample into pellets, then sintered at various temperatures 300 °C, 350 °C, 400 °C and 450 °C. Characterization is done by using the testing green density, sintered density, X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), vickers microhardness, and press test. XRD data analysis done by using X’Pert High Score Plus (HSP) to determine whether there is a new phase is formed. Test results show that the sintered density increasing sintering temperature, the resulting density is also increasing (shrinkage). However, at a temperature of 450 °C decreased (swelling). With the increased sinter density, interfacial bonding getting Kuta and more compact so that its hardness is also increased. From the test results of SEM / EDX, there Mg into Al in the border area. At temperatures of 300 °C, 350 °C, 400 °C, the phase formed is Al, Mg and MgO. While phase is formed at a temperature of 450 °C is aluminum magnesium (Al{sub 3}Mg{sub 2}), Aluminum Magnesium Zinc (AlMg{sub 2}Zn).« less

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.

A study on flash sintering and related phenomena in titania and its composite with alumina

NASA Astrophysics Data System (ADS)

Shikhar

In 2010, Cologna et. al. [1] reported that with a help of small electric field 120 Vcm-1, the sintering temperature of 3 mol % yittria stabilized zirconia could be brought down to 850°C from 1450°C. On top of reducing the temperature requirements, the green sample could be sintered from starting density of 50% to near full density in mere 5 seconds, a sintering rate three orders of magnitude higher than conventional methods. This discovery led to the emergence of a new field of enhanced sintering with electric field, named "Flash Sintering". The objective of this thesis is to understand the phenomenological behavior of flash-sintering and related phenomena on titania and its composites with alumina at elevated temperature. The possible mechanisms to explain flash sintering are discussed: Joule heating and the avalanche of defect generation [2], both induced by the rapid rise in conductivity just before the onset of the flash. Apparently, both mechanisms play a role. The thesis covers the response of pure titania and composites of titania-alumina under flash and compared with conventional sintering. We start with the sintering behavior of pure titania and observe lowering of sintering temperature requirements with higher applied electric field. The conductivity of titania during flash is also measured, and compared with the nominal conductivity of titania at equivalent temperatures. The conductivity during flash is determined to be have a different activation energy. For the composites of titania-alumina, effect of flash on the constrained sintering was studied. It is a known fact that sintering of one component of composite slows down when the other component of a different densification rate is added to it, called constrained sintering. In our case, large inclusions of alumina particles were added to nano-grained titania green compact that hindered its densification. Flash sintering was found to be overcoming this problem and near full densification was achieved. In another experiment, effect of high current density and hold time under flash on the chemical reaction (phase transformation) of titania and alumina to form Al2TiO5 is studied. It was found that not only flash enhances the kinetics of reaction when compared with conventional heating at equivalent temperatures, but also brought down the phase transformation temperature for this spinel formation, as reported by the phase diagram. In-situ X-ray diffraction experiments were performed at the synchrotron facility in Argonne National Laboratory. The specimen temperature were measured during the experiment on the basis of peak shift with temperature and were found to be matching with our predicted values by Black-Body-Radiation model. We also observed the instant evolution of texture in grain orientation of pure titania under flash and their disappearance as the fields were switched off. Study on chemical kinetics between titania and alumina were also performed which supported our findings of in-house experiments.

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.

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.

Effects of various additives on sintering of aluminum nitride

NASA Technical Reports Server (NTRS)

Komeya, K.; Inoue, H.; Tsuge, A.

1982-01-01

Effects of thirty additives on sintering A/N were investigated. The addition of alkali earth oxides and rare earth oxides gave fully densified aluminum nitride. This is due to the formation of nitrogen-containing aluminate liquid in the system aluminum nitride-alkali earth oxides or rare earth oxides. Microstructural studies of the sintered specimens with the above two types of additives suggested that the densification was due to the liquid phase sintering. Additions of silicon compounds resulted in poor densification by the formation of highly refractory compounds such as A/N polytypes.

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.

Multi-Scale Modeling of Liquid Phase Sintering Affected by Gravity: Preliminary Analysis

NASA Technical Reports Server (NTRS)

Olevsky, Eugene; German, Randall M.

2012-01-01

A multi-scale simulation concept taking into account impact of gravity on liquid phase sintering is described. The gravity influence can be included at both the micro- and macro-scales. At the micro-scale, the diffusion mass-transport is directionally modified in the framework of kinetic Monte-Carlo simulations to include the impact of gravity. The micro-scale simulations can provide the values of the constitutive parameters for macroscopic sintering simulations. At the macro-scale, we are attempting to embed a continuum model of sintering into a finite-element framework that includes the gravity forces and substrate friction. If successful, the finite elements analysis will enable predictions relevant to space-based processing, including size and shape and property predictions. Model experiments are underway to support the models via extraction of viscosity moduli versus composition, particle size, heating rate, temperature and time.

Raman and dielectric studies of GdMnO3 bulk ceramics synthesized from nano powders

NASA Astrophysics Data System (ADS)

Samantaray, S.; Mishra, D. K.; Roul, B. K.

2017-05-01

Nanocrystalline GdMnO3 (GMO) powders has been synthesized by a simple chemical route i. e. pyrophoric reaction technique and then sintered in the form of bulk pellet at 850°C for 24 hours by adopting slow step sintering schedule. It is observed that by reducing the particles size, chemical route enhances the mixing process as well as decreasing the sintering temperature to get single phase material system in compared to the polycrystalline sample prepared directly from the micron sized commercial powder. Raman spectroscopic studies confirm that the sample is in single phase without any detectable impurity. Frequency dependent dielectric properties i.e., dielectric constant (K) and dielectric loss (tanδ) of GMO ceramics sintered at 850°C for 24 hours were studied at room temperature. The sample showed high K value (˜2736) in the frequency of 100 Hz at room temperature.

Indentation Behavior and Mechanical Properties of Tungsten/Chromium co-Doped Bismuth Titanate Ceramics Sintered at Different Temperatures

PubMed Central

Xu, Jiageng; Chen, Yu; Tan, Zhi; Nie, Rui; Wang, Qingyuan; Zhu, Jianguo

2018-01-01

A sort of tungsten/chromium(W/Cr) co-doped bismuth titanate (BIT) ceramics (Bi4Ti2.95W0.05O12.05 + 0.2 wt % Cr2O3, abbreviate to BTWC) are ordinarily sintered between 1050 and 1150 °C, and the indentation behavior and mechanical properties of ceramics sintered at different temperatures have been investigated by both nanoindentation and microindentation technology. Firstly, more or less Bi2Ti2O7 grains as the second phase were found in BTWC ceramics, and the grain size of ceramics increased with increase of sintering temperatures. A nanoindentation test for BTWC ceramics reveals that the testing hardness of ceramics decreased with increase of sintering temperatures, which could be explained by the Hall–Petch equation, and the true hardness could be calculated according to the pressure-state-response (PSR) model considering the indentation size effect, where the value of hardness depends on the magnitude of load. While, under the application of microsized Vickers, the sample sintered at a lower temperature (1050 °C) gained four linearly propagating cracks, however, they were observed to shorten in the sample sintered at a higher temperature (1125 °C). Moreover, both the crack deflection and the crack branching existed in the latter. The hardness and the fracture toughness of BTWC ceramics presented a contrary variational tendency with increase of sintering temperatures. A high sintering tends to get a lower hardness and a higher fracture toughness, which could be attributed to the easier plastic deformation and the stronger crack inhibition of coarse grains, respectively, as well as the toughening effect coming from the second phase. PMID:29584677

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.

The improved mechanical properties of β-CaSiO3 bioceramics with Si3N4 addition.

PubMed

Pan, Ying; Zuo, Kaihui; Yao, Dongxu; Yin, Jinwei; Xin, Yunchuan; Xia, Yongfeng; Liang, Hanqin; Zeng, Yuping

2015-03-01

The motivation of this study is to investigate the effect of Si3N4 addition on the sinterability of β-CaSiO3 ceramics. β-CaSiO3 ceramics with different content of Si3N4 were prepared at the sintering temperature ranging from 1000°C to 1150°C. The results showed that Si3N4 can be successfully used as sintering additive by being oxidized to form SiO2. The β-CaSiO3 ceramics with 3wt% Si3N4 sintered at 1100°C revealed flexural strength, hardness and fracture toughness of 157.2MPa, 4.4GPa and 2.3MPam(1/2) respectively, which was much higher than that of pure β-CaSiO3 ceramics (41.1MPa, 1.0GPa, 1.1MPam(1/2)). XRD analysis and SEM observation indicated that the main phase maintained to be β-phase after sintering. Copyright © 2015 Elsevier Ltd. All rights reserved.

[Preparing of Al2O3/ZrO2 composite dental ceramics through isostatic pressing technology].

PubMed

Liang, Xiao-Feng; Yin, Guang-Fu; Yang, Shi-Yuan; Wang, Jun-Xia

2006-08-01

To find out how to prepare high-density dental ceramics through isostatic pressing so that sintering shrinkage will be reduced. To prepare Al2O3/ZrO2 composite powder first, then to mold through dry-pressing, and to shape the green-body through isostatic pressing. The green-bodies were sintered at the temperature of 1 400 degrees C and kept at the temperature for different period of time (2 h, 3 h, 4 h). After that, the density and fracture strength were measured and the microstructure observed by scanning electron microscope (SEM). The sample product's density, line-shrinkage, and fracture strength of ceramics was rising with the sintering time lengthened. The sample product kept under the temperature of 1 400 degrees C for 4 hours, the fracture strength was (497.27 +/- 78.45) MPa and glass phase distributed evenly in the ceramics and the grains were integrated owing to the glass phase. The longer the sintering time, the more even the microstructure was. The sintering quality and the efficiency were improved through isostatic pressing.

Porous Nb-Ti based alloy produced from plasma spheroidized powder

NASA Astrophysics Data System (ADS)

Li, Qijun; Zhang, Lin; Wei, Dongbin; Ren, Shubin; Qu, Xuanhui

Spherical Nb-Ti based alloy powder was prepared by the combination of plasma spheroidization and mechanical alloying. Phase constituents, microstructure and surface state of the powder, and pore characteristics of the resulting porous alloy were investigated. The results show that the undissolved W and V in the mechanically alloyed powder is fully alloyed after spheroidization, and single β phase is achieved. Particle size of the spheroidized powder is in the range of 20-110 μm. With the decrease of particle size, a transformation from typical dendrite solidification structure to fine cell microstructure occurs. The surface of the spheroidized powder is coated by a layer of oxides consisting mainly of TiO2 and Nb2O5. Probabilities of sinter-neck formation and particle coalescence increases with increasing sintering temperature. Porous skeleton with relatively homogeneous pore distribution and open pore channel is formed after vacuum sintering at 1700 °C, and the porosity is 32%. The sintering kinetic analysis indicates that grain boundary diffusion is the primary mass transport mechanism during sintering process.

A device for microwave sintering large ceramic articles

DOEpatents

Kimrey, H.D. Jr.

1987-07-24

A microwave sintering system is provided for uniform sintering of large and/or irregular shapes ceramic articles at microwave frequencies of at least 28 GHz in the hundreds of kilowatts power range in an untuned cavity. A 28 GHz, 200 kw gyrotron with variable power output is used as the microwave source connected to an untuned microwave cavity formed of an electrically conductive housing. The part to be sintered is placed in the cavity and supported on a removable high temperature table in a central location within the cavity. The part is surrounded by a microwave transparent bulk insulating material to reduce thermal heat loss at the part surfaces and maintain more uniform temperature. The cavity may be operated at a high vacuum to aid in preventing arcing. The system allows controlled increased heating rates of greater than 200/degree/C/min to provide rapid heating of a ceramic part to a selected sintering temperature where it is maintained by regulating the microwave power applied to the part. As a result of rapid heating, the extent on non-isothermal processes such as segregation of impurities to the grain boundaries are minimized and exaggerated grain growth is reduced, thereby strengthening the mechanical properties of the ceramic part being sintered. 1 fig.

Improved microstructure and thermoelectric properties of iodine doped indium selenide as a function of sintering temperature

NASA Astrophysics Data System (ADS)

Dhama, Pallavi; Kumar, Aparabal; Banerji, P.

2018-04-01

In this paper, we explored the effect of sintering temperature on the microstructure, thermal and electrical properties of iodine doped indium selenide in the temperature range 300 - 700 K. Samples were prepared by a collaborative process of vacuum melting, ball milling and spark plasma sintering at 570 K, 630 K and 690 K. Single phase samples were obtained at higher sintering temperature as InSe is stable only at lower temperature. With increasing sintering temperature, densities of the samples were found to improve with larger grain size formation. Negative values of Seebeck coefficient were observed which indicates n-type carrier transport. Seebeck coefficient increases with sintering temperature and found to be the highest for the sample sintered at 690 K. Thermal conductivity found to be lower in the samples sintered at lower temperatures. The maximum thermoelectric figure of merit found to be ˜ 1 at 700 K due to the enhanced power factor as a result of improved microstructure.

Composition and annealing effects on superconductivity in sintered and arc-melted Fe1+εTe0.5Se0.5

NASA Astrophysics Data System (ADS)

Foreman, M. M.; Ponti, G.; Mozaffari, S.; Markert, J. T.

2018-03-01

We present the results of x-ray diffraction, electrical resistivity, and ac magnetic susceptibility measurements on specimens of the “11”-structure superconductor Fe1+εTe0.50Se0.50 (0 ≤ ε ≤ 0.15). Samples were initially either sintered in sealed quartz tubes or melted in a zirconium-gettered arc furnace. Sintered samples were fired two to three times at temperatures of 425°C, 600°C, or 675°C, while arc-melted samples were studied both asmelted and after annealing at 650°C. X-ray diffraction data show a predominant PbO-type tetragonal phase, with a secondary hexagonal NiAs-type phase; for sintered specimens annealed at 600°C, the secondary phase decreases as ε increases over the range 0 ≤ ε ≤ 0.10, with the composition Fe1.10Te0.5Se0.5 exhibiting x-ray phase purity. A higher annealing temperature of 675°C provided such tetragonal phase purity at the composition Fe1.05Te0.5Se0.5. The resistive superconducting transition temperature Tc was nearly independent of the iron concentration 1+ε, suggesting a single superconducting phase, while the magnetic screening fraction varied greatly with concentration and conditions, peaking at ɛ = 0.07, indicating that the amount of superconducting phase is strongly dependent on conditions. We propose that the behaviour can also be viewed in terms of an electron-doped, chalcogen-deficient stoichiometry.

Challenges and Recent Developments in Hearing Aids: Part II. Feedback and Occlusion Effect Reduction Strategies, Laser Shell Manufacturing Processes, and Other Signal Processing Technologies

PubMed Central

Chung, King

2004-01-01

This is the second part of a review on the challenges and recent developments in hearing aids. Feedback and the occlusion effect pose great challenges in hearing aid design and usage. Yet, conventional solutions to feedback and the occlusion effect often create a dilemma: the solution to one often leads to the other. This review discusses the advanced signal processing strategies to reduce feedback and some new approaches to reduce the occlusion effect. Specifically, the causes of three types of feedback (acoustic, mechanical, and electromagnetic) are discussed. The strategies currently used to reduce acoustic feedback (i.e., adaptive feedback reduction algorithms using adaptive gain reduction, notch filtering, and phase cancellation strategies) and the design of new receivers that are built to reduce mechanical and electromagnetic feedback are explained. In addition, various new strategies (i.e., redesigned sound delivery devices and receiver-in-the-ear-canal hearing aid configuration) to reduce the occlusion effect are reviewed. Many manufacturers have recently adopted laser shell-manufacturing technologies to overcome problems associated with manufacturing custom hearing aid shells. The mechanisms of selected laser sintering and stereo lithographic apparatus and the properties of custom shells produced by these two processes are reviewed. Further, various new developments in hearing aid transducers, telecoils, channel-free amplification, open-platform programming options, rechargeable hearing aids, ear-level frequency modulated (FM) receivers, wireless Bluetooth FM systems, and wireless programming options are briefly explained and discussed. Finally, the applications of advanced hearing aid technologies to enhance other devices such as cochlear implants, hearing protectors, and cellular phones are discussed. PMID:15735871

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

DTIC Science & Technology

2014-10-31

UHTCs charge (zirconium and hafnium borides , SiC) with additives (chromium carbide, nickel, chromium, etc.), which activate sintering process, is...temperature phases in a form of carboborides of zirconium and bi borides of zirconium or chromium. Elevation of densification rate of sintered borides is...superplasticity under the slip mechanism of zirconium boride and silica carbide grains on grain boundary interlayers with nanocrystalline grains of carbon

Effect of sintering temperatures on the in vitro bioactivity, molecular structure and mechanical properties of titanium/carbonated hydroxyapatite nanobiocomposites

NASA Astrophysics Data System (ADS)

Youness, Rasha A.; Taha, Mohammed A.; Ibrahim, Medhat A.

2017-12-01

Titanium-containing carbonated hydroxyapatite (Ti-CHA) nanocomposite powders, with different CHA contents, have been prepared using high-energy ball milling method. The effect of sintering temperatures, 900, 1100 and 1300 °C on molecular structure and microstructure of these samples were examined by XRD; Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM), respectively. Furthermore, their mechanical properties including hardness, longitudinal modulus, Young's modulus, shear modulus, bulk modulus and Poisson's ratio were measured by ultrasonic non-destructive technique. Moreover, bioactivity of sintered samples at different firing temperatures was assessed by immersing them in simulated body fluid at 37 ± 0.5 °C for 7 days and then, analyzed by FTIR spectroscopy. The results pointed out that increasing sintering temperature up to 1100 °C caused significant increases in densities and mechanical properties of these nanocomposite samples. However, further increase of firing temperature to 1300 °C was responsible for complete CHA decomposition and the resultant α-tricalcium (α-TCP) phase greatly affected these properties. On the contrary, better bioactivity was observed for sintered samples at 900 °C only. However, increase of sintering temperature of these samples up to 1300 °C led to severe decrease in their bioactivity due to the formation of highly soluble α-TCP phase.

Powder Metallurgy Fabrication of Porous 51(at.%)Ni-Ti Shape Memory Alloys for Biomedical Applications

NASA Astrophysics Data System (ADS)

Ibrahim, Mustafa K.; Hamzah, E.; Saud, Safaa N.; Nazim, E. M.

2018-05-01

The effect of time and temperature on the microwave sintering of 51(at.%)Ni-Ti shape memory alloys (SMAs) was investigated in the current research. Furthermore, the microstructure, mechanical properties, and bio-corrosion properties were analyzed based on the sintering conditions. The results revealed that the sintering condition of 700 °C for 15 min produced a part with coherent surface survey that does not exhibit gross defects. Increasing the sintering time and temperature created defects on the outer surface, while reducing the temperature to 550 °C severely affected the mechanical properties. The microstructure of these samples showed two regions of Ni-rich region and Ti-rich region between them Ti2Ni, NiTi, and Ni3Ti phases. The differential scanning calorimeter (DSC) curves of Ni-Ti samples exhibited a multi-step phase transformation B19'-R-B2 during heating and cooling. An increase in the sintering temperature from 550 to 700 °C was found to increase the fracture strength significantly and decreased the fracture strain slightly. Reducing the sintering temperature from 700 to 550 °C severely affected the corrosion behaviors of 51%Ni-Ti SMAs. This research aims to select the optimum parameters to produce Ni-Ti alloys with desired microstructure, mechanical properties, and corrosion behaviors for biomedical applications.

Si-Ge Nano-Structured with Tungsten Silicide Inclusions

NASA Technical Reports Server (NTRS)

Mackey, Jon; Sehirlioglu, Alp; Dynys, Fred

2014-01-01

Traditional silicon germanium high temperature thermoelectrics have potential for improvements in figure of merit via nano-structuring with a silicide phase. A second phase of nano-sized silicides can theoretically reduce the lattice component of thermal conductivity without significantly reducing the electrical conductivity. However, experimentally achieving such improvements in line with the theory is complicated by factors such as control of silicide size during sintering, dopant segregation, matrix homogeneity, and sintering kinetics. Samples are prepared using powder metallurgy techniques; including mechanochemical alloying via ball milling and spark plasma sintering for densification. In addition to microstructural development, thermal stability of thermoelectric transport properties are reported, as well as couple and device level characterization.

WSi2 in Si(1-x)Ge(x) Composites: Processing and Thermoelectric Properties

NASA Technical Reports Server (NTRS)

Mackey, Jonathan A.; Sehirlioglu, Alp; Dynys, Fred

2015-01-01

Traditional SiGe thermoelectrics have potential for enhanced figure of merit (ZT) via nano-structuring with a silicide phase, such as WSi2. A second phase of nano-sized silicides can theoretically reduce the lattice component of thermal conductivity without significantly reducing the electrical conductivity. However, experimentally achieving such improvements in line with the theory is complicated by factors such as control of silicide size during sintering, dopant segregation, matrix homogeneity, and sintering kinetics. Samples were prepared using powder metallurgy techniques; including mechano-chemical alloying, via ball milling, and spark plasma sintering for densification. Processing, micro-structural development, and thermoelectric properties will be discussed. Additionally, couple and device level characterization will be introduced.

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

Structural evolution of plasma-sprayed nanoscale 3 mol% and 5 mol% yttria-stabilized zirconia coatings during sintering

NASA Astrophysics Data System (ADS)

Zhao, Yan; Gao, Yang

2017-12-01

The microstructure of plasma-sprayed nanostructured yttria-stabilized zirconia (YSZ) coatings may change during high-temperature exposure, which would influence the coating performance and service lifetime. In this study, the phase structure and the microstructural evolution of 3YSZ (zirconia-3 mol% yttria) and 5YSZ (zirconia-5 mol% yttria) nanostructured coatings were investigated by means of sintering at 1400 °C for 50-100 h. The microhardness, elastic moduli, and thermal shock cycles of the 3YSZ and 5YSZ nanostructured coatings were also investigated. The results showed that the redistribution of yttrium ions at 1400 °C caused the continuous increase of monoclinic-phase zirconia, but no obvious inter-splat cracking formed at the cross-sections, even after 100 h. Large voids appeared around the nanoporous zone because of the sintering of nanoscale granules upon high-temperature exposure. The microhardness and elastic moduli of the nanostructured coatings first increased and then decreased with increasing sintering times. The growth rate of the nanograins in the 3YSZ coating was lower than that in 5YSZ, which slowed the changes in 3YSZ coating porosity during sintering. Although the 3YSZ coating was prone to monoclinic phase transition, the experimental results showed that the thermal shock resistance of the 3YSZ coating was better than that of the 5YSZ coating.

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

Effects of Heat Treatment on the Microstructures and High Temperature Mechanical Properties of Hypereutectic Al-14Si-Cu-Mg Alloy Manufactured by Liquid Phase Sintering Process

NASA Astrophysics Data System (ADS)

Heo, Joon-Young; Gwon, Jin-Han; Park, Jong-Kwan; Lee, Kee-Ahn

2018-05-01

Hypereutectic Al-Si alloy is an aluminum alloy containing at least 12.6 wt.% Si. It is necessary to evenly control the primary Si particle size and distribution in hypereutectic Al-Si alloy. In order to achieve this, there have been attempts to manufacture hypereutectic Al-Si alloy through a liquid phase sintering. This study investigated the microstructures and high temperature mechanical properties of hypereutectic Al-14Si-Cu-Mg alloy manufactured by liquid phase sintering process and changes in them after T6 heat treatment. Microstructural observation identified large amounts of small primary Si particles evenly distributed in the matrix, and small amounts of various precipitation phases were found in grain interiors and grain boundaries. After T6 heat treatment, the primary Si particle size and shape did not change significantly, but the size and distribution of CuAl2 ( θ) and AlCuMgSi ( Q) changed. Hardness tests measured 97.36 HV after sintering and 142.5 HV after heat treatment. Compression tests were performed from room temperature to 300 °C. The results represented that yield strength was greater after heat treatment (RT 300 °C: 351 93 MPa) than after sintering (RT 300 °C: 210 89 MPa). Fracture surface analysis identified cracks developing mostly along the interface between the primary Si particles and the matrix with some differences among temperature conditions. In addition, brittle fracture mode was found after T6 heat treatment.

Relating adatom emission to improved durability of Pt-Pd diesel oxidation catalysts

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

Johns, Tyne Richele; Goeke, Ronald S.; Ashbacher, Valerie

Sintering of nanoparticles is an important contributor to loss of activity in heterogeneous catalysts, such as those used for controlling harmful emissions from automobiles. But mechanistic details, such as the rates of atom emission or the nature of the mobile species, remain poorly understood. Herein we report a novel approach that allows direct measurement of atom emission from nanoparticles. We use model catalyst samples and a novel reactor that allows the same region of the sample to be observed after short-term heat treatments (seconds) under conditions relevant to diesel oxidation catalysts (DOCs). Monometallic Pd is very stable and does notmore » sinter when heated in air (T ≤ 800 °C). Pt sinters readily in air, and at high temperatures (≥800 °C) mobile Pt species emitted to the vapor phase cause the formation of large, faceted particles. In Pt–Pd nanoparticles, Pd slows the rate of emission of atoms to the vapor phase due to the formation of an alloy. However, the role of Pd in Pt DOCs in air is quite complex: at low temperatures, Pt enhances the rate of Pd sintering (which otherwise would be stable as an oxide), while at higher temperature Pd helps to slow the rate of Pt sintering. DFT calculations show that the barrier for atom emission to the vapor phase is much greater than the barrier for emitting atoms to the support. Thus, vapor-phase transport becomes significant only at high temperatures while diffusion of adatoms on the support dominates at lower temperatures.« less

Relating adatom emission to improved durability of Pt-Pd diesel oxidation catalysts

DOE PAGES

Johns, Tyne Richele; Goeke, Ronald S.; Ashbacher, Valerie; ...

2015-06-05

Sintering of nanoparticles is an important contributor to loss of activity in heterogeneous catalysts, such as those used for controlling harmful emissions from automobiles. But mechanistic details, such as the rates of atom emission or the nature of the mobile species, remain poorly understood. Herein we report a novel approach that allows direct measurement of atom emission from nanoparticles. We use model catalyst samples and a novel reactor that allows the same region of the sample to be observed after short-term heat treatments (seconds) under conditions relevant to diesel oxidation catalysts (DOCs). Monometallic Pd is very stable and does notmore » sinter when heated in air (T ≤ 800 °C). Pt sinters readily in air, and at high temperatures (≥800 °C) mobile Pt species emitted to the vapor phase cause the formation of large, faceted particles. In Pt–Pd nanoparticles, Pd slows the rate of emission of atoms to the vapor phase due to the formation of an alloy. However, the role of Pd in Pt DOCs in air is quite complex: at low temperatures, Pt enhances the rate of Pd sintering (which otherwise would be stable as an oxide), while at higher temperature Pd helps to slow the rate of Pt sintering. DFT calculations show that the barrier for atom emission to the vapor phase is much greater than the barrier for emitting atoms to the support. Thus, vapor-phase transport becomes significant only at high temperatures while diffusion of adatoms on the support dominates at lower temperatures.« less

Processing of sintered alpha SiC

NASA Technical Reports Server (NTRS)

Storm, R. S.

1984-01-01

Processing methods of sintered alpha SiC for engine applications are developed in a cost effective manner, using a submicron sized powder blended with sintering aids (boron and carbon). The processes for forming a green powder compact, such as dry pressing, cold isostatic pressing and green machining, slip casting, aqueous extrusion, plastic extrusion, and injection molding, are described. Dry pressing is the simplest route to component fabrication, and is carried out at approximately 10,000 psi pressure, while in the cold isostatic method the pressure could go as high as 20,000 psi. Surfactants are added to control settling rates and casting characteristics in the slip casting. The aqueous extrusion process is accomplished by a hydraulic ram forcing the aqueous mixture through a die. The plastic forming processes of extrusion and injection molding offer the potential of greater diversity in shape capacity. The physical properties of sintered alpha SiC (hardness, Young's modulus, shear modulus, and thermal diffusivity) are extensively tested. Corrosion resistance test results of silicon carbide are included.

Improvements to Zirconia Thick-Film Oxygen Sensors

NASA Astrophysics Data System (ADS)

Maskell, William C.; Brett, Daniel J. L.; Brandon, Nigel P.

2013-06-01

Thick-film zirconia gas sensors are normally screen-printed onto a planar substrate. A sandwich of electrode-electrolyte-electrode is fired at a temperature sufficient to instigate sintering of the zirconia electrolyte. The resulting porous zirconia film acts as both the electrolyte and as the diffusion barrier through which oxygen diffuses. The high sintering temperature results in de-activation of the electrodes so that sensors must be operated at around 800 °C for measurements in the percentage range of oxygen concentration. This work shows that the use of cobalt oxide as a sintering aid allows reduction of the sensor operating temperature by 100-200 °C with clear benefits. Furthermore, an interesting and new technique is presented for the investigation of the influence of dopants and of the through-porosity of ionically-conducting materials.

In situ evaluation of supersolidus liquid phase sintering phenomena of stainless steel 316L: Densification and distortion

NASA Astrophysics Data System (ADS)

Bollina, Ravi

Supersolidus liquid phase sintering (SLPS) is a variant of liquid phase sintering. In SLPS, prealloyed powders are heated between the solidus and liquidus temperature of the alloy. This thesis focuses on processing of stainless steel 316L via SLPS by adding boron. Various amounts of boron were added to study the effect of boron on densification and distortion. The sintering window for water atomized 316L with 0.2% boron ranges from 1430 to 1435°C and 1225 to 1245°C for water atomized 316L with 0.8% boron. The rate of change of liquid content with temperature dVL/dt decreases from 1.5%/°C to 0.1%/°C for in increase in boron content from 0 to 0.8%, giving a wider range and better control during sintering. Further; effect of boron on mechanical properties and corrosion properties was researched. It was possible to achieve tensile strength of 476+/-21 MPa and an yield strength of 250+/-5 MPa with an elongation of 15+/-2 % in water atomized 316L with 0.8% boron. Fracture analysis indicates the presence of a brittle boride phase along the grain boundary causing intergranular fracture resulting in poor ductility. The crux of this thesis discusses the evolution of apparent viscosity and its relation to the microstructure. Beam bending viscometry was successfully used to evaluate the in situ apparent viscosity evolution of water atomized 316L with 0.2 and 0.8% boron additions. The apparent viscosity drops from 174 GPa.s at 1200°C to 4 GPa.s at 1275°C with increasing fractional liquid coverage in the water atomized 316L with 0.8% boron. The apparent viscosity calculated from bending beam and was used as an input into a finite element model (FEM) derived from constitutive equations and gives an excellent, fit between simulation and experiment. The densification behavior of boron doped stainless steel was modelled using Master Sintering Curve (MSC) (based on work of sintering) for the first time. It is proven that MSC can be used to identify change in densification rate upon liquid formation during SLPS.

Microstructure and phase analysis of Zirconia-ODS (Oxide Dispersion Strengthen) alloy sintered by APS with milling time variation

NASA Astrophysics Data System (ADS)

Sugeng, Bambang; Bandriyana, B.; Sugeng, Bambang; Salam, Rohmad; Sumariyo; Sujatno, Agus; Dimyati, Arbi

2018-03-01

Investigation on the relationship between the process conditions of milling time and the microstructure on the synthesis of the zirconia-ODS steel alloy has been performed. The elemental composition of the alloy was determined on 20 wt% Cr and zirconia dispersoid of 0.50 wt%. The synthesis was carried out by powder metallurgy method with milling time of 3, 5 and 7 hours, static compression of 20 Ton and sintering process for 4 minutes using the APS (Arc Plasma Sintering) equipment. SEM-EDX and XRD test was carried out to characterize the phase and morphology of the alloy and the effect to the mechanical properties was evaluated by the Vickers Hardness testing. The synthesis produced sample of ODS steel with good dense and very little porous with the Fe-Cr phase that clearly observed in the XRD peak pattern. In addition milling time increased the homogeneously of Fe-Cr phase formulation, enhanced the grain refinement of the structure and increase the hardness of the alloy.

Field-assisted sintering and phase transition of ZnS-CaLa 2S 4 composite ceramics

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

Li, Yiyu; Zhang, Lihua; Kisslinger, Kim

In the present study, zinc sulfide (ZnS) and calcium lanthanum sulfide (CaLa 2S 4, CLS) composite ceramics were consolidated via field-assisted sintering of 0.5ZnS-0.5CLS (volume ratio) composite powders at 800–1050 °C. Through sintering curve analyses and microstructural observations, it was determined that between 800 and 1000 °C, grain boundary diffusion was the main mechanism controlling grain growth for both the ZnS and CLS phases within the composite ceramics. The consolidated composite ceramics were determined to be composed of sphalerite ZnS, wurtzite ZnS and thorium phosphate CLS. The sphalerite-wurtzite phase transition of ZnS was further demonstrated to be accompanied by themore » formation of stacking faults and twins in the ceramics. Furthermore, it was also found that the addition of the CLS phase improved the indentation hardness of the ceramics relative to pure ZnS by homogeneous dispersion of ZnS and CLS small grains.« less

Field-assisted sintering and phase transition of ZnS-CaLa 2S 4 composite ceramics

DOE PAGES

Li, Yiyu; Zhang, Lihua; Kisslinger, Kim; ...

2017-07-17

In the present study, zinc sulfide (ZnS) and calcium lanthanum sulfide (CaLa 2S 4, CLS) composite ceramics were consolidated via field-assisted sintering of 0.5ZnS-0.5CLS (volume ratio) composite powders at 800–1050 °C. Through sintering curve analyses and microstructural observations, it was determined that between 800 and 1000 °C, grain boundary diffusion was the main mechanism controlling grain growth for both the ZnS and CLS phases within the composite ceramics. The consolidated composite ceramics were determined to be composed of sphalerite ZnS, wurtzite ZnS and thorium phosphate CLS. The sphalerite-wurtzite phase transition of ZnS was further demonstrated to be accompanied by themore » formation of stacking faults and twins in the ceramics. Furthermore, it was also found that the addition of the CLS phase improved the indentation hardness of the ceramics relative to pure ZnS by homogeneous dispersion of ZnS and CLS small grains.« less

Phase transformation upon cooling path in Ca2SiO4: Possible geological implication

NASA Astrophysics Data System (ADS)

Chang, Yun-Ting; Kung, Jennifer; Hsu, Han

2016-04-01

At the contact metamorphism zone two different Ca2SiO4 phases can be found; calcio-olivine (γ phase) and larnite (β phase). In-situ experiments illustrated the existence of five various polymorphs in Ca2SiO4, i.e., α, α'H, α'L, β and γ. The path of phase transformation and the transformation temperatures are shown as follows. γ → α'L(700° C) → α'H(1100° C) → α (1450° C) α'L → β (680° C) → γ (500° C) Experiments showed that the phase transitions at lower temperature is not reversible and seemed to be complicated; β phase is only stable from 500° C to 680° C upon cooling. To understand the possible mechanism of the β phase being metastable at room temperature, atmosphere condition, we were motivated to investigate the route of phase transition in Ca2SiO4 in different thermal process. Powder samples were synthesized by the solid-state reaction. Pure reagent oxides CaCO3 and SiO2 were mixed in 2:1 stoichiometric mole. Two control factors were designated in the experiments; the sintering temperature of starting materials and the cooling path. The sintering temperature was set within the range of stable phase field of α'L phase (˜900° C) and α'H phase (1300° C). The cooling process was designed in three different routes: 1) the quenched procedure from sintering temperature with rate of 900° C/min and 1300° C/min, 2) the furnace cooling procedure, 3) set a slow cooling rate (0.265 ° C/min). The products were examined for the crystal structure by X-ray powder diffraction. First-principle calculation was also applied to investigate the thermodynamic properties of α'H, β and γ phases. A major finding in this study showed that the γ phase presented in the final product when the sintering temperature was set at the stable field of α'H phase; on the other hand, the β phase would present when the sintering temperature was set within the field of α'L phase. It was noted that the existing phase in the product would be modified by the cooling procedures. Our calculation indicates the enthalpy of beta phase was slightly higher than that of the gamma phase at zero pressure, verifying the metastable β phase observed in the natural. In this meeting we present the detailed experimental results and discuss the potential implication for the thermal history of geological setting using the phase transition path upon cooling of Ca2SiO4.

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.

Biomimetic Coating on Porous Alumina for Tissue Engineering: Characterisation by Cell Culture and Confocal Microscopy

PubMed Central

Kolos, Elizabeth; Ruys, Andrew J

2015-01-01

In this study porous alumina samples were prepared and then coated using the biomimetic coating technique using a five times Simulated Body Fluid (5.0SBF) as the growth solution. A coating was achieved after pre-treatment with concentrated acid. From elemental analysis, the coating contained calcium and phosphorous, but also sodium and chlorine. Halite was identified by XRD, a sodium chloride phase. Sintering was done to remove the halite phase. Once halite was burnt off, the calcium phosphate crystals were not covered with halite and, therefore, the apatite phases can be clearly observed. Cell culturing showed sufficient cell attachment to the less porous alumina, Sample B, that has more calcium phosphate growth, while the porous alumina, Sample A, with minimal calcium phosphate growth attained very little cell attachment. This is likely due to the contribution that calcium phosphate plays in the attachment of bone-like cells to a bioinert ceramic such as alumina. These results were repeated on both SEM and confocal microscopy analysis. Confocal microscopy was a novel characterisation approach which gave useful information and was a visual aid.

Formation of Equiaxed Alpha and Titanium Nitride Precipitates in Spark Plasma Sintered TiB/Ti-6Al-4V Composites (Preprint)

DTIC Science & Technology

2012-08-01

AFRL-RX-WP-TP-2012-0372 FORMATION OF EQUIAXED ALPHA AND TITANIUM NITRIDE PRECIPITATES IN SPARK PLASMA SINTERED TiB/Ti-6Al-4V COMPOSITES...ALPHA AND TITANIUM NITRIDE PRECIPITATES IN SPARK PLASMA SINTERED TiB/Ti-6Al-4V COMPOSITES (PREPRINT) 5a. CONTRACT NUMBER FA8650-08-C-5226 5b...distribution of TiN precipitates, as revealed by TEM studies. 15. SUBJECT TERMS Ti-6Al-4V; TiB; TiN; Spark Plasma Sintering ; Composite; α/β phase

Study of structural and magnetic properties of cobalt ferrite nanoparticles sintered at different temperature

NASA Astrophysics Data System (ADS)

Kumari, Mukesh; Bhatnagar, Mukesh Chander

2018-05-01

Cobalt ferrite (CFO) has been synthesized in the form of nanoparticles (NPs) through sol-gel auto-combustion method. The prepared NPs of CFO were sintered for four hours at various temperatures from 300°C to 900°C. The physical properties of the sintered samples have been optimized using X-ray diffraction (XRD), Raman spectroscopy and physical properties measurement system (PPMS). The XRD and Raman studies have confirmed the cubic spinel phase formation of CFO NPs. XRD results showed that as we increase the sintering temperature the crystallite size of particles increases. Whereas the magnetic studies revealed that the saturation magnetization (MS) increases while the coercivity (HC) of nanoparticles decreases with increase of sintering temperature.

Sintering and crystallization behavior of CaMgSi{sub 2}O{sub 6}-NaFeSi{sub 2}O{sub 6} based glass-ceramics

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

Goel, Ashutosh; Kansal, Ishu; Dipartimento di Ingegneria dei Materiali e dell'Ambiente, Facolta di Ingegneria, Universita di Modena e Reggio Emilia, 41100 Modena

2009-11-01

We report on the synthesis, sintering, and crystallization behaviors of a glass with a composition corresponding to 90 mol % CaMgSi{sub 2}O{sub 6}-10 mol % NaFeSi{sub 2}O{sub 6}. The investigated glass composition crystallized superficially immediately after casting of the melt and needs a high cooling rate (rapid quenching) in order to produce an amorphous glass. Differential thermal analysis and hot-stage microscopy were employed to investigate the glass forming ability, sintering behavior, relative nucleation rate, and crystallization behavior of the glass composition. The crystalline phase assemblage in the glass-ceramics was studied under nonisothermal heating conditions in the temperature range of 850-950more » deg. C in both air and N{sub 2} atmosphere. X-ray diffraction studies adjoined with the Rietveld-reference intensity ratio method were employed to quantify the amount of crystalline phases, while electron microscopy was used to shed some light on the microstructure of the resultant glass-ceramics. Well sintered glass-ceramics with diopside as the primary crystalline phase were obtained where the amount of diopside varied with the heating conditions.« less

Marginal Accuracy and Internal Fit of Dental Copings Fabricated by Modern Additive and Subtractive Digital Technologies.

PubMed

Nelson, Neha; K S, Jyothi; Sunny, Kiran

2017-03-01

The margins of copings for crowns and retainers of fixed partial dentures affect the progress of microleakage and dental caries. Failures occur due to altered fit which is also influenced by the method of fabrication. An in-vitro study was conducted to determine among the cast base metal, copy milled zirconia, computer aided designing computer aided machining/manufacturing zirconia and direct metal laser sintered copings which showed best marginal accuracy and internal fit. Forty extracted maxillary premolars were mounted on an acrylic model and reduced occlusally using a milling machine up to a final tooth height of 4 mm from the cementoenamel junction. Axial reduction was accomplished on a surveyor and a chamfer finish line was given. The impressions and dies were made for fabrication of copings which were luted on the prepared teeth under standardized loading, embedded in self-cure acrylic resin, sectioned and observed using scanning electron microscope for internal gap and marginal accuracy. The copings fabricated using direct metal laser sintering technique exhibited best marginal accuracy and internal fit. Comparison of mean between the four groups by ANOVA and post-hoc Tukey HSD tests showed a statistically significant difference between all the groups (p⟨0.05). It was concluded that the copings fabricated using direct metal laser sintering technique exhibited best marginal accuracy and internal fit. Additive digital technologies such as direct metal laser sintering could be cost-effective for the clinician, minimize failures related to fit and increase longevity of teeth and prostheses. Copyright© 2017 Dennis Barber Ltd.

[Microwave sintering of nanometer powder of alumina and zirconia-based dental ceramics].

PubMed

Chen, Yi-Fan; Lu, Dong-Mei; Wan, Qian-Bing; Jin, Yong; Zhu, Ju-Mu

2006-02-01

The objective of the present study was to investigate the feasibility and reliability of sintering alumina and zirconia-based all-ceramic materials through a recently introduced microwave heating technique. The variation of crystal phases, the growth of grain sizes and microstructural features of these materials were evaluated after sintering. Four different groups of powder (l00%Al2O3, 60%Al2O3+40%ZrO2, 40% Al2O3+60%ZrO2, 100% ZrO2) were respectively press-compacted to fabricate green disk samples, 5 specimen of each group were prepared. All the samples were surrounded by refractory materials for heat containment and processed at 1 600 degrees C in a domestic microwave oven (850 W, 2 450 MHz), 1 600 degrees C/5 min for heating rate, 10 min for holding time. After sintering, the phase composition and average grain size of these ceramics were examined using X-ray diffraction (XRD). Their microstructure characteristics were studied by scanning electron microscopy (SEM). All the specimens were successfully sintered with the application of microwave heating system in combination with a suitable thermal insulator. No phase change was found in alumina while monoclinic-zirconia was found to be transformed to tetragonal-zirconia. A little grain size growth of Al2O3 and ZrO2 has been observed with Al2O3 24.1 nm/before and 51.8 nm/after; ZrO2 25.3 nm/before and 29.7 nm/after. The SEM photos indicated that the microwave-sintered Al2O3-ZrO2 ceramics had a uniform crystal distribution and their crystal sizes could be maintained within the range of nanometers. It is expected that in the near future microwave heating system could be a promising substitute for conventional processing methods due to its unparalled advantages, including more rapid heating rate, shortened sintering time, superfine grain size, improved microstructure and much less expensive equipment.

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.

Microstructure, mechanical properties, bio-corrosion properties and antibacterial properties of Ti-Ag sintered alloys.

PubMed

Chen, Mian; Zhang, Erlin; Zhang, Lan

2016-05-01

In this research, Ag element was selected as an antibacterial agent to develop an antibacterial Ti-Ag alloy by a powder metallurgy. The microstructure, phase constitution, mechanical properties, corrosion resistance and antibacterial properties of the Ti-Ag sintered alloys have been systematically studied by X-ray diffraction (XRD), scanning electron microscope (SEM), compressive test, electrochemical measurements and antibacterial test. The effects of the Ag powder size and the Ag content on the antibacterial property and mechanical property as well as the anticorrosion property have been investigated. The microstructure results have shown that Ti-Ag phase, residual pure Ag and Ti were the mainly phases in Ti-Ag(S75) sintered alloy while Ti2Ag was synthesized in Ti-Ag(S10) sintered alloy. The mechanical test indicated that Ti-Ag sintered alloy showed a much higher hardness and the compressive yield strength than cp-Ti but the mechanical properties were slightly reduced with the increase of Ag content. Electrochemical results showed that Ag powder size had a significant effect on the corrosion resistance of Ti-Ag sintered alloy. Ag content increased the corrosion resistance in a dose dependent way under a homogeneous microstructure. Antibacterial tests have demonstrated that antibacterial Ti-Ag alloy was successfully prepared. It was also shown that the Ag powder particle size and the Ag content influenced the antibacterial activity seriously. The reduction in the Ag powder size was benefit to the improvement in the antibacterial property and the Ag content has to be at least 3wt.% in order to obtain a strong and stable antibacterial activity against Staphylococcus aureus bacteria. The bacterial mechanism was thought to be related to the Ti2Ag and its distribution. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of Bi doping on morphotropic phase boundary and dielectric properties of PZT

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

Joshi, Shraddha; Acharya, Smita, E-mail: saha275@yahoo.com

2016-05-23

In our present attempt, Pb{sub (1-x)}Bi{sub x}Zr{sub 0.52}Ti{sub 0.48}O{sub 3} [PBZT] {where x = 0, 0.05, 0.1} is synthesized by sol-gel route. Effect of Bi addition on structure, sinterability and dielectric properties are observed. The presence of morphotropic phase boundary (coexistence of tetragonal and rhombohedral symmetry) is confirmed by X-ray diffraction. Enhancement of sinterability after Bi doping is observed through a systematic sintering program. Frequency and temperature dependent dielectric constant are studied. Bi doping in PZT is found to enhance room temperature dielectric constant. However, at high temperature the dielectric constant of pure PZT is more than that of dopedmore » PZT.« less

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.

Effects of sintering atmosphere on the physical and mechanical properties of modified BOF slag glass

NASA Astrophysics Data System (ADS)

Dai, Wen-bin; Li, Yu; Cang, Da-qiang; Zhou, Yuan-yuan; Fan, Yong

2014-05-01

This study proposes an efficient way to utilize all the chemical components of the basic oxygen furnace (BOF) slag to prepare high value-added glass-ceramics. A molten modified BOF slag was converted from the melting BOF slag by reducing it and separating out iron component in it, and the modified BOF slag was then quenched in water to form glasses with different basicities. The glasses were subsequently sintered in the temperature range of 600-1000°C in air or nitrogen atmosphere for 1 h. The effects of different atmospheres on the physical and mechanical properties of sintered samples were studied by using differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM) and by conducting experiment on evaluating the sintering shrinkage, water absorption and bulk density. It is found that the kinetics of the sintering process is significantly affected by sintering atmosphere. In particular, compared with sintering in air atmosphere, sintering in N2 atmosphere promotes the synergistic growth of pyroxene and melilite crystalline phases, which can contribute to better mechanical properties and denser microstructure.

Study of sintering on Mg-Zn-Ca alloy system

NASA Astrophysics Data System (ADS)

Annur, Dhyah; Lestari, Franciska P.; Erryani, Aprilia; Kartika, Ika

2018-05-01

Magnesium and its alloy have gained a lot of interest to be used in biomedical application due to its biodegradable and biocompatible properties. In this study, sintering process in powder metallurgy was chosen to fabricatenonporous Mg-6Zn-1Ca (in wt%) alloy and porous Mg-6Zn-1Ca-10 Carbamide alloy. For creating porous alloy, carbamide (CO(NH2)2 was added to alloy system as the space holder to create porous structure material. Effect of the space holder addition and sintering temperature on porosity, phase formation, mechanical properties, and corrosion properties was observed. Sintering process was done in a tube furnace under Argon atmosphere in for 5 hours. The heat treatment was done in two steps; heated up at 250 °C for 4 hours to decompose spacer particle, followed by heated up at 580 °C or 630 °C for 5 hours. The porous structure of the resulted alloys was examined using Scanning Electron Microscope (SEM), while the phase formation was characterized by X-ray diffraction (XRD) analysis. Mechanical properties were examined using compression testing. From this study, increasing sintering temperature up to 630 °C reduced the mechanical properties of Mg-Zn-Ca alloy.

Influence of sintering temperature on the phases and photoelectric characteristics of BiOCl/ZnO composite powders

NASA Astrophysics Data System (ADS)

Chen, Song; Zhu, De-gui

2017-12-01

Zinc oxide is a typical functional oxide that has been widely researched for various industry applications due to its peculiar physical characteristics. However, to achieve its potential in promising applications, much work has been diligently performed to improve the physical properties of ZnO. In this work, an aqueous suspension route was used to prepare BiOCl/ZnO composite powders, and sintering processes were applied to investigate the influence of sintering temperature on the phase evolutions, microstructures, and photoelectric characteristics of BiOCl/ZnO composite powders. The results indicated that the photoelectric properties mainly depend on the relevant content of BiOCl in the composite powders and the sintering temperature. The photoelectric measurements in K2SO4 solutions show that the photoelectric properties of the samples with the appropriate BiOCl content (0.3mol% and 2.0mol%) are better than those of ZnO and commercial TiO2 (P25) powders, but the photoelectric measurements in NaOH solutions indicate that the photoelectric characteristics of the as-sintered samples are only better than those of P25.

Improvement microstructural and damage characterization of ceramic composites Y{sub 2}O{sub 3} – V{sub 2}O{sub 5} with MgO nano particles

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

Issa, T. T., E-mail: alazbrh@yahoo.com; Hasan, J. M.; Abdullah, E. T.

2016-04-21

Compacted samples of Y{sub 2}O{sub 3}-V{sub 2}O{sub 5} – MgO Nano – particles wt. % sintered at different sintering temperature (700, 900, 1100, 1300) ) C° for 2 hours under static air were investigated by x-ray diffraction and differential thermal analysis(DTA), to identify the phase present .Microstructure examination achieved by scanning electron microscopy .Sintered density and porosity were measured for all sintered samples .Compression was tested too and the Brake down voltage and dielectric strength were measure for all sintered samples .The clear improvement were noticed in both microstructure and damage characterization respectively after existing the MgO Nano-particles, by increasingmore » in about 30% in sintered density and 25% for the compressive strength .The improvement also noticed on both brake down voltage and dielectric strength.« less

In vitro biodegradation testing of Mg-alloy EZK400 and manufacturing of implant prototypes using PM (powder metallurgy) methods.

PubMed

Wolff, M; Luczak, M; Schaper, J G; Wiese, B; Dahms, M; Ebel, T; Willumeit-Römer, R; Klassen, T

2018-09-01

The study is focussing towards Metal Injection Moulding (MIM) of Mg-alloys for biomedical implant applications. Especially the influence of the sintering processing necessary for the consolidation of the finished part is in focus of this study. In doing so, the chosen high strength EZK400 Mg-alloy powder material was sintered using different sintering support bottom plate materials to evaluate the possibility of iron impurity pick up during sintering. It can be shown that iron pick up took place from the steel bottom plate into the specimen. Despite the fact that a separating boron nitrite (BN) barrier layer was used and the Mg-Fe phase diagram is not predicting any significant solubility to each other. As a result of this study a new bottom plate material not harming the sintering and the biodegradation performance of the as sintered material, namely a carbon plate material, was found.

A novel in situ synthesis of SiBCN-Zr composites prepared by a sol-gel process and spark plasma sintering.

PubMed

Miao, Yang; Yang, Zhihua; Liang, Bin; Li, Quan; Chen, Qingqing; Jia, Dechang; Cheng, Yi-Bing; Zhou, Yu

2016-08-09

In the work reported here, SiBCN amorphous powders were first prepared by a mechanical alloying technique, employing cubic silicon, graphite and hexagonal boron nitride powders as raw materials. Zirconia was then introduced via sol-gel methods. The resulting powder composite was then consolidated via SPS sintering. The SPS sintering sample was evaluated using XRD, SEM and TEM. XRD reveals a chemical transformation wherein amorphous BN(C) and ZrO2 form the primary ZrC and ZrB2 phases after SPS processing along with SiC and BN(C). Thereafter ZrC reacts with BN(C) completely to form ZrB2. The reaction starts at the temperature of 1500 °C and is complete at the temperature of 1900 °C. The fracture toughness of the sintered composites reaches 4.9 ± 0.2 MPa m(1/2) due to the presence of the laminated structure of the BN(C) phase.

Grain refinement in heavy rare earth element-free sintered Nd–Fe–B magnets by addition of a small amount of molybdenum

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

Kim, Jin Woo; Lee, Won Suk; Byun, Jong Min

2015-05-07

We employed a modified refractory-metal-addition method to achieve higher coercivity and remanence in heavy rare earth element (HREE)-free Nd–Fe–B sintered magnets. This process involved inducing the formation of a homogeneous secondary phase at the grain boundaries during sintering, making it possible to control the intergrain diffusion by adding small amounts of Mo, a refractory metal. To control the microstructure of the secondary phase effectively, a metal organic compound of the refractory metal was coated on the surfaces of the particles of an HREE-free Nd–Fe–B powder. The average grain size after this process was 5.60 μm, which was approximately 1.8 μm smaller thanmore » that of the HREE-free sintered Nd–Fe–B magnets (7.4 μm). The coercivity of the magnets prepared through this process could be increased from 11.88 kOe to 13.91 kOe without decreasing their remanence.« less

Liquid Phase Sintering

NASA Technical Reports Server (NTRS)

2004-01-01

Industry spends billions of dollars each year on machine tools to manufacture products out of metal. This includes tools for cutting every kind of metal part from engine blocks to Shuttle main engine components. Cutting tool tips often break because of weak spots or defects in their composition. Based on a new concept called defect trapping, space offers a novel environment to study defect formation in molten metal materials as they solidify. After the return of these materials from space, researchers can evaluate the source of the defect and seek ways to eliminate them in products prepared on Earth. A widely used process for cutting tip manufacturing is liquid phase sintering. Compared to Earth-sintered samples which slump due to buoyancy induced by gravity, space samples are uniformly shaped and defects remain where they are formed. By studying metals sintered in space the US tool industry can potentially enhance its worldwide competitiveness. The Consortium for Materials Development in Space along with Wyle Labs, Teledyne Advanced Materials, and McDornell Douglas have conducted experiments in space.

Effects of La2O3-B2O3-ZnO additions on the low temperature sintering and microwave dielectric properties of (Ca0.61La0.26) TiO3 ceramics

NASA Astrophysics Data System (ADS)

Chen, Y. W.; Li, E. Z.; Niu, N.; Zou, M. Y.; Duan, S. X.; Zhang, S. R.

2017-02-01

The influence of La2O3-B2O3-ZnO (LBZ) additions on the sintering behavior, microstructure, phase composition, and the microwave dielectric properties of (Ca0.61La0.26) TiO3 (CLT) ceramics have been investigated. The results indicate that the LBZ additions could efficiently lower the sintering temperature of the CLT ceramics from 1400°C to 950°C, and excellent microwave properties remain. Small amount of LBZ glass promotes the densification of the CLT ceramics and enhances the microwave dielectric properties. However, excess amount of LBZ glass deteriorates the dielectric properties because of the increasing glass phase. The CLT ceramic with 3 wt. % LBZ additions, sintered at 950°C, exhibit excellent properties: εr= 103.12, Q× f = 8826 GHz(f=3.312 GHz) and τƒ=299.52 ppm/°C.

Method and device for microwave sintering large ceramic articles

DOEpatents

Kimrey, Jr., Harold D.

1990-01-01

A microwave sintering system and method are provided for extremely uniform sintering of large and/or irregular shaped ceramic articles at microwave frequencies of at least 28 GHz in the hundreds of kilowatts power range in an untuned cavity. A 28 GHz, 200 kw gyrotron with variable power output is used as the microwave source connected to an untuned microwave cavity formed of an electrically conductive housing through an overmoded waveguide arrangement which acts in conjunction with a mode promoter within the cavity to achieve unexpected field uniformity. The part to be sintered is placed in the cavity and supported on a removable high temperature table in a central location within the cavity. The part is surrounded by a microwave transparent bulk insulating material to reduce thermal heat loss at the part surfaces and maintain more uniform temperature. The cavity may be operated at a high vacuum to aid in preventing arcing. The system allows controlled increased heating rates of greater than 200.degree. C./min to provide rapid heating of a ceramic part to a selected sintering temperature where it is maintained by regulating the microwave power applied to the part. As a result of rapid heating, the extent of non-isothermal processes such as segregation of impurities to the grain boundaries are minimized and exaggerated grain growth is reduced, thereby strengthening the mechanical properties of the ceramic part being sintered.

CAD/CAM machining Vs pre-sintering in-lab fabrication techniques of Y-TZP ceramic specimens: Effects on their mechanical fatigue behavior.

PubMed

Zucuni, C P; Guilardi, L F; Fraga, S; May, L G; Pereira, G K R; Valandro, L F

2017-07-01

This study evaluated the effects of different pre-sintering fabrication processing techniques of Y-TZP ceramic (CAD/CAM Vs. in-lab), considering surface characteristics and mechanical performance outcomes. Pre-sintered discs of Y-TZP ceramic (IPS e.max ZirCAD, Ivoclar Vivadent) were produced using different pre-sintering fabrication processing techniques: Machined- milling with a CAD/CAM system; Polished- fabrication using a cutting device followed by polishing (600 and 1200 SiC papers); Xfine- fabrication using a cutting machine followed by grinding with extra-fine diamond bur (grit size 30 μm); Fine- fabrication using a cutting machine followed by grinding with fine diamond bur (grit size 46 μm); SiC- fabrication using a cutting machine followed by grinding with 220 SiC paper. Afterwards, the discs were sintered and submitted to roughness (n=35), surface topography (n=2), phase transformation (n=2), biaxial flexural strength (n=20), and biaxial flexural fatigue strength (fatigue limit) (n=15) analyses. No monoclinic-phase content was observed in all processing techniques. It can be observed that obtaining a surface with similar characteristics to CAD/CAM milling is essential for the observation of similar mechanical performance. On this sense, grinding with fine diamond bur before sintering (Fine group) was the best mimic protocol in comparison to the CAD/CAM milling. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis and Study on Ionic Conductive (Bi1−x,Vx)O1.5−δ Materials with a Dual-Phase Microstructure

PubMed Central

Lai, Yu-Wei; Wei, Wen-Cheng J.

2016-01-01

Homogeneous Bi2O3-V2O5 powder mixtures with different amounts of V2O5 content (≤15 mol%) were prepared by colloidal dispersion and sintering to high density. The sintered and annealed samples were studied by thermal analysis, quantitative X-ray diffraction and scanning electron microscopy. The electrical and ionic conductivities of the conductors were also measured by a four-probe direct current (DC) method. The results of the samples prepared at 600–800 °C and annealed for as long as 100 h show that the sintered samples consisting of a pure γ phase or δ + γ binary phase perform differently in conductivity. The highly conductive δ phase in the composition of Bi0.92V0.08O1.5−δ enhances the electric conductivity 10-times better than that of the pure γ-sample (Bi0.94V0.06O1.5−δ) between 400 and 600 °C. The compatible regions of the γ phase with the α- or δ phase are also reported and discussed, so a part of the previously published Bi2O3-V2O5 phase diagram below 800 °C is revised. PMID:28773981

Effect of LiF as Sintering Agent on the Densification and Phase Formation in Al2O3-4 Wt Pct Nb2O5 Ceramic Compound

NASA Astrophysics Data System (ADS)

Santos, J. L.; Marçal, R. L. S. B.; Jesus, P. R. R.; Gomes, A. V.; Lima, E. P.; Monteiro, S. N.; de Campos, J. B.; Louro, L. H. L.

2017-10-01

Different amounts of LiF were added to an Al2O3-4 pct Nb2O5 basic ceramic, as sintering agent. Improved new ceramics were obtained with LiF concentrations varying from 0.25 to 1.50 wt pct and three sintering temperatures of 1573 K, 1623 K, and 1673 K (1300 °C, 1350 °C, and 1400 °C). The addition of 0.5 wt pct LiF yielded the highest densification, 94 pct of the theoretical density, in association with a sintering temperature of 1673 K (1400 °C). Based on X-ray diffraction (XRD), this improvement was due not only to the presence of transformed phases, more precisely Nb3O7F, but also to the absence of LiAl5O8. The preferential interaction of LiF with Nb2O5, instead of Al2O3, contributed to increase the alumina sintering ability by liquid phase formation. Scanning electron microscopy (SEM) results revealed well-connected grains and isolated pores, whereas the chemical composition analysis by energy dispersive energy (EDX) indicated a preferential interaction of fluorine with niobium, in agreement with the results of XRD. It was also observed from thermal analysis that the polyethylene glycol binder burnout temperature increased for all LiF concentrations. This may be related to the formation of hydrogen bridge bonds.

Characterization of the distribution of the sintering activator boron in powder metallurgical steels with SIMS.

PubMed

Krecar, Dragan; Vassileva, Vassilka; Danninger, Herbert; Hutter, Herbert

2004-06-01

Powder metallurgy is a well-established method for manufacturing ferrous precision parts. A very important step is sintering, which can be strongly enhanced by the formation of a liquid phase during the sintering process. Boron activates this process by forming such a liquid phase at about 1200 degrees C. In this work, the sintering of Fe-B was performed under the protective atmospheres of hydrogen, argon or nitrogen. Using different grain sizes of the added ferroboron leads to different formations of pores and to the formation of secondary pores. The effect of boron was investigated by means of Secondary Ion Mass Spectrometry (SIMS) supported by Scanning Electron Microscopy (SEM) and Light Microscopy (LM). To verify the influence of the process parameters on the mechanical properties, the microstructure (pore shape) was examined and impact energy measurements were performed. The concentrations of B in different samples were varied from 0.03-0.6 weight percent (wt%). Higher boron concentrations are detectable by EPMA, whereas the distributions of boron in the samples with interesting overall concentration in the low wt% range are only detectable by means of SIMS. This work shows that the distribution of boron strongly depends on its concentration and the sintering atmosphere used. At low concentration (up to 0.1 wt%) there are boride precipitations; at higher concentration there is a eutectic iron-boron grain boundary network. There is a decrease of the impact energy observed that correlates with the amount of eutectic phase.

The corrosion mechanism of the sintered (Ce, Nd)-Fe-B magnets prepared by double main phase and single main phase approaches

NASA Astrophysics Data System (ADS)

Shi, Xiaoning; Zhu, Minggang; Zhou, Dong; Song, Liwei; Guo, Zhaohui; Li, Jia; Li, Wei

2018-05-01

The sintered (Ce, Nd)-Fe-B magnets were produced widely by Double Main Phase (DMP) method in China as the magnetic properties of the DMP magnets are superior to those of single main phase (SMP) magnets with the same nominal composition. In this work, the microstructure and corrosion mechanism of the sintered (Ce0.2Nd0.8)30FebalB (wt.%) magnets prepared by DMP and SMP method were studied in detail. Compared to SMP magnets, the DMP magnets have more positive corrosion potential, lower corrosion current density, larger electron transfer resistance, and lower mass loss of the free corrosion experiment in 0.5mol/l Na2SO4 aqueous solution. All of the results show that the DMP magnets have better corrosion resistance than SMP magnets. The back scattered electron images show that the crystalline grains of the DMP magnets are sphericity with a smooth surface while the SMP ones have plenty of edges and corners. Besides, the distribution of Ce/Nd is much more uneven in both magnetic phase and rare earth (Re)-rich phase of the DMP magnets than those of SMP magnets. After corrosion, DMP magnets show eroded magnetic phase and intact Re-rich phase, which indicate that galvanic corrosion of the Re-rich phase acting as the cathode appears.

Systematic variations in sinter mineralogy, microtexture and diagenesis in modern siliceous hot springs: Clues for interpreting depositional conditions in ancient deposits

NASA Astrophysics Data System (ADS)

Mills, V. W.; Farmer, J. D.; Ruff, S. W.; Nunez, J.; Jahnke, L. L.

2011-12-01

The deposits of siliceous hydrothermal springs are known to capture and preserve a wide range of microbial fossil information. The recent discovery of hydrothermal silica at Home Plate, Columbia Hills, Mars has once again raised interest in the potential importance of ancient spring sinters as targets for future astrobiological mission to Mars. To create additional context information to support future in situ missions to Mars, we have documented systematic changes in the mineralogy and microtexture of modern siliceous hot spring deposits, observed along gradients in temperature, pH and flow velocity. Specific objectives are to: 1) identify chemical and physical factors that promote early diagenetic transformations of amorphous silica (opal-A), to progressively more ordered and crystalline phases (cristobalite, tridymite and quartz); 2) determine the composition and abundance of minor mineral phases, especially clays, in relationship to pH, temperature and paragenesis; and 3) to assess the usefulness of sinter mineralogy and microtexture in reconstructing the paleoenvironmental records preserved in ancient deposits. Study sites for acidic (pH 2-5) sinters included Nymph Creek, located in the Norris Geyser Basin of Yellowstone National Park (YNP). Active alkaline (pH 7-10) springs included Rabbit Creek, Steep Cone and Mound Spring located in the Lower Geyser Basin, YNP. Field measurements in active springs included pH, temperature and flow velocity, along with general microfacies assignments. To better constrain types and rates of silica diagenesis, the study also sampled older (Holocene-Pleistocene-aged) deposits. Laboratory analyses included X-ray powder diffraction (XRPD), thermal infrared spectroscopy (TIR) and thin section petrography for characterizing sinter microtextures and for placing mineral phases (identified by XRPD and TIR) into a time-ordered diagenetic framework. In analyzing the phyllosilicates present in sinters, we applied clay separation and glycolization methods, with XRPD. Results indicate that all of the acidic sinters we studied showed more extensive early diagenetic ordering of silica phases (opal-A to cristobalite and quartz) than the comparable microfacies of alkaline-neutral sinters. Clay analyses showed no evidence for smectitic (expansive) clays, but kaolin family clays (dickite, kaolinite and halloysite) were present in both acidic and alkaline sinters. The microfacies distribution observed for clays suggests: 1) dickite being more abundant in higher temperature (near-vent) microfacies, 2) kaolinite dominating mid-temperature outflow channels, slope and upper distal apron microfacies, and 3) halloysite being restricted to lower distal apron-marsh microfacies transitions. Future work will expand clay analyses to apply near-IR spectroscopy to a broader range of samples to assess the consistency with patterns suggested from XRPD.

Effect of sintering on structure and magnetic properties of Mn-doped Zn ferrite

NASA Astrophysics Data System (ADS)

Farheen, Atiya; Singh, Rajender

2018-05-01

The Mn-doped zinc ferrites, MnxZn1-xFe2O4 (x= 0 and 0.1) were prepared using co-precipitation method. The as-prepared samples were sintered at different temperatures. The x-ray diffraction pattern for all the samples confirms single phase spinel structure with Fd-3m space group. The lattice parameters have been estimated using Rietveld fitting. The magnetic moment is found to increase with Mn-doping. The magnetization increases as the sintering temperature increases up to 1200°C. The as-prepared samples are super paramagnetic, while the sintered samples are ferrimagnetic in nature.

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.

Flash sintering of stoichiometric and hyper-stoichiometric urania

DOE PAGES

Valdez, James Anthony; Byler, Darrin David; Kardoulaki, Erofili; ...

2018-03-29

Flash sintering (FS), a novel fabrication technique belonging to the family of field assisted sintering (FAS) techniques, has been utilized in this study to fabricate uranium dioxide (UO 2) pellets. Stoichiometric (UO 2.00) and hyper-stoichiometric (UO 2.16) pellets were flash sintered at 600 °C within a few (2–3) minutes. This is in sharp contrast to conventional sintering where temperatures hundreds of degrees higher are necessary and the sintering time extends to hours. Relating this in terms of the homologous temperature ratio (T H) for both conditions shows that in the case of flash sintering at 600 °C, T H =more » 0.3 versus T H = 0.6 for conventional sintering at 1600 °C. The highest density achieved for a UO 2.00 pellet was 81% theoretical density (TD) when flash sintered at 600 °C for 184 s at a field of 188 V/cm and a current density of 442 mA/mm 2. For the UO 2.16 pellet, the highest achieved density was 92% TD when flash sintered at 600 °C for 140 s at a field of 188 V/cm and a current density of 632 mA/mm 2. X-ray diffraction (XRD) characterization of the sintered pellets showed the final sintered material to be single cubic fluorite phase. Scanning electron microscopy (SEM) of longitudinal sections revealed non-uniform microstructures with regions of high density where the grain size ranged from 1 to 15 μm. Comparisons between conventionally and flash sintered pellets that achieved equivalent shrinkage strains were also conducted. Lastly, in all cases, the flash sintered pellets achieved similar densification to the conventionally sintered pellets at much lower furnace temperatures and shorter times.« less

Flash sintering of stoichiometric and hyper-stoichiometric urania

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

Valdez, James Anthony; Byler, Darrin David; Kardoulaki, Erofili

Flash sintering (FS), a novel fabrication technique belonging to the family of field assisted sintering (FAS) techniques, has been utilized in this study to fabricate uranium dioxide (UO 2) pellets. Stoichiometric (UO 2.00) and hyper-stoichiometric (UO 2.16) pellets were flash sintered at 600 °C within a few (2–3) minutes. This is in sharp contrast to conventional sintering where temperatures hundreds of degrees higher are necessary and the sintering time extends to hours. Relating this in terms of the homologous temperature ratio (T H) for both conditions shows that in the case of flash sintering at 600 °C, T H =more » 0.3 versus T H = 0.6 for conventional sintering at 1600 °C. The highest density achieved for a UO 2.00 pellet was 81% theoretical density (TD) when flash sintered at 600 °C for 184 s at a field of 188 V/cm and a current density of 442 mA/mm 2. For the UO 2.16 pellet, the highest achieved density was 92% TD when flash sintered at 600 °C for 140 s at a field of 188 V/cm and a current density of 632 mA/mm 2. X-ray diffraction (XRD) characterization of the sintered pellets showed the final sintered material to be single cubic fluorite phase. Scanning electron microscopy (SEM) of longitudinal sections revealed non-uniform microstructures with regions of high density where the grain size ranged from 1 to 15 μm. Comparisons between conventionally and flash sintered pellets that achieved equivalent shrinkage strains were also conducted. Lastly, in all cases, the flash sintered pellets achieved similar densification to the conventionally sintered pellets at much lower furnace temperatures and shorter times.« less

Flash sintering of stoichiometric and hyper-stoichiometric urania

NASA Astrophysics Data System (ADS)

Valdez, J. A.; Byler, D. D.; Kardoulaki, E.; Francis, J. S. C.; McClellan, K. J.

2018-07-01

Flash sintering (FS), a novel fabrication technique belonging to the family of field assisted sintering (FAS) techniques, has been utilized in this study to fabricate uranium dioxide (UO2) pellets. Stoichiometric (UO2.00) and hyper-stoichiometric (UO2.16) pellets were flash sintered at 600 °C within a few (2-3) minutes. This is in sharp contrast to conventional sintering where temperatures hundreds of degrees higher are necessary and the sintering time extends to hours. Relating this in terms of the homologous temperature ratio (TH) for both conditions shows that in the case of flash sintering at 600 °C, TH = 0.3 versus TH = 0.6 for conventional sintering at 1600 °C. The highest density achieved for a UO2.00 pellet was 81% theoretical density (TD) when flash sintered at 600 °C for 185 s at a field of 188 V/cm and a current density of 442 mA/mm2. For the UO2.16 pellet, the highest achieved density was 91% TD when flash sintered at 600 °C for 123 s at a field of 188 V/cm and a current density of 632 mA/mm2. X-ray diffraction (XRD) characterization of the sintered pellets showed the final sintered material to be single cubic fluorite phase. Scanning electron microscopy (SEM) of longitudinal sections revealed non-uniform microstructures with regions of high density where the grain size ranged from 1 to 15 μm. Comparisons between conventionally and flash sintered pellets that achieved equivalent shrinkage strains were also conducted. In all cases, the flash sintered pellets achieved similar densification to the conventionally sintered pellets at much lower furnace temperatures and shorter times.

Sintering behavior of ultrafine silicon carbide powders obtained by vapor phase reaction

NASA Technical Reports Server (NTRS)

Okabe, Y.; Miyachi, K.; Hojo, J.; Kato, A.

1984-01-01

The sintering behavior of ultrafine SiC powder with average particle size of about 0.01-0.06 microns produced by a vapor phase reaction of the Me4Si-H2 system was studied at the temperature range of 1400-2050 deg. It was found that the homogeneous dispersion of C on SiC particles is important to remove the surface oxide layer effectively. B and C and inhibitive effect on SiC grain growth.

Effect of low-melting point phases on the microstructure and properties of spark plasma sintered and hot deformed Nd-Fe-B alloys

NASA Astrophysics Data System (ADS)

Zhang, Li; Wang, Meiyu; Yan, Xueliang; Lin, Ye; Shield, Jeffrey

2018-04-01

The effect of adding a low melting point Pr-Cu-Al alloy during spark plasma sintering of melt-spun Nd-Fe-B ribbons is investigated. Regions of coarse grains were reduced and overall grain refinement was observed after the addition of Pr68Cu25Al7, leading to an enhancement of coercivity from 12.7 kOe to 20.4 kOe. Hot deformation of the samples in the spark plasma sintering system resulted in the formation of platelet-like grains, producing crystallographic alignment and magnetic anisotropy. The hot deformation process improved the remanence and energy product but reduced the coercivity. The decrease of coercivity resulted from grain growth and aggregation of Pr and Nd elements at triple-junction phases.

Phase equilibrium and preparation, crystallization and viscous sintering of glass in the alumina-silica-lanthanum phosphate system

NASA Astrophysics Data System (ADS)

He, Feng

The phase equilibrium, viscosity of melt-quenched glasses, and processing of sol-gel glasses of the alumina-silica-lanthanum phosphate system were studied. These investigations were directed towards serving the objective of synthesizing nano-structured ceramic-matrix-composites via controlled crystallization of glass precursors. The thermal stability, phase equilibrium, and liquidus temperatures of the alumina- and mullite-lanthanum phosphate systems are determined. An iridium wire heater was constructed to anneal samples up to 2200°C. Phosphorus evaporation losses were significant at high temperatures, especially over 1800°C. The tentative phase diagrams of the two quasi-binary systems were presented. The viscosity of the melt-quenched mullite-lanthanum phosphate glasses was measured by three different methods, including viscous sintering of glass powder compacts, neck formation between two Frenkel glass beads, and thermal analysis of the glass transition. Improved methodologies were developed for applying the interpretative mathematical models to the results of the sintered powder and thermal analytical experiments. Good agreement was found between all three methods for both absolute values and temperature dependence. A sol-gel process was developed as a low temperature route to producing glasses. A unique, single phase mullite gel capable of low temperature (575°C) mullitization was made from tetraethoxysilane and aluminum isopropoxide at room temperature in three days. Low temperature crystallization was attributed to the avoidance of phase segregation during gel formation and annealing. This was greatly enhanced by a combination of low temperature preheating in the amorphous state, a high heating rate during crystallization and low water content. The Al2O3 content in mullite (61-68 mol%) depended on the highest annealing temperature. Two mullite-lanthanum phosphate gels were made based upon modifying the chemical procedures used for the homogeneous single phase and heterogeneous diphasic mullite gels from same starting chemicals. Amorphous powders were obtained after optimized calcinations. Their different crystallization routes and sintering behavior were investigated and correlated with the different homogeneities of precursor gels. Structurally stable open, porous ceramics (up to 80% porosity) were produced from the single-phase gel derived powder, where gases exsolved during calcination caused foaming coincident with sintering. Translucent, dense glass ceramic was made from the calcined diphasic gel by hot-pressing.

Effect of starting powder characteristics on density, microstructure and low temperature oxidation behavior of a Si3N48w/o Y2O3 ceramic

NASA Technical Reports Server (NTRS)

Schuon, S.; Dutta, S.

1980-01-01

The densification and oxidation behavior of Si3N4 - 8w/oY2O3 prepared from three commercial starting powders were studied. Bars of SN 402, SN 502, and CP 85/15 were sintered for 3 to 4.5 hours at 1750 C. A second set was hot pressed for 2 hours at 1750 C. The microstructures were studied by transmission electron microscopy and scanning electron microscopy, densities were determined, and the phase compositions were determined by X-ray diffraction. Densification and microstructure were greatly influenced by the starting powder morphology and impurity content. Although SN 402 exhibited the maximum weight lose, the highest sintered and hot pressed densities were obtained with this powder. All powders had both equiaxed and elongated grains. Sintered bars were composed of beta silicon nitride and n-melelite. In contrast, hot pressed bars contained beta silicon nitride, H-phase, and J-phase, but no melelite. Yttria distribution in sintered bars was related to the presence of cation impurities such as Ca, Fe, and Mg. A limited oxidation study at 750 C in air showed no instability in these Si3N4 - 8 w/oY2O3 specimens, regardless of startin powder.

Vacuum Pressureless Sintering of Ti-6Al-4V Alloy with Full Densification and Forged-Like Mechanical Properties

NASA Astrophysics Data System (ADS)

Zhang, Ce; Lu, Boxin; Wang, Haiying; Guo, Zhimeng; Paley, Vladislav; Volinsky, Alex A.

2018-01-01

Ti-6Al-4V ingots with a nearly 100% density, fine and homogeneous basket-weave microstructure, and better comprehensive mechanical properties (UTS = 935 MPa, Y.S. = 865 MPa, El. = 15.8%), have been manufactured by vacuum pressureless sintering of blended elemental powders. Coarse TiH2 powder, Al powder (2, 20 μm), V powder, and Al-V master alloy powder were used as raw materials to produce different powder mixtures ( D 50 = 10 μm). Then, the compacts made by cold isostatic pressing were consolidated by different sintering curves. A detailed investigation of different as-sintered samples revealed that a higher density can be obtained by generating transient molten Al in the sintering process. Coarse Al powder and a rapid heating rate under the melting point of Al contribute to molten Al formation. The presence of temporary liquid phase changes the sintering mechanism, accelerating the sintering neck formation, improving sinterability of the powder mixtures. Density of 99.5% was achieved at 1150 °C, which is markedly lower than the sintering temperatures reported for conventional blended elemental powder metallurgy routes. In addition, low interstitial content, especially for oxygen (0.17 wt.%), is obtained by strict process control.

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.

Influence of Basicity on High-Chromium Vanadium-Titanium Magnetite Sinter Properties, Productivity, and Mineralogy

NASA Astrophysics Data System (ADS)

Zhou, Mi; Yang, Songtao; Jiang, Tao; Xue, Xiangxin

2015-05-01

The effect of basicity on high-chromium vanadium-titanium magnetite (V-Ti-Cr) sintering was studied via sintering pot tests. The sinter rate, yield, and productivity were calculated before determining sinter strength (TI) and reduction degradation index (RDI). Furthermore, the effect of basicity on V-Ti-Cr sinter mineralogy was clarified using metallographic microscopy, x-ray diffraction, and scanning electron microscopy-energy-dispersive x-ray spectroscopy. The results indicate that increasing basicity quickly increases the sintering rate from 25.4 mm min-1 to 28.9 mm min-1, yield from 75.3% to 87.2%, TI from 55.4% to 64.8%, and productivity from 1.83 t (m2 h)-1 to 1.94 t (m2 h)-1 before experiencing a slight drop. The V-Ti-Cr sinter shows complex mineral composition, with main mineral phases such as magnetite, hematite, silicate (dicalcium silicate, Ca-Fe olivine, glass), calcium and aluminum silico-ferrite (SFCA/SFCAI) and perovskite. Perovskite is notable because it lowers the V-Ti sinter strength and RDI. The well intergrowths between magnetite and SFCA/SFCAI, and the decrease in perovskite and secondary skeletal hematite are the key for improving TI and RDI. Finally, a comprehensive index was calculated, and the optimal V-Ti-Cr sinter basicity also for industrial application was 2.55.

Influence of Sintering Temperature on Hardness and Wear Properties of TiN Nano Reinforced SAF 2205

NASA Astrophysics Data System (ADS)

Oke, S. R.; Ige, O. O.; E Falodun, O.; Obadele, B. A.; Mphalele, M. R.; Olubambi, P. A.

2017-12-01

Conventional duplex stainless steel degrade in wear and mechanical properties at high temperature. Attempts have been made by researchers to solve this problems leading to the dispersion of second phase particles into duplex matrix. Powder metallurgy methods have been used to fabricate dispersion strengthened steels with a challenge of obtaining fully dense composite and grain growth. This could be resolved by appropriate selection of sintering parameters especially temperature. In this research, spark plasma sintering was utilized to fabricate nanostructured duplex stainless steel grade SAF 2205 with 5 wt.% nano TiN addition at different temperatures ranging from 1000 °C to 1200 °C. The effect of sintering temperature on the microstructure, density, hardness and wear of the samples was investigated. The results showed that the densities and grain sizes of the sintered nanocomposites increased with increasing the sintering temperature. The microstructures reveal ferrite and austenite grains with fine precipitates within the ferrite grains. The study of the hardness and wear behaviors, of the samples indicated that the optimum properties were obtained for the sintering temperature of 1150 °C.

Compatibility of AlN with liquid lithium

NASA Astrophysics Data System (ADS)

Terai, T.; Suzuki, A.; Yoneoka, T.; Mitsuyama, T.

2000-12-01

Development of ceramic coatings is one of the most important subjects in liquid blanket research and development. Compatibility of sintered AlN and AlN coatings with liquid lithium, a candidate breeding material, was investigated. Sintered AlN with or without the sintering aid of Y 2O 3 examined in lithium at 773 K for 1390 h showed a slight decrease in electrical resistivity because of a reduction in Al 2O 3 impurity, though AlN and Y 2O 3 components themselves were subject to no severe corrosion. On the other hand, AlN ceramic coatings on SUS430 with high resistivity (> 10 11 Ω m) fabricated by the RF sputtering method disappeared in liquid lithium at 773 K in 56 h. This may be because cracks were formed due to the difference in thermal expansion between the coatings and the substrate or because the oxide formed between the two was removed by liquid lithium.

Yb:Y2O3 transparent ceramics processed with hot isostatic pressing

NASA Astrophysics Data System (ADS)

Wang, Jun; Ma, Jie; Zhang, Jian; Liu, Peng; Luo, Dewei; Yin, Danlei; Tang, Dingyuan; Kong, Ling Bing

2017-09-01

Highly transparent 5 at.% Yb:Y2O3 ceramics were fabricated by using a combination method of vacuum sintering and hot isostatic pressing (HIP). Co-precipitated Yb:Y2O3 powders, with 1 at.% ZrO2 as the sintering aid, were used as the starting material. The Yb:Y2O3 ceramics, vacuum sintered at 1700 °C for 2 h and HIPed at 1775 °C for 4 h, exhibited small grain size of 1.9 μm and highly dense microstructure. In-line optical transmittance of the ceramics reached 83.4% and 78.9% at 2000 and 600 nm, respectively. As the ceramic slab was pumped by a fiber-coupled laser diode at about 940 nm, a maximum output power of 0.77 W at 1076 nm was achieved, with a corresponding slope efficiency of 10.6%.

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

Influence of Y2O3 Addition on Crystallization, Thermal, Mechanical, and Electrical Properties of BaO-Al2O3-B2O3-SiO2 Glass-Ceramic for Ceramic Ball Grid Array Package

NASA Astrophysics Data System (ADS)

Li, Bo; Li, Wei; Zheng, Jingguo

2018-01-01

Y2O3 addition has a significant influence on the crystallization, thermal, mechanical, and electrical properties of BaO -Al2O3 -B2O3 -SiO2 (BABS) glass-ceramics. Semi-quantitative calculation based on x-ray diffraction demonstrated that with increasing Y2O3 content, both the crystallinity and the phase content of cristobalite gradually decreased. It is effective for the additive Y2O3 to inhibit the formation of cristobalite phase with a large coefficient of thermal expansion value. The flexural strength and the Young's modulus, thus, are remarkably increased from 140 MPa to 200 MPa and 56.5 GPa to 63.7 GPa, respectively. Also, the sintering kinetics of BABS glass-ceramics with various Y2O3 were investigated using the isothermal sintering shrinkage curve at different sintering temperatures. The sintering activation energy Q sharply decreased from 99.8 kJ/mol to 81.5 kJ/mol when 0.2% Y2O3 was added, which indicated that a small amount of Y2O3 could effectively promote the sintering procedure of BABS glass-ceramics.

Electrical and dielectric properties of Na1/2La1/2Cu3Ti4O12 ceramics prepared by high energy ball-milling and conventional sintering

NASA Astrophysics Data System (ADS)

Mahfoz Kotb, H.; Ahmad, Mohamad M.

2016-12-01

We report on the measurements of the electrical and dielectric properties of Na1/2La1/2Cu3Ti4O12 (NLCTO) ceramics prepared by high energy ball-milling and conventional sintering without any calcination steps. The x-ray powder diffraction analysis shows that pure perovskite-like CCTO phase is obtained after sintering at 1025 °C-1075 °C. Higher sintering temperatures result in multi-phase ceramics due to thermal decomposition. Scanning electron microscope observations reveal that the grain size is in a range of ˜3 μm-5μm for these ceramics. Impedance spectroscopy measurements performed in a wide frequency range (1 Hz-10 MHz) and at various temperatures (120 K-470 K) are used to study the dielectric and electrical properties of NLCTO ceramics. A good compromise between high ɛ‧ (5.7 × 103 and 4.1 × 103 at 1.1 kHz and 96 kHz, respectively) and low tan δ (0.161 and 0.126 at 1.1 kHz and 96 kHz, respectively) is obtained for the ceramic sintered at 1050 °C. The observed high dielectric constant behavior is explained in terms of the internal barrier layer capacitance effect.

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.

New potassium-sodium niobate lead-free piezoceramic: Giant-d33 vs. sintering temperature

NASA Astrophysics Data System (ADS)

Wu, Jiagang; Wang, Xiaopeng; Cheng, Xiaojing; Zheng, Ting; Zhang, Binyu; Xiao, Dingquan; Zhu, Jianguo; Lou, Xiaojie

2014-03-01

The objective of this work is to achieve a giant piezoelectric constant in (K,Na)NbO3-based lead-free ceramics, and then 0.96K0.46Na0.54Nb0.95Sb0.05O3-0.04Bi0.5(Na0.82K0.18)0.5ZrO3 lead-free piezoceramics were designed and prepared by optimizing the sintering temperature (TS). The rhombohedral-tetragonal phase boundary is found in the ceramics sintered at 1070 ˜ 1105 °C and is suppressed when sintered at low TS of 1060 ˜ 1065 °C. The threshold for TS is 1070 °C in terms of their ferroelectric and piezoelectric properties owing to the difference in the phase boundary and the microstructure, and a large d33 of 388 ˜ 465 pC/N could be attained in a wide TS range of 1070 ˜ 1105 °C, benefiting their practical applications because of broad TS. More interestingly, the ceramic sintered at 1075 °C has a giant d33 of ˜465 pC/N. We think that such a giant d33 of this material system can benefit the development of (K,Na)NbO3-based piezoceramics.

Thermal boundary resistance between liquid helium and silver sinter at low temperatures

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

Voncken, A.P.J.; Koenig, R.; Pobell, F.

1996-10-01

The authors present measurements of the thermal coupling between Ag sinter (nominal grain size {approx} 700{angstrom}) and superfluid {sup 3}He-B at p=0.3, 10, and 20 bar as well as a phase-separated {sup 3}He-{sup 4}He mixture at p=0.5 bar in the submillikelvin regime. In order to analyze the data of the pure {sup 3}He-B sample with respect to different contributions to the thermal resistance, a one-dimensional model for the heat flow in the sinter is presented. As a result it is shown that the thermal conductivity of the liquid in the sinter has to be taken into account to extract themore » temperature and pressure dependence of the boundary resistance in the confining geometry of the sinter. Depending on the value of this thermal conductivity, a boundary resistance proportional to T{sup {minus}2} or T{sup {minus}3} is found. Moreover, it is shown that a pressure dependence of the boundary resistance might be explained by a pressure dependence of the thermal conductivity of the liquid in the sinter. The data on the phase-separated mixture are equally well described by a T{sup {minus}2}- and a T{sup {minus}3}-dependence of the boundary resistance. The authors point out that a common problem in most measurements of the Kapitza resistance performed so far is the small temperature interval investigated, which usually does not allow a definite conclusion concerning the temperature dependence.« less

Structural and magnetic properties of spark plasma sintered Co-Mg-Zn substituted Ba-Sr hexagonal ferrite magnets

NASA Astrophysics Data System (ADS)

Harikrishnan, V.; Vizhi, R. Ezhil; Rajan Babu, D.; Saravanan, P.

2018-02-01

The effect of conventional and spark plasma sintering processes on the structural and magnetic properties of Ba0.5Sr0.5Fe12-2xCox(MgZn)x/2O19 (x = 0.2, 0.4 and 0.6) was investigated in this study. XRD patterns of both conventionally sintered (CS) and spark plasma sintered (SPS) samples with x = 0.2 and 0.4 showed the crystallization of Ba0.5Sr0.5Fe12O19-phase with space group of P63/mmc. However, in the case of SPS sample with x = 0.4, a secondary peak of α-Fe2O3 was observed. SEM analysis on the SPS samples revealed dense morphology with low porosity; while the CS samples showed the presence of aggregated particles with spherical shapes. Maximum values of saturation magnetization, MS (58 emu/g) and coercivity, HC (3.5 kOe) were obtained for the CS samples with x = 0.4; while their SPS counterparts revealed increased MS (65 emu/g) and HC (3.9 kOe) values. The observed magnetization reversal behaviour for both sintering conditions were not smooth in the case of x = 0.2, which indicated the existence of two-phase behavior. The temperature dependent magnetization studies for x = 0.2 and 0.4 were performed in order to analyze the variation in Curie temperature against Co-Mg-Zn substitution and the obtained results are discussed on the basis of crystallization of hexaferrite-phase.

Structure and properties of sintered MM-Fe-B magnets

NASA Astrophysics Data System (ADS)

Shang, R. X.; Xiong, J. F.; Li, R.; Zuo, W. L.; Zhang, J.; Zhao, T. Y.; Chen, R. J.; Sun, J. R.; Shen, B. G.

2017-05-01

MM14Fe79.9B6.1 magnets were prepared by conventional sintering method. The Curie temperature of the sintered MM2Fe14B magnet was about 210 °C. When the sintering temperature increased from 1010 °C to 1030 °C, the density of the magnet increased from 6.85 g/cm3 to 7.52 g/cm3. After the first stage tempering at 900 °C, the (BH)max and Hcj had a slight increase. The maximum value of (BH)max = 7.6 MGOe and Hcj = 1080 Oe was obtained when sintered at 1010 °C and tempering at 900 °C, respectively. The grain size grew very large when the sintering temperature increased to 1050 °C, and the magnetic properties deteriorated rapidly. La reduced by ˜ 7.5 at. % in grains, which is almost equal to the increased percentage of Nd. That is mainly because La-Fe-B is very difficult to form the 2: 14: 1 phase.

The Effects of High Al2O3 on the Metallurgical Properties of Sinter

NASA Astrophysics Data System (ADS)

Yu, Wen-tao; Zuo, Hai-bin; Zhang, Jian-liang; Zhang, Tao

Sintering-pot tests and metallurgical performances of sinter with 4 kind of different Al2O3 contents are experimented in this paper. Results show: when the Al2O3 contents increase from 2.0% to 3.5%, acicular calcium ferrites in mine phase will be gradually replaced by plate-like iron calcium. The increase of Al2O3 contents will lead to the addition of liquid viscosity and the reduction of permeability of sinter bed. Sintering time will be prolonged. The rate of yield is stable basically but production is low; besides, the increase of liquid viscosity will decrease of drum strength. The change of permeability of the material layer will make RDI+3.15 decrease first and then increase when Al2O3 contents changed from 2.0% to 3.5%. RI of sinter shows a contrary trend because many open voids are formed by deterioration of liquidity first and then pores closed.

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

Investigation of consolidation kinetics and microstructure evolution of Al alloys in direct metal laser sintering using phase field simulation

NASA Astrophysics Data System (ADS)

Bimal Satpathy, Bubloom; Nandy, Jyotirmoy; Sahoo, Seshadev

2018-03-01

Direct metal laser sintering is one of the very efficient processes which comes under the field of additive manufacturing and is capable of producing products of good mechanical and physical properties. The process parameters affect the physical and mechanical properties of the final products. Rapid solidification plays an important role in the consolidation kinetics as the powdered material sinters and forms a polycrystalline structure. In the recent times, the enormous use of computational modeling has helped in examining the utility of final products in a wide range of applications. In this study, a phase field model has been implemented to foresee the consolidation kinetics during the liquid state sintering. Temperature profiles have been used to study the densification behavior and neck growth which is caused by the surface diffusion of particles at initial stage. Later, importance of grain boundary and the volume diffusion during densification process is analyzed. It is also found that with rise in temperature, neck growth also increases rapidly due to the interaction of adjacent grains through grain boundary diffusion and stabilization of grain growth.

Correlative multi-scale characterization of a fine grained Nd-Fe-B sintered magnet.

PubMed

Sasaki, T T; Ohkubo, T; Hono, K; Une, Y; Sagawa, M

2013-09-01

The Nd-rich phases in pressless processed fine grained Nd-Fe-B sintered magnets have been characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and three dimensional atom probe tomography (3DAP). The combination of the backscattered electron (BSE) and in-lens secondary electron (IL-SE) images in SEM led to an unambiguous identification of four types of Nd-rich phases, NdOx, Ia3 type phase, which is isostructural to Nd₂O₃, dhcp-Nd and Nd₁Fe₄B₄. In addition, the 3DAP analysis of thin Nd-rich grain boundary layer indicate that the coercivity has a close correlation with the chemistry of the grain boundary phase. Copyright © 2013 Elsevier B.V. All rights reserved.

Sintering of compacts of UN, (U,Pu)N, and PuN

DOEpatents

Tennery, V.J.; Godfrey, T.G.; Bomar, E.S.

1973-10-16

>A method is provided for preparing a densified compact of a metal nitride selected from the group consisting of UN, (U,Pu)N, and PuN which comprises heating a green compact of at least one selected nitride in the mononitride single-phase region, as displayed by a phase diagram of the mononitride of said compact, in a nitrogen atmosphere at a pressure of nitrogen less than 760 torr. At a given temperature, this process produces a singlephase structure and a maximal sintered density as measured by mercury displacement. (Official Gazette)

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.

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

Colomer, M.T., E-mail: tcolomer@icv.csic.es; Kilner, J.A.

This work reports the effect of two different sintering times, 6 and 48 h on the structural, microstructural, and chemical features of Ni-doped La{sub 0.90}Sr{sub 0.10}GaO{sub 3.00−δ}. Independently of the sintering time, La{sub 0.90}Sr{sub 0.10}Ga{sub 1−x}Ni{sub x}O{sub 3.00−δ} (where x=0.10, and 0.20 (mol)) presents a rhombohedral symmetry with a lattice volume that decreases when NiO dopant increases. Besides the perovskite, LaSrGa{sub 3.00}O{sub 7.00} (nominal composition) is present as second phase in all cases. When the samples are doped with NiO, the peaks of this second phase are shifted with respect to the peaks of the pure phase. These shifts suggestmore » that this second phase could admit some Ni ions in its structure. According to the XRD patterns, the amount of the latter phase is larger when sintering time is increased. Electron probe microanalysis (EPMA) indicated that the matrix of the samples sintered for 6 h is constituted by a perovskite with an experimental composition very close to the nominal one. However, when the samples are sintered for 48 h the matrix of each sample is constituted by two perovskites; both with compositional deviations with respect to their nominal one. In particular, a significant Sr depletion compensated by a La increment in the A site is observed. Those compositional deviations could be mainly due to the diffusion of the cations in the bulk and/or from the bulk to the surface of the samples. That diffusion can favour the formation, not only, of a second perovskite with a different composition in relation with the first one formed, but also, the formation of second phases. In addition, a very slight broadening of Bragg peaks of the perovskites sintered for 48 h is observed by XRD and can be related to the presence of two different perovskites in each sample according to EPMA results. By BSEM and EPMA analyses La{sub 4.00}Ga{sub 2.00}O{sub 9.00} (nominal composition) is also observed as second phase when samples are treated for 48 h. - Graphical abstract: Typical microstructures, observed by FEG-SEM, of La{sub 0.90}Sr{sub 0.10}Ga{sub 1−x}Ni{sub x}O{sub 3.00−δ} materials with x=0.00 and 0.10 (nominal compositions) and sintered at 1450 °C for 48 h after polishing and thermal etching are shown. Lighter grey grains with a bimodal grain size are observed and according to XEDS analysis correspond to two perovskites with different experimental compositions (labelled as 1 and 2 for x=0.00 and labelled as 4 and 5 for x=0.10, respectively), meanwhile the darker grey phases correspond to LaSrGa{sub 3.00}O{sub 7.00} (labelled as 3 for x=0.00) and LaSr(Ga{sub 1−y′},Ni{sub y′}){sub 3.00}O{sub 7.00} (labelled as 6 for x=0.10), respectively. - Highlights: • When NiO is introduced into La{sub 0.90}Sr{sub 0.10}GaO{sub 3.00−δ} a change in symmetry is produced. • A significant Sr depletion in the A-site of perovskites treated for 48 h is observed. • Compositional deviations could be due to a thermally-activated diffusional process. • The phase purity of these materials is deteriorated when the sintering time is extended.« less

Ratio

NASA Astrophysics Data System (ADS)

Webster, Nathan A. S.; Pownceby, Mark I.; Madsen, Ian C.; Studer, Andrew J.; Manuel, James R.; Kimpton, Justin A.

2014-12-01

Effects of basicity, B (CaO:SiO2 ratio) on the thermal range, concentration, and formation mechanisms of silico-ferrite of calcium and aluminum (SFCA) and SFCA-I iron ore sinter bonding phases have been investigated using an in situ synchrotron X-ray diffraction-based methodology with subsequent Rietveld refinement-based quantitative phase analysis. SFCA and SFCA-I phases are the key bonding materials in iron ore sinter, and improved understanding of the effects of processing parameters such as basicity on their formation and decomposition may assist in improving efficiency of industrial iron ore sintering operations. Increasing basicity significantly increased the thermal range of SFCA-I, from 1363 K to 1533 K (1090 °C to 1260 °C) for a mixture with B = 2.48, to ~1339 K to 1535 K (1066 °C to 1262 °C) for a mixture with B = 3.96, and to ~1323 K to 1593 K (1050 °C to 1320 °C) at B = 4.94. Increasing basicity also increased the amount of SFCA-I formed, from 18 wt pct for the mixture with B = 2.48 to 25 wt pct for the B = 4.94 mixture. Higher basicity of the starting sinter mixture will, therefore, increase the amount of SFCA-I, considered to be more desirable of the two phases. Basicity did not appear to significantly influence the formation mechanism of SFCA-I. It did, however, affect the formation mechanism of SFCA, with the decomposition of SFCA-I coinciding with the formation of a significant amount of additional SFCA in the B = 2.48 and 3.96 mixtures but only a minor amount in the highest basicity mixture. In situ neutron diffraction enabled characterization of the behavior of magnetite after melting of SFCA produced a magnetite plus melt phase assemblage.

Electric field-assisted sintering of nanocrystalline hydroxyapatite for biomedical applications

NASA Astrophysics Data System (ADS)

Tran, Tien Bich

As the main inorganic component of bone, hydroxyapatite (HA, Ca 10(PO4)6(OH)2) should be an ideal candidate in biomaterials selection. When grain sizes are in the nanometric regime, protein adsorption and cell adhesion are enhanced, while strength, hardness, and wear resistance are improved. Unfortunately, low phase stability, poor sinterability, and a tendency towards exaggerated grain coarsening challenge full densification of nanocrystalline hydroxyapatite by conventional sintering methods. The field-assisted sintering technique (FAST) has successfully consolidated a variety of nanocrystalline metals and ceramics in dramatically reduced times. The sintering enhancements observed during FAST can be attributed to thermal and athermal effects. The rapid heating rates (up to ˜1000ºC/min) afforded by FAST contribute a significant thermal effect. Since fast heating rates reduce powder exposure to sub-sintering temperatures, non-densifying surface diffusion is limited. The athermal effects of FAST are less well understood and can include plasma generation, dielectric breakdown, particle surface cleaning, grain boundary pinning, and space charge effects. Applying the field-assisted sintering technique to nanocrystalline hydroxyapatite yielded surprising results. Deviations from conventional densification behavior were observed, with dehydroxylation identified as the most deleterious process to densification as well as mechanical and biological performance. Since hydroxyapatite is not a stable phase at high temperatures and low water partial pressure atmospheres, desintering due to dehydroxylation-related pore formation became apparent during Stage III sintering. In fact, the degree of desintering and pore formation increased with the extent of Stage III sintering and grain growth. The atomic rearrangements taking place during grain boundary migration are believed to favor the formation of more-stable oxyapatite through hydroxyapatite dehydroxylation. This behavior was consistent during varied heating rate (50--400ºC/min) and varied pressure application (25--90 MPa) studies. While in vitro cytocompatibility studies using MG63 osteoblast-like cells demonstrated the biocompatibility of the FAST-processed specimens, bioactivity was sensitive to processing parameters. Since extensive dehydroxylation reduces the surface charge of the sintered materials, apatite deposition during simulated body fluid immersion only occurred when dehydroxylation was mild---i.e., on specimens sintered at low temperatures (800--900ºC) or for short periods. Microstructural investigations revealed that HA sintered at temperatures above 900ºC under an applied electric field contained nanometric residual pores in grain interiors, as well as micron-sized dehydroxylation-related pores at grain boundaries and grain boundary junctions. These larger pores were responsible for the increasing embrittlement of specimens sintered at higher temperatures. Although grain size dependence could not be found in the 60--100 nm grain size range, fracture toughness (KIC = 1.92 MPa√m, maximum) increased with decreasing sintering temperature. Results from the suite of investigations conducted demonstrate that biocompatible and bioactive nanocrystalline hydroxyapatite with enhanced mechanical properties can be efficiently manufactured by field-assisted sintering under controlled processing conditions.

Method of joining ITM materials using a partially or fully-transient liquid phase

DOEpatents

Butt, Darryl Paul; Cutler, Raymond Ashton; Rynders, Steven Walton; Carolan, Michael Francis

2006-03-14

A method of forming a composite structure includes: (1) providing first and second sintered bodies containing first and second multicomponent metallic oxides having first and second identical crystal structures that are perovskitic or fluoritic; (2) providing a joint material containing at least one metal oxide: (a) containing (i) at least one metal of an identical IUPAC Group as at least one sintered body metal in one of the multicomponent metallic oxides, (ii) a first row D-Block transition metal not contained in the multicomponent metallic oxides, and/or (iii) a lanthanide not contained in the multicomponent metallic oxides; (b) free of metals contained in the multicomponent metallic oxides; (c) free of cations of boron, silicon, germanium, tin, lead, arsenic, antimony, phosphorus and tellurium; and (d) having a melting point below the sintering temperatures of the sintered bodies; and (3) heating to a joining temperature above the melting point and below the sintering temperatures.

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.

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.

Structure and characteristics of functional powder composite materials obtained by spark plasma sintering

NASA Astrophysics Data System (ADS)

Oglezneva, S. A.; Kachenyuk, M. N.; Kulmeteva, V. B.; Ogleznev, N. B.

2017-07-01

The article describes the results of spark plasma sintering of ceramic materials based on titanium carbide, titanium carbosilicide, ceramic composite materials based on zirconium oxide, strengthened by carbon nanostructures and composite materials of electrotechnical purpose based on copper with addition of carbon structures and titanium carbosilicide. The research shows that the spark plasma sintering can achieve relative density of the material up to 98%. The effect of sintering temperature on the phase composition, density and porosity of the final product has been studied. It was found that with addition of carbon nanostructures the relative density and hardness decrease, but the fracture strength of ZrO2 increases up to times 2. The relative erosion resistance of the electrodes made of composite copper-based powder materials, obtained by spark plasma sintering during electroerosion treatment of tool steel exceeds that parameter of pure copper up to times 15.

Molten salt synthesis of La0.8Sr0.2MnO3 powders for SOFC cathode electrode

NASA Astrophysics Data System (ADS)

Gu, Sin-il; Shin, Hyo-soon; Hong, Youn-woo; Yeo, Dong-hun; Kim, Jong-hee; Nahm, Sahn; Yoon, Sang-ok

2012-08-01

For La0.8Sr0.2MnO3 (LSM) perovskite, used as the cathode material for solid oxide fuel cells (SOFC), it is known that the formation of a triple-phase-boundary is restrained due to the formation of a second phase at the YSZ/electrode interface at high temperature. To decrease the 2nd phase, lowering the sintering temperature has been used. LSM powder was synthesized by molten salt synthesis method to control its particle size, shape, and agglomeration. We have characterized the phase formation, particle size, shape, and sintering behavior of LSM in the synthesis using the variation of KCl, LiCl, KF and its mixed salts as raw materials. In the case of KCl and KCl-KF salts, the particle size and shape of the LSM was well controlled and synthesized. However, in the case of LiCl and KCl-LiCl salts, LiMnOx as 2nd phase and LSM were synthesized simultaneously. In the case of the mixed salt of KCl-KF, the growth mechanism of the LSM particle was changed from `diffusion-controlled' to `reaction-controlled' according to the amount of mixed salt. The sintering temperature can be decreased below 1000 °C by using the synthesized LSM powder.

Possible observation of Griffith phase over large temperature range in plasma sintered La0.67Ca0.33MnO3

NASA Astrophysics Data System (ADS)

Mishra, D. K.; Roul, B. K.; Singh, S. K.; Srinivasu, V. V.

2018-02-01

We report on the possible observation of Griffith phase in a wide range of temperature (>272-378 K) in the 2.5 min plasma sintered La0.67Ca0.33MnO3 (LCMO) as deduced from careful electron spin resonance studies. This is 106 K higher than the paramagnetic to ferromagnetic transition (Curie transition ∼272 K) temperature. The indication of Griffith phase in such a wide range is not reported earlier by any group. We purposefully prepared LCMO samples by plasma sintering technique so as to create a disordered structure by rapid quenching which we believe, is the prime reason for the observation of Griffith Phase above the Curie transition temperature. The inverse susceptibility curve represents the existence of ferromagnetic cluster in paramagnetic region. The large resonance peak width (40-60 mT) within the temperature range 330-378 K confirms the sample magnetically inhomogeneity which is also established from our electron probe microstructure analysis (EPMA). EPMA establishes the presence of higher percentage of Mn3+ cluster in comparison to Mn4+. This is the reason for which Griffith state is enhanced largely to a higher range of temperature.

Effect of Sintering Temperature on Dielectric Properties of Iron Deficient Nickel-Ferrite

NASA Astrophysics Data System (ADS)

Rani, Renu; Singh, Sangeeta; Juneja, J. K.; Prakash, Chandra; Raina, K. K.

2011-11-01

Nickel Ferrite among all the magneto ceramic materials have been studied very much due to its large number of applications. But there is a large scope of modification of its properties. Thus people still working on it for improvisation of its properties via compositional and structural modifications. Present paper reporting the preparation and characterization of iron deficient Nickel ferrite for different sintering temperature. Ferrite samples having the general formula NiFe1.98O4 were prepared using the standard ceramic method. The phase formation was confirmed by X-ray diffraction technique. The effect of sintering temperature on the electrical properties and resistivity was studied. The data shows that dielectric properties are highly dependent on the sintering temperature.

Comparison of aged polyamide powders for selective laser sintering

NASA Astrophysics Data System (ADS)

Martínez, A.; Ibáñez, A.; Sánchez, A.; León, M. A.

2012-04-01

Selective Laser Sintering (SLS) is an additive manufacturing technology in which a three-dimensional object is manufactured layer by layer by melting powder materials with heat generated from a CO2 laser. However, a disadvantage of sintered materials is that the unsintered powder material during the process can be reused only a limited number of cycles, as during the heating phase in the sintering chamber the material remains at a temperature near the fusion point for a certain period of time and lose properties. This work shows the study of two polyamides (PA12)-based powders used in SLS with the aim of understanding the modification of their properties mainly with the temperature and the time at which they are exposed during the processing.

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

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.

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.

Temperature, Crystalline Phase and Influence of Substrate Properties in Intense Pulsed Light Sintering of Copper Sulfide Nanoparticle Thin Films.

PubMed

Dexter, Michael; Gao, Zhongwei; Bansal, Shalu; Chang, Chih-Hung; Malhotra, Rajiv

2018-02-02

Intense Pulsed Light sintering (IPL) uses pulsed, visible light to sinter nanoparticles (NPs) into films used in functional devices. While IPL of chalcogenide NPs is demonstrated, there is limited work on prediction of crystalline phase of the film and the impact of optical properties of the substrate. Here we characterize and model the evolution of film temperature and crystalline phase during IPL of chalcogenide copper sulfide NP films on glass. Recrystallization of the film to crystalline covellite and digenite phases occurs at 126 °C and 155 °C respectively within 2-7 seconds. Post-IPL films exhibit p-type behavior, lower resistivity (~10 -3 -10 -4  Ω-cm), similar visible transmission and lower near-infrared transmission as compared to the as-deposited film. A thermal model is experimentally validated, and extended by combining it with a thermodynamic approach for crystal phase prediction and via incorporating the influence of film transmittivity and optical properties of the substrate on heating during IPL. The model is used to show the need to a-priori control IPL parameters to concurrently account for both the thermal and optical properties of the film and substrate in order to obtain a desired crystalline phase during IPL of such thin films on paper and polycarbonate substrates.

Phase composition and in vitro bioactivity of porous implants made of bioactive glass S53P4.

PubMed

Fagerlund, S; Massera, J; Moritz, N; Hupa, L; Hupa, M

2012-07-01

This work studied the influence of sintering temperature on the phase composition, compression strength and in vitro properties of implants made of bioactive glass S53P4. The implants were sintered within the temperature range 600-1000°C. Over the whole temperature range studied, consolidation took place mainly via viscous flow sintering, even though there was partial surface crystallization. The mechanical strength of the implants was low but increased with the sintering temperature, from 0.7 MPa at 635°C to 10 MPa at 1000°C. Changes in the composition of simulated body fluid (SBF), the immersion solution, were evaluated by pH measurements and ion analysis using inductively coupled plasma optical emission spectrometry. The development of a calcium phosphate layer on the implant surfaces was verified using scanning electron microscopy-electron-dispersive X-ray analysis. When immersed in SBF, a calcium phosphate layer formed on all the samples, but the structure of this layer was affected by the surface crystalline phases. Hydroxyapatite formed more readily on amorphous and partially crystalline implants containing both primary Na(2)O·CaO·2SiO(2) and secondary Na(2)Ca(4)(PO(4))(2)SiO(4) crystals than on implants containing only primary crystals. Copyright © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Phase identification and morphology study of hematite (Fe2O3) with sintering time varitions

NASA Astrophysics Data System (ADS)

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

2017-09-01

Iron oxide has been the interest of many studies due to its applications in various scientific and industrial fields including in environment, corrosion, soil science, and exhaust emissions. Iron oxide (Fe2O3) has potential applications in catalytic reactions in electronic devices such as semiconductors, paint formulations, and lithium rechargeable batteries. Fe2O3 can be synthesized through the process of stirring, decomposition of organic iron, sol-gel, combustion, and evaporating solvents. Most of the methods used involve several steps and take a long time. The aim of this research was to investigate the phase and morphology characterization of iron oxide (Fe2O3) powder with solvent ethylene glycol after being sintered for 1 hour, 2 hours and 3 hours. The characterization tools utilized were XRD, SEM-EDX, and FTIR. The results of XRD analysis showed that the Fe2O3 sintered for 1 hour had the smallest crystallite size with a diameter of 21.05 nm. In the XRD test, the beam of X-ray was shot directly at the grain being tested. The results of SEM analysis showed thatthe Fe2O3 sintered for 1 hour produced the best result due to its crystallite size of 12.36 nm and hada shape of homogeneous nanosphere; the duration of sintering indeed had a great influence on the grain size of iron oxide (Fe2O3). In addition, the results of the elemental composition analysis indicate that the longer the sintering process, the higher the concentration of O but the lower the Fe.

Densification, phase stability and in vitro biocompatibility property of hydroxyapatite-10 wt% silver composites.

PubMed

Nath, Shekhar; Kalmodia, Sushma; Basu, Bikramjit

2010-04-01

In this paper, we demonstrate how a simple fabrication route, i.e., pressureless sintering of mechanically mixed powders can be employed to develop hydroxyapatite (HAp, Ca(10)(PO(4))(6)(OH)(2))-silver (Ag) bioceramic composites with superior combination of physical (hardness, toughness), non-cytotoxicity, cytocompatiblity and anti-microbial property. The densification results show that such composites can be sintered at 1200 degrees C for 2 h near to theoretical density (>98% rho(th).) An important observation is that the dissociation of HAp phase can be prevented during sintering up to 1300 degrees C for 2 h in HAp-10 wt% Ag composites. The stability of HAp in presence of silver is discussed in reference to the results obtained using XRD, FTIR and Raman spectroscopy. The hardness values of the composites are comparable (approximately 6.5 GPa) to that of pure HAp, despite of the presence of softer Ag particles. The sintered composites exhibit modest crack growth resistance property and their toughness varies in the range of 0.9-1.2 MPa m(0.5), depending on sintering temperature. For selected samples, the in vitro characterization was performed using mouse fibroblast (L929) and human osteosarcoma (MG63) cell lines. The combination of biochemical assays (MTT, ALP and osteocalcin) confirm that HAp-10 wt% Ag biocomposites have comparable or even better cellular viability, osteogenic differentiation and bone mineralization as well as osteoinduction property. Antibacterial experiments involving gram-negative bacteria, Escherichia coli confirm excellent bactericidal property of HAp-10 wt% Ag composites, sintered using mechanically mixed powders.

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.

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.

Reaction-sintered porous mineral-based mullite ceramic membrane supports made from recycled materials.

PubMed

Dong, Yingchao; Zhou, Jian-Er; Lin, Bin; Wang, Yongqing; Wang, Songlin; Miao, Lifeng; Lang, Ying; Liu, Xingqin; Meng, Guangyao

2009-12-15

Bulk porous mullite supports for ceramic membranes were prepared directly using a mixture of industrial waste fly ash and bauxite by dry-pressing, followed by sintering between 1200 and 1550 degrees C. The effects of sintering temperature on the phase composition and shrinkage percent of porous mullite were studied. The XRD results indicate that secondary mullitization reaction took place above 1200 degrees C, and completed at 1450 degrees C. During sintering, the mixture samples first shrunk, then expanded abnormally between 1326 and 1477 degrees C, and finally shrunk again above 1477 degrees C. This unique volume self-expansion is ascribed to the secondary mullitization reaction between bauxite and fly ash. More especially, the micro-structural variations induced by this self-expansion sintering were verified by SEM, porosity, pore size distribution and nitrogen gas permeation flux. During self-expansion sintering, with increasing temperature, an abnormal increase in both open porosity and pore size is observed, which also results in the increase of nitrogen gas flux. The mineral-based mullite supports with increased open porosity were obtained. Furthermore, the sintered porous mullite membrane supports were characterized in terms of thermal expansion co-efficient and mechanical strength.

Grain growth effects on magnetic properties of Ni0.6Zn0.4Fe2O4 material prepared using mechanically alloyed nanoparticles

NASA Astrophysics Data System (ADS)

Syazwan, M. M.; Hapishah, A. N.; Azis, R. S.; Abbas, Z.; Hamidon, M. N.

2018-06-01

The effect of grain growth via sintering temperature on some magnetic properties is reported in this research. Ni0.6Zn0.4Fe2O4 nanoparticles were mechanically alloyed for 6 h and the sintering process starting from 600 to 1200 °C with 25 °C increment with only one sample subjected to all sintering scheme. The resulting change in the material was observed after each sintering. Single phase has been formed at 600 °C and above and the intensity peaks increased with sintering temperature as well as crystallinity increment. The morphological studies showed grain size increment as the sintering temperature increased. Moreover, the density increased while the porosity decreased with increasing sintering temperature. The saturation induction, Bs increased with the increased of grain size. On the other hand, the coercivity-vs-grain size plot reveals the critical single-domain-to-multidomain grain size to be about ∼400 nm. The initial permeability, μi value was increased with grain size enhancement. The microstructural grain growth, as exposed for the first time by this research, is shown as a process of multiple activation energy barriers.

Copper sludge from printed circuit board production/recycling for ceramic materials: a quantitative analysis of copper transformation and immobilization.

PubMed

Tang, Yuanyuan; Lee, Po-Heng; Shih, Kaimin

2013-08-06

The fast development of electronic industries and stringent requirement of recycling waste electronics have produced a large amount of metal-containing waste sludge. This study developed a waste-to-resource strategy to beneficially use such metal-containing sludge from the production and recycling processes of printed circuit board (PCBs). To observe the metal incorporation mechanisms and phase transformation processes, mixtures of copper industrial waste sludge and kaolinite-based materials (kaolinite and mullite) were fired between 650 and 1250 °C for 3 h. The different copper-hosting phases were identified by powder X-ray diffraction (XRD) in the sintered products, and CuAl2O4 was found to be the predominant hosting phase throughout the reactions, regardless of the strong reduction potential of copper expected at high temperatures. The experimental results indicated that CuAl2O4 was generated more easily and in larger quantities at low-temperature processing when using the kaolinite precursor. Maximum copper transformations reached 86% and 97% for kaolinite and mullite systems, respectively, when sintering at 1000 °C. To monitor the stabilization effect after thermal process, prolonged leaching tests were carried out using acetic acid with an initial pH value of 2.9 to leach the sintered products for 20 days. The results demonstrated the decrease of copper leachability with the formation of CuAl2O4, despite different sintering behavior in kaolinite and mullite systems. This study clearly indicates spinel formation as the most crucial metal stabilization mechanism when sintering copper sludge with aluminosilicate materials, and suggests a promising and reliable technique for reusing metal-containing sludge as ceramic materials.

Cu ion ink for a flexible substrate and highly conductive patterning by intensive pulsed light sintering.

PubMed

Wang, Byung-Yong; Yoo, Tae-Hee; Song, Yong-Won; Lim, Dae-Soon; Oh, Young-Jei

2013-05-22

Direct printing techniques that utilize nanoparticles to mitigate environmental pollution and reduce the processing time of the routing and formation of electrodes have received much attention lately. In particular, copper (Cu) nanoink using Cu nanoparticles offers high conductivity and can be prepared at low cost. However, it is difficult to produce homogeneous nanoparticles and ensure good dispersion within the ink. Moreover, Cu particles require a sintering process over an extended time at a high temperature due to high melting temperature of Cu. During this process, the nanoparticles oxidize quickly in air. To address these problems, the authors developed a Cu ion ink that is free of Cu particles or any other impurities. It consequently does not require separate dispersion stability. In addition, the developed ink is environmentally friendly and can be sintered even at low temperatures. The Cu ion ink was sintered on a flexible substrate using intense pulsed light (IPL), which facilitates large-area, high-speed calcination at room temperature and at atmospheric pressures. As the applied light energy increases, the Cu2O phase diminishes, leaving only the Cu phase. This is attributed to the influence of formic acid (HCOOH) on the Cu ion ink. Only the Cu phase was observed above 40 J cm(-2). The Cu-patterned film after sintering showed outstanding electrical resistivity in a range of 3.21-5.27 μΩ·cm at an IPL energy of 40-60 J cm(-2). A spiral-type micropattern with a line width of 160 μm on a PI substrate was formed without line bulges or coffee ring effects. The electrical resistivity was 5.27 μΩ·cm at an energy level of 40.6 J cm(-2).

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.

Improved magnetic properties of barium hexaferrite by CoFe2O4 nanoparticles prepared by ultrasonic irradiation

NASA Astrophysics Data System (ADS)

Nastiti, G.; Manaf, A.

2017-07-01

Magnetic properties of composite magnets made of nanoparticles of Barium Hexaferrite (BHF) and CoFe2O4 were reported in this paper. The two types of magnetic particles have a high total magnetization value which was required for permanent magnet applications. Both CoFe2O4 and BHF were synthesized through mechanical alloying coupled with high-frequency ultrasonic irradiation. In this respect, mechanically milled BHF precursors was sintered at a temperature of 1250 °C for 2 hours leading to single-phase powders. A similar method was also employed in the preparation of CoFe2O4 materials, but this required a relatively longer sintering time up to 12 hours at a sintering temperature of 900 °C. Composite magnets were obtained after sintering the mechanically mixed the two types of nanoparticles as constituted components of the composite. The hysteresis loop of CoFe2O4 materials as evaluated by Vibrating Sample Magnetometer (VSM) showing soft magnetic phase with a total magnetization value of 0.47 T and a coercivity of 47.37 kA/m. It is shown that the magnetic properties of composite magnets are a composition dependent in which the remanent was enhanced above the value of an isotropic single phase BHF magnet. The enhancement in remanent magnetization raised the effect of grain exchange interaction between hard and soft magnetic phases. The microstructure studied by X-Ray diffraction (XRD), Particle Size Analyzer (PSA) and their respective enhancement in magnetic properties are discussed in detail in term of grain exchange interactions.

Effects of the copper content on the structural and electrical properties of Cu2ZnSnSe4 bulks

NASA Astrophysics Data System (ADS)

Tsega, Moges; Dejene, F. B.; Koao, L. F.

2016-01-01

We have investigated the concept of defect in CuxZnSnSe4 (x=1.6-2.0) and Cuy(Zn0.9Sn1.1)Se4 (y= 1.6-2.0) bulks prepared by liquid-phase sintering at 600 °C for 2 h with soluble sintering aids of Sb2S3 and Te. All samples were found to exhibit p-type semiconductor for CuxZnSnSe4, while n-type of behavior obtained at y= 1.8-2.0 for Cuy(Zn0.9Sn1.1)Se4 pellets. The Cu vacancy acts as an acceptor point defect to form the p-type semiconductor, and Sn4+ acts as a donor to form the n-type behavior for the Sn-rich CZTSe. SEM images of pellets show dense surface morphology, and increase in grain size upon Cu inclusion. The largely increased Hall mobility and the slightly changed carrier concentration for Cuy(Zn0.9Sn1.1)Se4 with increasing the Cu content is related to the types of its defects. At y=2.0 with carrier concentration of 4.88×1017 cm-3 showed the highest mobility of around 58 cm2/V s. Based upon the proposed point defects, the CZTSe property can be consistently explained.

Marginal Accuracy and Internal Fit of 3-D Printing Laser-Sintered Co-Cr Alloy Copings.

PubMed

Kim, Myung-Joo; Choi, Yun-Jung; Kim, Seong-Kyun; Heo, Seong-Joo; Koak, Jai-Young

2017-01-23

Laser sintered technology has been introduced for clinical use and can be utilized more widely, accompanied by the digitalization of dentistry and the development of direct oral scanning devices. This study was performed with the aim of comparing the marginal accuracy and internal fit of Co-Cr alloy copings fabricated by casting, CAD/CAM (Computer-aided design/Computer-assisted manufacture) milled, and 3-D laser sintered techniques. A total of 36 Co-Cr alloy crown-copings were fabricated from an implant abutment. The marginal and internal fit were evaluated by measuring the weight of the silicone material, the vertical marginal discrepancy using a microscope, and the internal gap in the sectioned specimens. The data were statistically analyzed by One-way ANOVA (analysis of variance), a Scheffe's test, and Pearson's correlation at the significance level of p = 0.05, using statistics software. The silicone weight was significantly low in the casting group. The 3-D laser sintered group showed the highest vertical discrepancy, and marginal-, occlusal-, and average- internal gaps ( p < 0.05). The CAD/CAM milled group revealed a significantly high axial internal gap. There are moderate correlations between the vertical marginal discrepancy and the internal gap variables ( r = 0.654), except for the silicone weight. In this study, the 3-D laser sintered group achieved clinically acceptable marginal accuracy and internal fit.

Marginal Accuracy and Internal Fit of 3-D Printing Laser-Sintered Co-Cr Alloy Copings

PubMed Central

Kim, Myung-Joo; Choi, Yun-Jung; Kim, Seong-Kyun; Heo, Seong-Joo; Koak, Jai-Young

2017-01-01

Laser sintered technology has been introduced for clinical use and can be utilized more widely, accompanied by the digitalization of dentistry and the development of direct oral scanning devices. This study was performed with the aim of comparing the marginal accuracy and internal fit of Co-Cr alloy copings fabricated by casting, CAD/CAM (Computer-aided design/Computer-assisted manufacture) milled, and 3-D laser sintered techniques. A total of 36 Co-Cr alloy crown-copings were fabricated from an implant abutment. The marginal and internal fit were evaluated by measuring the weight of the silicone material, the vertical marginal discrepancy using a microscope, and the internal gap in the sectioned specimens. The data were statistically analyzed by One-way ANOVA (analysis of variance), a Scheffe’s test, and Pearson’s correlation at the significance level of p = 0.05, using statistics software. The silicone weight was significantly low in the casting group. The 3-D laser sintered group showed the highest vertical discrepancy, and marginal-, occlusal-, and average- internal gaps (p < 0.05). The CAD/CAM milled group revealed a significantly high axial internal gap. There are moderate correlations between the vertical marginal discrepancy and the internal gap variables (r = 0.654), except for the silicone weight. In this study, the 3-D laser sintered group achieved clinically acceptable marginal accuracy and internal fit. PMID:28772451

Bonding of TRIP-Steel/Al2O3-(3Y)-TZP Composites and (3Y)-TZP Ceramic by a Spark Plasma Sintering (SPS) Apparatus

PubMed Central

Miriyev, Aslan; Grützner, Steffen; Krüger, Lutz; Kalabukhov, Sergey; Frage, Nachum

2016-01-01

A combination of the high damage tolerance of TRIP-steel and the extremely low thermal conductivity of partially stabilized zirconia (PSZ) can provide controlled thermal-mechanical properties to sandwich-shaped composite specimens comprising these materials. Sintering the (TRIP-steel-PSZ)/PSZ sandwich in a single step is very difficult due to differences in the sintering temperature and densification kinetics of the composite and the ceramic powders. In the present study, we successfully applied a two-step approach involving separate SPS consolidation of pure (3Y)-TZP and composites containing 20 vol % TRIP-steel, 40 vol % Al2O3 and 40 vol % (3Y)-TZP ceramic phase, and subsequent diffusion joining of both sintered components in an SPS apparatus. The microstructure and properties of the sintered and bonded specimens were characterized. No defects at the interface between the TZP and the composite after joining in the 1050–1150 °C temperature range were observed. Only limited grain growth occurred during joining, while crystallite size, hardness, shear strength and the fraction of the monoclinic phase in the TZP ceramic virtually did not change. The slight increase of the TZP layer’s fracture toughness with the joining temperature was attributed to the effect of grain size on transformation toughening. PMID:28773680

Effect of sintering temperature on physical, structural and optical properties of wollastonite based glass-ceramic derived from waste soda lime silica glasses

NASA Astrophysics Data System (ADS)

Almasri, Karima Amer; Sidek, Hj. Ab Aziz; Matori, Khamirul Amin; Zaid, Mohd Hafiz Mohd

The impact of different sintering temperatures on physical, optical and structural properties of wollastonite (CaSiO3) based glass-ceramics were investigated for its potential application as a building material. Wollastonite based glass-ceramics was provided by a conventional melt-quenching method and followed by a controlled sintering process. In this work, soda lime silica glass waste was utilized as a source of silicon. The chemical composition and physical properties of glass were characterized by using Energy Dispersive X-ray Fluorescence (EDXRF) and Archimedes principle. The Archimedes measurement results show that the density increased with the increasing of sintering temperature. The generation of CaSiO3, morphology, size and crystal phase with increasing the heat-treatment temperature were examined by field emission scanning electron microscopy (FESEM), Fourier transforms infrared reflection spectroscopy (FTIR), and X-ray diffraction (XRD). The average calculated crystal size gained from XRD was found to be in the range 60 nm. The FESEM results show a uniform distribution of particles and the morphology of the wollastonite crystal is in relict shapes. The appearance of CaO, SiO2, and Ca-O-Si bands disclosed from FTIR which showed the formation of CaSiO3 crystal phase. In addition to the calculation of the energy band gap which found to be increased with increasing sintering temperature.

Preparation and evaluation of silicon nitride matrices for silicon nitride-SiC fiber composites. M.S. Thesis Final Technical Report

NASA Technical Reports Server (NTRS)

Axelson, Scott R.

1988-01-01

Continuous silicon carbide (SiC) fiber was added to three types of silicon nitride (Si3N4) matrices. Efforts were aimed at producing a dense Si3N4 matrix from reaction-bonded silicon nitride (RBSN) by hot-isostatic-pressing (HIP) and pressureless sintering, and from Si3N4 powder by hot-pressing. The sintering additives utilized were chosen to allow for densification, while not causing severe degradation of the fiber. The ceramic microstructures were evaluated using scanning optical microscopy. Vickers indentation was used to determine the microhardness and fracture toughness values of the matrices. The RBSN matrices in this study did not reach more than 80 percent of theoretical density after sintering at various temperatures, pressures, and additive levels. Hot-pressing Si3N4 powder produced the highest density matrices; hardness and toughness values were within an order of magnitude of the best literature values. The best sintering aid composition chosen included Y2O3, SiO2, and Al2O3 or AlN. Photomicrographs demonstrate a significant reduction of fiber attack by this additive composition.

Slip casting and extruding shapes of rhemium with metal oxide additives. Part 2: Development of grain stabilized rhenium parts for resistojets

NASA Technical Reports Server (NTRS)

Barr, Francis A.; Page, Russell J.

1987-01-01

The adaptation of the powdered particle process used for pure metal oxides to the coprocessing of rhenium oxides suitable to produce pure miniature resistojet hardware has been successful. Both slip casting and extrusion processes were used. The metal oxide ZrO2 was stabilized into the cubic phase with Y2O3, for use as a potentially grain stabilizing additive to rhenium. Straight meter long tubing in two sizes are reported. Tubing suitable for resistojet ohmic heater use of fully fired dimensions of nominally 3.8 mm o.d. x 2.2 mm i.d.. and 1.26 mm o.d. x .45 mm i.d. with 0, 0.5, 1.0 and 5.0% zirconia additives were produced for further study. Photomicrographs of these are discussed. The addition of the metal oxide zirconia to rhenium resulted in more dense and less porous parts. The additions of phase stabilized zirconia most likely act as a sintering aid. Tubes of varying diameter were slip cast which were representative of miniature pressure cases.

Effect of titanium addition on the thermal properties of diamond/cu-ti composites fabricated by pressureless liquid-phase sintering technique.

PubMed

Chung, Chih-Yu; Chu, Chao-Hung; Lee, Mu-Tse; Lin, Chun-Ming; Lin, Su-Jien

2014-01-01

In this study, minor-addition elements such as Si, Co, Cr, W, Mo, and Ti were added to matrix to improve the wettability between the diamonds and Cu matrix. The pressureless liquid-phase sintering technique adopted in this study provides a low-cost method for producing diamond/Cu composites with high potential for industrial mass production. Thermal properties of the diamond/Cu-Ti composites fabricated by pressureless liquid-phase sintering at 1373 K with variation in Ti contents were thoroughly investigated. XRD and TEM analysis show that TiC layer formed in the interface between Cu and diamond. The composites exhibited thermal conductivity as high as 620 W/m · K for 50 vol% diamond/Cu-0.6 at % Ti composite with diamond particle size of 300 µm. This value comes up to 85% of the thermal conductivity calculated by the Hasselman and Johnson (H-J) theoretical analysis. Under these conditions, a suitable coefficient of thermal expansion of 6.9 ppm/K was obtained.

Effect of Titanium Addition on the Thermal Properties of Diamond/Cu-Ti Composites Fabricated by Pressureless Liquid-Phase Sintering Technique

PubMed Central

Chung, Chih-Yu; Chu, Chao-Hung; Lee, Mu-Tse; Lin, Chun-Ming; Lin, Su-Jien

2014-01-01

In this study, minor-addition elements such as Si, Co, Cr, W, Mo, and Ti were added to matrix to improve the wettability between the diamonds and Cu matrix. The pressureless liquid-phase sintering technique adopted in this study provides a low-cost method for producing diamond/Cu composites with high potential for industrial mass production. Thermal properties of the diamond/Cu-Ti composites fabricated by pressureless liquid-phase sintering at 1373 K with variation in Ti contents were thoroughly investigated. XRD and TEM analysis show that TiC layer formed in the interface between Cu and diamond. The composites exhibited thermal conductivity as high as 620 W/m·K for 50 vol% diamond/Cu-0.6  at % Ti composite with diamond particle size of 300 µm. This value comes up to 85% of the thermal conductivity calculated by the Hasselman and Johnson (H-J) theoretical analysis. Under these conditions, a suitable coefficient of thermal expansion of 6.9 ppm/K was obtained. PMID:24715816

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.

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.

Improving hardness and toughness of boride composites based on aluminum magnesium boride

NASA Astrophysics Data System (ADS)

Peters, Justin Steven

The search for new super-hard materials has usually focused on strongly bonded, highly symmetric crystal structures similar to diamond. The two hardest single-phase materials, diamond and cubic boron nitride (cBN), are metastable, and both must be produced at high temperatures and pressures, which makes their production costly. In 2000, a superhard composite based on a low-symmetry, boron-rich compound was reported. Since then, many advances have been made in the study of this AlMgB14--TiB2 composite. The composite has been shown to exhibit hardness greater than either of its constituent phases, relying on its sub-micron microstructure to provide hardening and strengthening mechanisms. With possible hardness around 40 GPa, an AlMgB 14--60 vol% TiB2 approaches the hardness of cBN, yet is amenable to processing under ambient pressure conditions. There are interesting aspects of both the AlMgB14 and TiB 2 phases. AlMgB14 is comprised of a framework of boron, mostly in icosahedral arrangements. It is part of a family of 12 known compounds with the same boron lattice, with the metal atoms replaced by Li, Na, Y or a number of Lanthanides. Another peculiar trait of this family of compounds is that every one contains a certain amount of intrinsic vacancies on one or both of the metal sites. These vacancies are significant, ranging from 3 to 43% of sites depending on the composition. TiB2 is a popular specialty ceramic material due to its high hardness, moderate toughness, good corrosion resistance, and high thermal and electrical conductivity. The major drawback is the difficulty of densification of pure TiB2 ceramics. A combination of sintering aids, pressure, and temperatures of 1800°C are often required to achieve near full density articles. The AlMgB14--TiB2 composites can achieve 99% density from hotpressing at 1400°C. This is mostly due to the preparation of powders by a high-energy milling technique known as mechanical alloying. The resulting fine powders have high activity, and Fe from wear debris acts as a sintering aid. Mechanical alloying improves the sinterability of the composite material, it has the same effect on pure TiB2. TiB 2 processed by high-energy milling has been found to achieve 99% theoretical density at 1400°C with the addition of ˜1 wt% Fe. Both the AlMgB14--TiB2 composites and pure TiB2 produced from these methods have enhanced mechanical properties due to their fine microstructures. These materials show exceptional promise in the field of wear resistance. This includes cutting tools, erosion resistant coatings, and low-friction sliding contacts to name a few. Under certain wear conditions, the composite material can show performance on par with that of current high-end cBN and WC materials tailored for wear resistance. The composite material also exhibits low reactivity with Ti alloys, a pre-requisite for effective machining of these alloys, a trait that few hard materials possess.

Monolithic Pellets, Composites and Thick Films of Hydroxyapatite: Correlation of Mechanical Properties with Microstructure.

NASA Astrophysics Data System (ADS)

Wang, Pauchiu Either

Hydroxyapatite Ca_{10}(PO _4)_6(OH)_2 (abbreviated as HA) has great biocompatibility. Poor mechanical properties of HA implants and decomposition of HA during processing are the major obstacles for widespread uses of HA. In the present thesis we have attempted to understand the sintering behavior of monolithic HA and metal-reinforced HA-matrix composites, and the mechanism of formation of HA coating in the solutions at the normal temperature. The powders of two calcium phosphates, namely hydroxyapatite and dicalcium phosphate (DCP: chemical formula Ca_2P_2O_7), were sintered at various temperatures and in various environments. The density, flexural strength and knoop hardness of both phosphates sintered in air for 4 h initially increased with the sintering temperature, reaching maxima at around 1000-1150 ^circC, and then decreased due to decomposition. To reduce dehydroxylation, HA powder was sintered in moisture at various temperatures up to 1350^circ C and X-ray diffraction study did not indicate any decomposition at the highest sintering temperature. It is seen that dehydroxylation did not hinder sintering, but decomposition obstructed sintering of both HA and DCP. Ductile-phase reinforcement of hydroxyapatite was achieved by addition of silver particulates (5-30 vol.%) in HA powder compacts. A composite made by sintering 10 vol.% Ag and balance HA at 1200^circ C for 1 h in air had flexural strength of 75 +/- 7 MPa, which was almost double that of pure HA sintered under an identical condition. Silver in the composite melted during sintering, but due to poor wetting, did not spread in between HA particles. The increase in the flexural strength of the composites was thought to be due to crack-bridging and crack-arrest by silver inclusions. Thick films (several μm) of hydroxyapatite were deposited on silicon single crystal placed in close proximity to a plate of apatite- and wollastonite -containing glass and dipped into a simulated body fluid (SBF) at 36^circC. Amorphous calcium phosphate phase present in the glass leached into the SBF, causing supersaturation of Ca^ {2+} and (PO_4)^ {3-} ions. HA films grown on Si(111) showed strong (102) texture. As a contrast hardly any HA film could be grown on Si(100) surface. Our results suggest that the driving force for formation of apatite films arises from lowering of free energy of the supersatured solution by deposition of ions in certain crystallographic arrangements on suitable substrates with low interface energies.

Influence of sintering temperature on the characteristics of shale brick containing oil well-derived drilling waste.

PubMed

Li, Xiang-Guo; Lv, Yang; Ma, Bao-Guo; Jian, Shou-Wei; Tan, Hong-Bo

2011-11-01

The influence of sintering temperature on the physico-mechanical characteristics (such as water absorption, apparent porosity, bulk density, weight loss on ignition, firing shrinkage, and compressive strength), leachability, and microstructure of shale brick containing oil well-derived drilling waste (DW) was investigated. The experiments were conducted at a temperature ranging from 950°C to 1,050°C with 30% DW addition. The results indicate that increasing the sintering temperature decreases the water absorption and apparent porosity and increases the shrinkage, density, and compressive strength of sintered specimens. Moreover, the physico-mechanical properties of samples sintered at 1,050°C meet the requirements of the MU20 according to GB/T 5101-2003 (in China). The heavy metal concentrations of the leachate are much lower than the current regulatory limits according to GB16889-2008. The results from XRD and SEM show that increasing sintering temperature results in an increase of the high temperature liquid phase, which may have a significant effect on the densification process of the samples.

NiTi-Nb micro-trusses fabricated via extrusion-based 3D-printing of powders and transient-liquid-phase sintering.

PubMed

Taylor, Shannon L; Ibeh, Amaka J; Jakus, Adam E; Shah, Ramille N; Dunand, David C

2018-06-15

We present a novel additive manufacturing method for NiTi-Nb micro-trusses combining (i) extrusion-based 3D-printing of liquid inks containing NiTi and Nb powders, solvents, and a polymer binder into micro-trusses with 0/90° ABAB layers of parallel, ∼600 µm struts spaced 1 mm apart and (ii) subsequent heat-treatment to remove the binder and solvents, and then bond the NiTi powders using liquid phase sintering via the formation of a transient NiTi-Nb eutectic phase. We investigate the effects of Nb concentration (0, 1.5, 3.1, 6.7 at.% Nb) on the porosity, microstructure, and phase transformations of the printed NiTi-Nb micro-trusses. Micro-trusses with the highest Nb content exhibit long channels (from 3D-printing) and struts with smaller interconnected porosity (from partial sintering), resulting in overall porosities of ∼75% and low compressive stiffnesses of 1-1.6 GPa, similar to those of trabecular bone and in agreement with analytical and finite element modeling predictions. Diffusion of Nb into the NiTi particles from the bond regions results in a Ni-rich composition as the Nb replaces Ti atoms, leading to decreased martensite/austenite transformation temperatures. Adult human mesenchymal stem cells seeded on these micro-trusses showed excellent viability, proliferation, and extracellular matrix deposition over 14 days in culture. Near-equiatomic NiTi micro-trusses are attractive for biomedical applications such as stents, actuators, and bone implants because of their combination of biocompatibility, low compressive stiffness, high surface area, and shape-memory or superelasticity. Extrusion-based 3D-printing of NiTi powder-based inks into micro-trusses is feasible, but the subsequent sintering of the powders into dense struts is unachievable due to low diffusivity, large particle size, and low packing density of the NiTi powders. We present a solution, whereby Nb powders are added to the NiTi inks, thus forming during sintering a eutectic NiTi-Nb liquid phase which bonds the solid NiTi powders and improves densification of the struts. This study investigates the microstructure, porosity, phase transformation behavior, compressive stiffness, and cytocompatibility of these printed NiTi-Nb micro-trusses. Copyright © 2018 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Physical properties and microstructure study of 316L SS fabricated by metal injection moulding process

NASA Astrophysics Data System (ADS)

Dandang, Nur Aidah Nabihah; Harun, Wan Sharuzi Wan; Khalil, Nur Zalikha; Ismail, Muhammad Hussain; Ibrahim, Rosdi

2017-12-01

Metal injection moulding (MIM) has been practised to process alloy powders to become components with significant physical and mechanical properties. Dissimilar than other methods, MIM focuses on the production of high volume, a small, and complex shape of products. The performance of the compacts depends on the suitable sintering parameters that governs their strengths in the final phase which determines the excellent properties of the sintered compacts. Three different sintering temperatures were utilised; 1100, 1200, and 1300 °C with two different soaking times; 1 and 3 hours at 10 °C/min heating rate to study their effect on the physical properties and microstructure analysis of 316L SS alloy compacts. The shrinkage measurement, surface roughness, and density measurement had been conducted for physical properties study. Different sintering temperatures give an effect to the physical properties of the sintered compacts. The shrinkage measurement at 1300 °C and 3-hour sintering condition demonstrated the highest percentage reading which was 10.1 % compared to the lowest percentage reading of 6.4 % at 1100 °C and 1-hour sintering conditions. Whereas, the minimum percentage of density measurement can be found at sintering conditions of 1100 °C and 1-hour which is 83.9 % and the highest percentage is at 1300 °C and 3-hour sintering condition which is about 89.51 %. Therefore, it has been determined that there could be a significant relationship between sintering temperature and physical properties in which it can be found from the porosity of the compact based on the microstructure studies.

Temperature dependences of the electromechanical and electrocaloric properties of Ba(Zr,Ti)O3 and (Ba,Sr)TiO3 ceramics

NASA Astrophysics Data System (ADS)

Maiwa, Hiroshi

2017-10-01

The electrocaloric properties of Ba(Zr,Ti)O3 and (Ba,Sr)TiO3 ceramics (BZT and BST, respectively) were investigated by the indirect estimation and direct measurement of temperature-electric field (T-E) hysteresis loops. The measured T-E loops had shapes similar to those of the strain-electric field (s-E) loops. The measured temperature changes (ΔTs) at around 30 °C of the BZT ceramics sintered at 1450 °C and BST ceramics sintered at 1600 °C upon the release of the electric field from 30 kV/cm to 0 were 0.34 and 0.57 K, respectively. The temperature dependences of the electromechanical and electrocaloric properties were investigated. The BZT ceramics sintered at 1450 °C exhibited the largest electromechanical and electrocaloric properties at around 30 °C, which corresponds to the phase transition temperature. BST is more temperature dependent than BZT. BST ceramics sintered at 1600 °C exhibited the largest electromechanical and electrocaloric properties at around 29 °C, which is about 10 °C higher than the phase transition temperature.

Microstructures and Hardness of the High Chromium Oxide Dispersion Strengthened Alloy Fe-25Cr-Y2O3Sintered by the Arc Plasma Sintering (APS)

NASA Astrophysics Data System (ADS)

Bandriyana; Dimyati, Arbi; Sujatno, Agus; Salam, Rohmad; Sumaryo; Untoro, Pudji; Suharno, Bambang

2018-03-01

High chromium ODS alloy has been developed for application as structural material in high temperature nuclear reactor. In the present study, Fe-25Cr-Y2O3 with dispersed 0.5 wt.% Ytria (Y2O3) were synthesized and characterized by means of various techniques as a function of milling time 1, 2 and 3 hours. The alloy synthesis was carried out by the Mechanical Alloying (MA) process and subsequent sintering by means the new plasma technique using the APS apparatus. Scaning Electron Microscopy (SEM) and X-ray diffraction (XRD) were conducted for morphology and phase analysis. Evaluation of the mechanical properties was studied based on the Vickers hardness measurement. SEM examination revealed that the sample after sintering by APS method at different milling duration exhibited some particle aglomeration and homogenized oxide dispersion that obviously strengthened the alloy. The XRD test, however, proved the formation of the main phase Fe-Cr. The alloy showed exceptionally high hardness of 193 VHR which is mainly due to the grain refining that increase by the increasing of the milling time.

Powder metallurgy preparation of Mg-Ca alloy for biodegradable implant application

NASA Astrophysics Data System (ADS)

Annur, D.; Suhardi, A.; Amal, M. I.; Anwar, M. S.; Kartika, I.

2017-04-01

Magnesium and its alloys is a promising candidate for implant application especially due to its biodegradability. In this study, Mg-7Ca alloys (in weight %) were processed by powder metallurgy from pure magnesium powder and calcium granule. Milling process was done in a shaker mill using stainless steel balls in various milling time (3, 5, and 8 hours) followed by compaction and sintering process. Different sintering temperatures were used (450°C and 550°C) to examine the effect of sintering temperature on mechanical properties and corrosion resistance. Microstructure evaluation was characterized by X-ray diffraction, scanning electron microscope and energy dispersive X-ray spectroscopy. Mechanical properties and corrosion behavior were examined through hardness testing and electrochemical testing in Hank’s solution (simulation body fluid). In this report, a prolonged milling time reduced particle size and later affected mechanical properties of Mg alloy. Meanwhile, the phase analysis showed that α Mg, Mg2Ca, MgO phases were formed after the sintering process. Further, this study showed that Mg-Ca alloy with different powder metallurgy process would have different corrosion rate although there were no difference of Ca content in the alloy.

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.

New nano-sized Al2O3-BN coating 3Y-TZP ceramic composites for CAD/CAM-produced all-ceramic dental restorations. Part I. Fabrication of powders.

PubMed

Yang, Se Fei; Yang, Li Qiang; Jin, Zhi Hao; Guo, Tian Wen; Wang, Lei; Liu, Hong Chen

2009-06-01

Partially sintered 3 mol % yttria-stabilized tetragonal zirconium dioxide (ZrO(2), zirconia) polycrystal (3Y-TZP) ceramics are used in dental posterior restorations with computer-aided design-computer-aided manufacturing (CAD/CAM) techniques. High strength is acquired after sintering, but shape distortion of preshaped compacts during their sintering is inevitable. The aim of this study is to fabricate new machinable ceramic composites with strong mechanical properties that are fit for all-ceramic dental restorations. Aluminum oxide (Al(2)O(3))-coated 3Y-TZP powders were first prepared by the heterogeneous precipitation method starting with 3Y-TZP, Al(NO(3))(3) . 9H(2)O, and ammonia, then amorphous boron nitride (BN) was produced and the as-received composite powders were coated via in situ reaction with boric acid and urea. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) were used to analyze the status of Al(2)O(3)-BN on the surface of the 3Y-TZP particles. TEM micrographs show an abundance of Al(2)O(3) particles and amorphous BN appearing uniformly on the surface of the 3Y-TZP particles after the coating process. The size of the Al(2)O(3) particles is about 20 nm. The XRD pattern shows clearly the peak of amorphous BN among the peaks of ZrO(2).

Crystallization studies and dielectric properties of (Ba0.7Sr0.3)TiO3 in bariumaluminosilicate glass

NASA Astrophysics Data System (ADS)

Divya, P. V.; Vignesh, G.; Kumar, V.

2007-12-01

Ferroelectric glass-ceramics with a basic composition (1 - y)(Ba0.70Sr0.30)TiO3 : y(BaO : Al2O3 : 2SiO2) have been synthesized by the sol-gel method. The major crystalline phase is the perovskite. The crystallization of the ferroelectric phase in the glass matrix have been studied using differential thermal analysis and x-ray diffraction and the kinetic parameters characterizing the crystallization have been determined using an Arrhenius model. Glass contents <= 5 mol% promoted liquid phase sintering, which reduced the sintering temperature to 1250 °C. The dielectric permittivity of the glass-ceramic samples decreased and the ferroelectric-paraelectric phase transition became more diffuse with increasing glass content. The dielectric connectivity of the ferroelectric phase in the composite have also been investigated and are reported.

Y-TZP zirconia regeneration firing: Microstructural and crystallographic changes after grinding.

PubMed

Ryan, Daniel Patrick Obelenis; Fais, Laiza Maria Grassi; Antonio, Selma Gutierrez; Hatanaka, Gabriel Rodrigues; Candido, Lucas Miguel; Pinelli, Ligia Antunes Pereira

2017-07-26

This study evaluated microstructural and crystallographic phase changes after grinding (G) and regeneration firing/anneling (R) of Y-TZP ceramics. Thirty five bars (Lava TM and Ice Zirkon) were divided: Y-TZP pre-sintered, control (C), regeneration firing (R), dry grinding (DG), dry grinding+regeneration firing (DGR), wet grinding (WG) and wet grinding+regeneration firing (WGR). Grinding was conducted using a diamond bur and annealing at 1,000°C. The microstructure was analyzed by SEM and the crystalline phases by X-ray diffraction (XRD). XRD showed that pre-sintered specimens contained tetragonal and monoclinic phases, while groups C and R showed tetragonal, cubic and monoclinic phases. After grinding, the cubic phase was eliminated in all groups. Annealing (DGR and WGR) resulted in only tetragonal phase. SEM showed semi-circular cracks after grinding and homogenization of particles after annealing. After grinding, surfaces show tetragonal and monoclinic phases and R can be assumed to be necessary prior to porcelain layering when grinding is performed.

Final Report on Initial Samples Supplied by LLNL for Task 3.3 Binder Burnout and Sintering Schedule Optimisation

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

Walls, P

Sixteen of the twenty-one samples have been investigated using the scanning laser dilatometer. This includes all three types of samples with different preparation routes and organic content. Cracks were observed in all samples, even those only heated to 300 C. It was concluded that the cracking was occurring in the early part of the heat treatment before the samples reached 300 C. Increase in the rate of dilation of the samples occurred above 170 C which coincided with the decomposition of the binder/wax additives as determined by differential thermal analysis. A comparison was made with SYNROC C material (Powder Runmore » 143), samples of which had been CIPed and green machined to a similar diameter and thickness as the 089mm SRTC pucks. These samples contained neither binder nor other organic processing aids and had been kept in the same desiccator as the SRTC samples. The CIPed Synroc C samples sintered to high density with zero cracks. As the cracks made up only a small contribution to the change in diameter of the sample compared to the sintering shrinkage, useful information could still be gained from the runs. The sintering curves showed that there was much greater shrinkage of the Type III samples containing only the 5% PEG binder compared to the Type I which contained polyolefin wax as processing aid. Slight changes in gradient of the sintering curve were observed, however, due to the masking effect of the cracking, full analysis of the sintering kinetics cannot be conducted. Even heating the samples to 300 C at 1.0 or 0.5 C/min could not prevent crack formation. This indicated that heating rate was not the critical parameter causing cracking of the samples. Sectioning of green bodies revealed the inhomogeneous nature of the binder/lubricant distribution in the samples. Increased homogeneity would reduce the amount of binder/lubricant required, which should in turn, reduce the degree of cracking observed during heating to the binder burnout temperature. A combination of: (1) use of a higher forming pressure, (2) reduction of organics content, (3) improvement in the distribution of the organic wax and binder components throughout the green body, could possibly alleviate cracking. Ultrasonic emulsification of the binder and wax with a small quantity of water prior to adding to the ball or attrition mill is advised to ensure more even distribution of the wax/binder system. This would also reduce the proportion of organic additives required. The binder burnout stage of the operation must first be optimized (i.e. production of pucks with no cracks) prior to optimization of the sintering stage.« less

Method for preparing configured silicon carbide whisker-reinforced alumina ceramic articles

DOEpatents

Tiegs, Terry N.

1987-01-01

A ceramic article of alumina reinforced with silicon carbide whiskers suitable for the fabrication into articles of complex geometry are provided by pressureless sintering and hot isostatic pressing steps. In accordance with the method of the invention a mixture of 5 to 10 vol. % silicon carbide whiskers 0.5 to 5 wt. % of a sintering aid such as yttria and the balance alumina powders is ball-milled and pressureless sintered in the desired configuration in the desired configuration an inert atmosphere at a temperature of about 1800.degree. C. to provide a self-supporting configured composite of a density of at least about 94% theoretical density. The composite is then hot isostatically pressed at a temperature and pressure adequate to provide configured articles of at least about 98% of theoretical density which is sufficient to provide the article with sufficient strength and fracture toughness for use in most structural applications such as gas turbine blades, cylinders, and other components of advanced heat engines.

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.

On the Mechanism of Microwave Flash Sintering of Ceramics

PubMed Central

Bykov, Yury V.; Egorov, Sergei V.; Eremeev, Anatoly G.; Kholoptsev, Vladislav V.; Plotnikov, Ivan V.; Rybakov, Kirill I.; Sorokin, Andrei A.

2016-01-01

The results of a study of ultra-rapid (flash) sintering of oxide ceramic materials under microwave heating with high absorbed power per unit volume of material (10–500 W/cm3) are presented. Ceramic samples of various compositions—Al2O3; Y2O3; MgAl2O4; and Yb(LaO)2O3—were sintered using a 24 GHz gyrotron system to a density above 0.98–0.99 of the theoretical value in 0.5–5 min without isothermal hold. An analysis of the experimental data (microwave power; heating and cooling rates) along with microstructure characterization provided an insight into the mechanism of flash sintering. Flash sintering occurs when the processing conditions—including the temperature of the sample; the properties of thermal insulation; and the intensity of microwave radiation—facilitate the development of thermal runaway due to an Arrhenius-type dependency of the material’s effective conductivity on temperature. The proper control over the thermal runaway effect is provided by fast regulation of the microwave power. The elevated concentration of defects and impurities in the boundary regions of the grains leads to localized preferential absorption of microwave radiation and results in grain boundary softening/pre-melting. The rapid densification of the granular medium with a reduced viscosity of the grain boundary phase occurs via rotation and sliding of the grains which accommodate their shape due to fast diffusion mass transport through the (quasi-)liquid phase. The same mechanism based on a thermal runaway under volumetric heating can be relevant for the effect of flash sintering of various oxide ceramics under a dc/ac voltage applied to the sample. PMID:28773807

Gas-phase and particle-phase PCDD/F congener distributions in the flue gas from an iron ore sintering plant.

PubMed

Liu, Xiaolong; Ye, Meng; Wang, Xue; Liu, Wen; Zhu, Tingyu

2017-04-01

The activated carbon injection-circulating fluidized bed (ACI-CFB)-bag filter coupling technique was studied in an iron ore sintering plant. For comparison, the removal efficiencies under the conditions without or with ACI technology were both evaluated. It was found that the polychlorinated dibenzo-p-dioxins and dibenzofuran (PCDD/F) removal efficiency for total international toxic equivalence quantity (I-TEQ) concentration was improved from 91.61% to 97.36% when ACI was employed, revealing that ACI was very conducive to further controlling the PCDD/F emissions. Detailed congener distributions of PCDD/Fs in the gas-phase and particle-phase of the Inlet and Outlet samples were determined. Additionally, the PCDD/F distribution for the Fly ash-with ACI sample of was also studied. Copyright © 2016. Published by Elsevier B.V.

Electrochemical corrosion behavior, microstructure and magnetic properties of sintered Nd-Fe-B permanent magnet doped by CuZn5 powders

NASA Astrophysics Data System (ADS)

Liu, W. Q.; Wang, Z.; Sun, C.; Yue, M.; Liu, Y. Q.; Zhang, D. T.; Zhang, J. X.

2014-05-01

Nd-Fe-B permanent magnets with a small amount of CuZn5 powders doping were prepared by conventional sintered method. The effects of CuZn5 contents on magnetic properties and microstructure, electrochemical corrosion resistance of sintered Nd-Fe-B magnets were systematically studied. The results show that the magnetic properties of magnets do not have a significant variation by CuZn5 powders doping; the coercivity of magnets rises gradually, while the remanence of the magnets decreases a little with increasing of the CuZn5 amount. The CuZn5 doped magnets have more positive corrosion potential, Ecorr, and much lower corrosion current density, icorr, than the magnets without CuZn5 doping, indicating CuZn5 doping could improve the corrosion resistance. Both Zn and Cu enrich mainly into the Nd-rich phase, fully improve the wettability between the Nd-rich phase and the Nd2Fe14B phase, and repair the defects of the main phase, so the coercivity of magnets doped with CuZn5 powders rises. Such microstructure modification effectively restrains the aggressive inter-granular corrosion. As a result, the CuZn5 doped magnet possesses excellent corrosion resistance in NaCl electrolyte.

New ZrO2/Al2O3 Nanocomposite Fabricated from Hybrid Nanoparticles Prepared by CO2 Laser Co-Vaporization

PubMed Central

Bartolomé, José F.; Smirnov, Anton; Kurland, Heinz-Dieter; Grabow, Janet; Müller, Frank A.

2016-01-01

Alumina toughened zirconia (ATZ) and zirconia toughened alumina (ZTA) are currently the materials of choice to meet the need for tough, strong, and bioinert ceramics for medical devices. However, the mechanical properties of ZrO2/Al2O3 dispersion ceramics could be considerably increased by reducing the corresponding grain sizes and by improving the homogeneity of the phase dispersion. Here, we prepare nanoparticles with an intraparticular phase distribution of Zr(1−x)AlxO(2−x/2) and (γ-, δ-)Al2O3 by the simultaneous gas phase condensation of laser co-vaporized zirconia and alumina raw powders. During subsequent spark plasma sintering the zirconia defect structures and transition alumina phases transform to a homogeneously distributed dispersion of tetragonal ZrO2 (52.4 vol%) and α-Al2O3 (47.6 vol%). Ceramics sintered by spark plasma sintering are completely dense with average grain sizes in the range around 250 nm. Outstanding mechanical properties (flexural strength σf = 1500 MPa, fracture toughness KIc = 6.8 MPa m1/2) together with a high resistance against low temperature degradation make these materials promising candidates for next generation bioceramics in total hip replacements and for dental implants. PMID:26846310

New ZrO2/Al2O3 Nanocomposite Fabricated from Hybrid Nanoparticles Prepared by CO2 Laser Co-Vaporization

NASA Astrophysics Data System (ADS)

Bartolomé, José F.; Smirnov, Anton; Kurland, Heinz-Dieter; Grabow, Janet; Müller, Frank A.

2016-02-01

Alumina toughened zirconia (ATZ) and zirconia toughened alumina (ZTA) are currently the materials of choice to meet the need for tough, strong, and bioinert ceramics for medical devices. However, the mechanical properties of ZrO2/Al2O3 dispersion ceramics could be considerably increased by reducing the corresponding grain sizes and by improving the homogeneity of the phase dispersion. Here, we prepare nanoparticles with an intraparticular phase distribution of Zr(1-x)AlxO(2-x/2) and (γ-, δ-)Al2O3 by the simultaneous gas phase condensation of laser co-vaporized zirconia and alumina raw powders. During subsequent spark plasma sintering the zirconia defect structures and transition alumina phases transform to a homogeneously distributed dispersion of tetragonal ZrO2 (52.4 vol%) and α-Al2O3 (47.6 vol%). Ceramics sintered by spark plasma sintering are completely dense with average grain sizes in the range around 250 nm. Outstanding mechanical properties (flexural strength σf = 1500 MPa, fracture toughness KIc = 6.8 MPa m1/2) together with a high resistance against low temperature degradation make these materials promising candidates for next generation bioceramics in total hip replacements and for dental implants.

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.

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

Effects of High-Pressure High-Temperature Sintering on the Band Gap and Thermoelectric Properties of PbSe

NASA Astrophysics Data System (ADS)

Chen, Bo; Li, Yi; Sun, Zhen-Ya

2018-06-01

In this study, PbSe bulk samples were prepared by a high-pressure high-temperature (HPHT) sintering technique, and the phase compositions, band gaps and thermoelectric properties of the samples were systematically investigated. The sintering pressure exerts a significant influence on the preferential orientation, band gap and thermoelectric properties of PbSe. With increasing pressure, the preferential orientation decreases, mainly due to the decreased crystallinity, while the band gap first decreases and then increases. The electrical conductivity and power factor decrease gradually with increasing pressure, mainly attributed to the decreased carrier concentration and mobility. Consequently, the sample prepared by 2 GPa shows the highest thermoelectric figure-of-merit, ZT, of 0.55 at ˜ 475 K. The ZT of the HPHT-sintered PbSe could be further improved by properly doping or optimizing the HPHT parameters. This study further demonstrates that the sintering pressure could be another degree of freedom to manipulate the band structure and thermoelectric properties of materials.

Effects of sintering atmosphere and temperature on structural and magnetic properties of Ni-Cu-Zn ferrite nano-particles: Magnetic enhancement by a reducing atmosphere

NASA Astrophysics Data System (ADS)

Gholizadeh, Ahmad; Jafari, Elahe

2017-01-01

In this work, effects of sintering atmosphere and temperature on structural and magnetic properties of Ni0.3Cu0.2Zn0.5Fe2O4 nanoparticles prepared by citrate precursor method have been studied. The structural characterization of the samples by X-ray powder diffraction and FT-IR spectroscopy is evidence for formation of a cubic structure with no presence of impurity phase. Calculated values of crystallite size and unit cell parameter show an increase with sintering temperature under different atmospheres. Variation of saturation magnetization with sintering temperature and atmosphere can be attributed to change of three factors: magnetic core size, inversion parameter and the change of Fe3+-ion concentration due to the presence of Fe4+ and Fe2+ ions. The saturation magnetization gradually grows with sintering temperature due to increase of magnetic core size and a maximum 63 emu/g was achieved at 600 °C under carbon monoxide-ambient atmosphere.

Effect of Spark-Plasma-Sintering Conditions on Tensile Properties of Aluminum Matrix Composites Reinforced with Multiwalled Carbon Nanotubes (MWCNTs)

NASA Astrophysics Data System (ADS)

Chen, B.; Imai, H.; Umeda, J.; Takahashi, M.; Kondoh, K.

2017-04-01

In this study, aluminum (Al) matrix composites containing 2 wt.% multiwalled carbon nanotubes (CNTs) were fabricated by powder metallurgy using high-energy ball milling (HEBM), spark plasma sintering (SPS), and subsequent hot extrusion. The effect of SPS conditions on the tensile properties of CNT/Al composites was investigated. The results showed that composites with well-dispersed CNTs and nearly full-density CNT/Al can be obtained. During HEBM, CNTs were shortened, inserted into welded Al powder particles, bonded to Al, and still stable without CNT-Al reaction. After consolidation, Al4C3 phases formed in composites under different sintering conditions. With the increase of sintering temperature and holding time, the strength decreased. Conversely, the ductility and toughness noticeably increased. As a result, a good balance between strength (367 MPa in ultimate tensile strength) and ductility (13% in elongation) was achieved in the as-extruded CNT/Al composite sintered at 630°C with a holding time of 300 min.

Sintering of polydisperse viscous droplets

NASA Astrophysics Data System (ADS)

Wadsworth, Fabian B.; Vasseur, Jérémie; Llewellin, Edward W.; Dingwell, Donald B.

2017-03-01

Sintering—or coalescence—of compacts of viscous droplets is driven by the interfacial tension between the droplets and the interstitial gas phase. The process, which occurs in a range of industrial and natural settings, such as the manufacture of ceramics and the welding of volcanic ash, causes the compact to densify, to become stronger, and to become less permeable. We investigate the role of droplet polydispersivity in sintering dynamics by conducting experiments in which populations of glass spheres with different size distributions are heated to temperatures above the glass transition interval. We quantify the progress of sintering by tracking changes in porosity with time. The sintering dynamics is modeled by treating the system as a random distribution of interstitial gas bubbles shrinking under the action of interfacial tension only. We identify the scaling between the polydispersivity of the initial droplets and the dynamics of bulk densification. The framework that we develop allows the sintering dynamics of arbitrary polydisperse populations of droplets to be predicted if the initial droplet (or particle) size distribution is known.

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.

The influence of co-sintering Bi2O3 on Yb0.2Ce0.8O2-δ ceramic SOFC

NASA Astrophysics Data System (ADS)

Budiana, B.; Suasmoro, S.

2017-01-01

Ceramic Yb-doped CeO2 were prepared through two ways. First, sintering of mixed 20 mol % Yb2O3 and 80 mol % CeO2 at 1350 °C for 20 h and second sintering of mixed 96 mol % calcined Yb-doped CeO2 with 4 mol % Bi2O3 as a co-sintering agent at 1100 °C for 8h. Phase identification revealed that for the first sample was a cubic phase (a=5,3939Å) while the second sample showed three phases, CeO2 (cubic a=5,4254Å), YbxCe1-xO2-δ (cubic a=5,3980Å) and Bi5Yb3O12 (cubic a=10,5343Å). Cole-cole plot of impedance revealed 3 semicircles as marked of grain, grain boundary and electrode responses for B1 while for B2 showed two semicircles as marked of grain, grain boundary+electrode responses. Plot of log (σt) versus 1/T for both samples possed 2 activation energy regime, for the Sample B1 at T>650 °C Ea grain =1,01±0,04 eV and T<650 °C Ea grain =0,76±0,06 eV while for the sample B2 at T>650 °C, Ea grain =0,99±0,03 eV and T<650 °C Ea grain=0,70±0,09 eV.

Sintering effects on dielectric properties of Zn-doped CaCu3Ti4O12 ceramic synthesized by modified sol-gel route

NASA Astrophysics Data System (ADS)

Singh, Laxman; Rai, U. S.; Rai, Alok Kumar; Mandal, K. D.

2013-01-01

CaCu2.90Zn0.10Ti4O12 ceramic was synthesized by a novel semi-wet route and calcined at 800°C in air for 8 h. The obtained powder was divided into three parts and sintered in air at 950°C for 6 h, 8 h, and 12 h, separately. XRD results confirmed the single phase formation of all the sintered samples with similar cubic structure of CaCu3Ti4O12 (CCTO). Scanning electron micrographs of the CaCu2.9Zn0.1Ti4O12 ceramic sintered for 6 h shows bimodal grain size distribution. Increasing the sintering time significantly promotes the grain growth and microstructural densification. The sintering duration was found to have tremendous influence on microstructure and dielectric properties of CaCu2.90Zn0.10Ti4O12 ceramic. The CaCu2.9Zn0.1Ti4O12 ceramic sintered for 12 h exhibited high dielectric constant ɛ r ˜ 5971 at 1 kHz and room temperature. It is found that ɛ r is independent at high frequency and weakly dependent on temperature.

Effects of sintering temperature on properties of toroid cores using NiZnCu ferrites for power applications at >1 MHz

NASA Astrophysics Data System (ADS)

Liu, Junchang; Mei, Yunhui; Liu, Wen; Li, Xin; Hou, Feng; Lu, Guo-Quan

2018-05-01

The microstructures, magnetic and electronic performance of NiZnCu ferrites have been investigated at temperature from 850 °C to 1000 °C. X-ray diffraction (XRD) patterns showed that only single phase with spinel structure existed. Scanning electron microscopy (SEM) results showed that grain size increased with enhancement of sintering temperature and the most homogeneous, compact microstructure was obtained at 950 °C. Magnetic properties measurements revealed that both complex permeability and saturation magnetization increased with increasing of sintering temperature. The initial permeability was approximately linear within the scope of 850-1000 °C as well as the resonance frequency decreased from 70 MHz to 30 MHz. Power loss density tests demonstrated that the core sintered at 950 °C instead of the one sintered at 1000 °C had the lower power loss density at both 5 mT and 10 mT and the higher inductance under a certain exciting direct current at 1 MHz. Also the inductance of the sample sintered at the higher temperature dropped faster than that at the lower temperature. The results showed that the core sintered at 950 °C had better electrical performance and was suitable for wide usage.

Microstructure evaluation for Dy-free Nd-Fe-B sintered magnets with high coercivity

NASA Astrophysics Data System (ADS)

Goto, R.; Matsuura, M.; Sugimoto, S.; Tezuka, N.; Une, Y.; Sagawa, M.

2012-04-01

Nd-Fe-B sintered magnets are used for motors of hybrid or electric vehicles due to their high energy products. Dy is added to Nd-Fe-B sintered magnets to work in a high temperature environment. Although the addition of Dy decreases the magnetization of Nd-Fe-B magnets, it increases coercivity; a decrease in the amount of Dy is strongly required. Recently, Nd-Fe-B sintered magnets with a grain size of 1 μm achieved high coercivity of ˜20 kOe without the addition of Dy or other heavy rare earth elements. In this paper, the microstructure of their magnets was observed and compared to magnets with a grain size of ˜3 μm. The coercivity of magnets consisting of larger particles was 17 kOe. Microstructures were observed by the scanning electron microscope and the shapes of grains and the distribution of the Nd-rich phase were evaluated. The observation was promoted in two directions. One direction is the plane perpendicular to the magnetically aligned direction (c plane side) and the other is the side parallel to the magnetically aligned direction (c axis side). For magnets consisting of smaller particles, the shapes of grains are isotropic for the c plane side and elongated for the c axis side. The angle of minor axis prefers to be parallel to magnetically aligned direction. The distribution of the Nd-rich phase for magnets was also evaluated for both magnets. The distribution of the Nd-rich phase at triple junctions for the magnets with smaller particles becomes homogeneous compared to that for magnets with larger particles. It is considered that Dy-free magnets with high coercivity were realized by the achievement of homogeneous distribution of Nd-rich phase besides decreasing grain size.

[Raman studies of nanocrystalline BaTiO3 ceramics].

PubMed

Xiao, Chang-jiang; Jin, Chang-qing; Wang, Xiao-hui

2008-12-01

High pressure can significantly increase the densification. Further, during the high pressure assisted sintering, the nucleation rate is increased due to reduced energy barrier and the growth rate is suppressed due to the decreased diffusivity. Thus high pressure enables the specimen to be fabricated with relatively lower temperature and shorter sintering period that assures to obtain dense nanocrystalline ceramics. Dense nanocrystalline BaTiO3 ceramics with uniform grain sizes of 60 and 30 nm, respectively, were obtained by pressure assisted sintering. The crystal structure and phase transitions were investigated by Raman scattering at temperatures ranging from -190 to 200 degrees C. The Raman results indicated that the evolution of Raman spectrum with grain size is characterized by an intensity decrease, a broadening of the line width, a frequency shift, and the disappearance of the Raman mode. With increasing temperature, similar to 3 mm BaTiO3 normal ceramics, the successive phase transitions from rhombohedral to orthorhombic, orthorhombic to tetragonal, and tetragonal to cubic were also observed in nanocrystalline BaTiO3 ceramics. In addition, when particle size is reduced to the nanoscale, one will find some unusual physical properties in nanocrystalline ceramics, compared with those of coarse-grained BaTiO3 ceramics. The different coexistences of multiphase were found at different temperature. Especially, the ferroelectric tetragonal and orthorhombic phase can coexist at room temperature in nanocrystalline BaTiO3 ceramics. The phenomenon can be explained by the internal stress. The coexistences of different ferroelectric phases at room temperature indicate that the critical grain size for the disappearance of ferroelectricity in nanocrystalline BaTiO3 ceramics fabricated by pressure assisted sintering is below 30 nm.

Vanadium dioxide-based materials for potential thermal switching applications

NASA Astrophysics Data System (ADS)

Jeong, Minyoung

One of the materials able to exhibit a transition from insulators to metals (IMT materials) is vanadium dioxide (VO2). Through IMT, VO2 shows a drop of resistivity of five orders of magnitude at a picosecond timescale. In this work, the feasibility of using VO2 as an efficient thermal switching device is discussed. Several synthesis methods (sol-gel, hot press and spark plasma sintering) were attempted to obtain VO2 sample in pellet form. From the X-ray diffraction results, it was found that spark plasma sintering (SPS) yielded the highest phase purity. Several sintering parameters such as temperature or sintering time were tested to determine the optimal sintering conditions. For better thermal switching behavior, high-energy ball milling was used to reduce lattice thermal conductivity (klat.) in the insulator phase. Ball-milling time was varied from 30 minutes to 2 hours. It was found that with increasing milling time, the k lat. was reduced. Thus, it was demonstrated that thermal switching behavior was most efficient with 2 hour-milling. To improve electronic thermal conductivity ( kelec.) in the metallic state, nano-sized copper particles were added to the VO2 system with a subtle amount variation ranging from 3at % to 5 at%. Results show that a composite with 5 at% Cu (copper) addition exhibited the largest increase in thermal conductivity ( k) in the metallic state. In addition to this, a basic mechanism behind IMT and some of the exemplary IMT-based applications were introduced.

Development of Economical Improved Thick Film Solar Cell Contact

NASA Technical Reports Server (NTRS)

Ross, B.

1979-01-01

Materials were surveyed to provide candidates for an all metal electrode paste system. These consisted of a major constituent metal powder, a low melting metal powder suitable for a liquid phase sintering medium, and a powder material suitable as an etchant for silicon dioxide at sintering temperatures. By means of thermal gravimetric analysis a suitable binder was identified for low temperature fired inks.

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.

Sintering Characteristics of Multilayered Thermal Barrier Coatings Under Thermal Gradient and Isothermal High Temperature Annealing Conditions

NASA Technical Reports Server (NTRS)

Rai, Amarendra K.; Schmitt, Michael P.; Bhattacharya, Rabi; Zhu, Dongming; Wolfe, Douglas E.

2014-01-01

Pyrochlore oxides have most of the relevant attributes for use as next generation thermal barrier coatings such as phase stability, low sintering kinetics and low thermal conductivity. One of the issues with the pyrochlore oxides is their lower toughness and therefore higher erosion rate compared to the current state-of-the-art TBC material, yttria (6 to 8 wt%) stabilized zirconia (YSZ). In this work, sintering characteristics were investigated for novel multilayered coating consisted of alternating layers of pyrochlore oxide viz Gd2Zr2O7 and t' low k (rare earth oxide doped YSZ). Thermal gradient and isothermal high temperature (1316 C) annealing conditions were used to investigate sintering and cracking in these coatings. The results are then compared with that of relevant monolayered coatings and a baseline YSZ coating.

Study of sintering temperature on the structure of silicon carbide membrane

NASA Astrophysics Data System (ADS)

Sadighzadeh, A.; Mashayekhan, Sh.; Nedaie, B.; Ghorashi, A. H.

2014-09-01

Study of the microstructure of silicon carbide (SiC) membrane as a function of sintering temperature and the percentage amount of additive kaolin is the outcome of the experimental fabrications presented in this paper. The SEM micrographs are used to investigate the impact of above parameters on the porosity of membrane. The experimental results show that the rise in the temperature causes more sintering of powder particles, growing granules, augmentation of the number of pores and consequently increasing the total porosity of membrane. Using XRD analyses, it is found that SiC amorphous phase is highly sensitive to the temperature and its crystallization physically grows with temperature increase.

Preparation and flash sintering of MgTiO3 nanopowders obtained by the polyacrylamide gel method

NASA Astrophysics Data System (ADS)

Su, Xinghua; Bai, Ge; Zhang, Jing; Zhou, Jie; Jia, Yongjie

2018-06-01

Using a polyacrylamide gel method, phase pure and well-dispersed MgTiO3 nanopowders were prepared at 800 °C for 2 h. It was found that a high mole ratio of monomers to precursors resulted in low formation temperature of MgTiO3, due to the highly mixing homogeneity and smaller particle sizes of precursors. Sintering behaviors of MgTiO3 nanopowders under DC electric field from 500 to 800 V/cm were investigated. Nearly full dense MgTiO3 ceramics can be prepared in 30 s. An abrupt and simultaneous increase in current density and power dissipation were observed in sintering process, which are characteristics of flash sintering. The power dissipation for the flash sintering was found to be 82 mW/mm3. The densities and average grain sizes of samples increase with the increase of the electrical field strength. It was suggested that Joule heating was the main mechanism of flash sintering of MgTiO3 ceramics. Our work provides a useful route for the fabrication of dense MgTiO3 ceramics at low temperature in short time.

Mechanical behaviour of pressed and sintered CP Ti and Ti-6Al-7Nb alloy obtained from master alloy addition powder.

PubMed

Bolzoni, L; Weissgaerber, T; Kieback, B; Ruiz-Navas, E M; Gordo, E

2013-04-01

The Ti-6Al-7Nb alloy was obtained using the blending elemental approach with a master alloy and elemental titanium powders. Both the elemental titanium and the Ti-6Al-7Nb powders were characterised using X-ray diffraction, differential thermal analysis and dilatometry. The powders were processed using the conventional powder metallurgy route that includes uniaxial pressing and sintering. The trend of the relative density with the sintering temperature and the microstructural evolution of the materials sintered at different temperatures were analysed using scanning electron microscopy and X-ray diffraction. A minimum sintering temperature of 1200°C has to be used to ensure the homogenisation of the alloying elements and to obtain a pore structure composed of spherical pores. The sintered samples achieve relative density values that are typical for powder metallurgy titanium and no intermetallic phases were detected. Mechanical properties comparable to those specified for wrought Ti-6Al-7Nb medical devices are normally obtained. Therefore, the produced materials are promising candidates for load bearing applications as implant materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

Internal fit of three-unit fixed dental prostheses produced by computer-aided design/computer-aided manufacturing and the lost-wax metal casting technique assessed using the triple-scan protocol.

PubMed

Dahl, Bjørn E; Dahl, Jon E; Rønold, Hans J

2018-02-01

Suboptimal adaptation of fixed dental prostheses (FDPs) can lead to technical and biological complications. It is unclear if the computer-aided design/computer-aided manufacturing (CAD/CAM) technique improves adaptation of FDPs compared with FDPs made using the lost-wax and metal casting technique. Three-unit FDPs were manufactured by CAD/CAM based on digital impression of a typodont model. The FDPs were made from one of five materials: pre-sintered zirconium dioxide; hot isostatic pressed zirconium dioxide; lithium disilicate glass-ceramic; milled cobalt-chromium; and laser-sintered cobalt-chromium. The FDPs made using the lost-wax and metal casting technique were used as reference. The fit of the FDPs was analysed using the triple-scan method. The fit was evaluated for both single abutments and three-unit FDPs. The average cement space varied between 50 μm and 300 μm. Insignificant differences in internal fit were observed between the CAD/CAM-manufactured FDPs, and none of the FPDs had cement spaces that were statistically significantly different from those of the reference FDP. For all FDPs, the cement space at a marginal band 0.5-1.0 mm from the preparation margin was less than 100 μm. The milled cobalt-chromium FDP had the closest fit. The cement space of FDPs produced using the CAD/CAM technique was similar to that of FDPs produced using the conventional lost-wax and metal casting technique. © 2017 Eur J Oral Sci.

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.

Fully-Enclosed Ceramic Micro-burners Using Fugitive Phase and Powder-based Processing

NASA Astrophysics Data System (ADS)

Do, Truong; Shin, Changseop; Kwon, Patrick; Yeom, Junghoon

2016-08-01

Ceramic-based microchemical systems (μCSs) are more suitable for operation under harsh environments such as high temperature and corrosive reactants compared to the more conventional μCS materials such as silicon and polymers. With the recent renewed interests in chemical manufacturing and process intensification, simple, inexpensive, and reliable ceramic manufacturing technologies are needed. The main objective of this paper is to introduce a new powder-based fabrication framework, which is a one-pot, cost-effective, and versatile process for ceramic μCS components. The proposed approach employs the compaction of metal-oxide sub-micron powders with a graphite fugitive phase that is burned out to create internal cavities and microchannels before full sintering. Pure alumina powder has been used without any binder phase, enabling more precise dimensional control and less structure shrinkage upon sintering. The key process steps such as powder compaction, graphite burnout during partial sintering, machining in a conventional machine tool, and final densification have been studied to characterize the process. This near-full density ceramic structure with the combustion chamber and various internal channels was fabricated to be used as a micro-burner for gas sensing applications.

Fully-Enclosed Ceramic Micro-burners Using Fugitive Phase and Powder-based Processing

PubMed Central

Do, Truong; Shin, Changseop; Kwon, Patrick; Yeom, Junghoon

2016-01-01

Ceramic-based microchemical systems (μCSs) are more suitable for operation under harsh environments such as high temperature and corrosive reactants compared to the more conventional μCS materials such as silicon and polymers. With the recent renewed interests in chemical manufacturing and process intensification, simple, inexpensive, and reliable ceramic manufacturing technologies are needed. The main objective of this paper is to introduce a new powder-based fabrication framework, which is a one-pot, cost-effective, and versatile process for ceramic μCS components. The proposed approach employs the compaction of metal-oxide sub-micron powders with a graphite fugitive phase that is burned out to create internal cavities and microchannels before full sintering. Pure alumina powder has been used without any binder phase, enabling more precise dimensional control and less structure shrinkage upon sintering. The key process steps such as powder compaction, graphite burnout during partial sintering, machining in a conventional machine tool, and final densification have been studied to characterize the process. This near-full density ceramic structure with the combustion chamber and various internal channels was fabricated to be used as a micro-burner for gas sensing applications. PMID:27546059

Glass composite waste forms for iodine confined in bismuth-embedded SBA-15

NASA Astrophysics Data System (ADS)

Yang, Jae Hwan; Park, Hwan Seo; Ahn, Do-Hee; Yim, Man-Sung

2016-11-01

The aim of this study was to stabilize bismuth-embedded SBA-15 that captured iodine gas by fabrication of monolithic waste forms. The iodine containing waste was mixed with Bi2O3 (a stabilizing additive) and low-temperature sintering glass followed by pelletizing and the sintering process to produce glass composite materials. Iodine volatility during the sintering process was significantly affected by the ratio of Bi2O3 and the glass composition. It was confirmed that BiI3, the main iodine phase within bismuth-embedded SBA-15, was effectively transformed to the mixed phases of Bi5O7I and BiOI. The initial leaching rates of iodine from the glass composite waste forms ranged 10-3-10-2 g/m2 day, showing the stability of the iodine phases encapsulated by the glassy networks. It was also observed that common groundwater anions (e.g., chloride, carbonate, sulfite, and fluoride) elevated the iodine leaching rate by anion exchange reactions. The present results suggest that the glass composite waste form of bismuth-embedded SBA-15 could be a candidate material for stable storage of 129I.

Research on sintering behavior and microwave dielectric property of (Mg0.95Ca0.05)TiO3 ceramics for cross coupling filter

NASA Astrophysics Data System (ADS)

Luo, Chunya; Ma, Zhichao; Hu, Laisheng; Hu, Mingzhe; Huang, Xiaomin

2015-12-01

The microwave dielectric properties of 0.95%MgTiO3-0.05%CaTiO3 (abbreviated as 95MCT hereafter) ceramics have been studied for application in dielectric cross coupling filters. ZnO and Nb2O5 were selected as liquid sintering aids to lower the sintering temperature and enhance the Qf value of 95MCT and simultaneously we varied the mole ratio of ZnO : Nb2O5 to tune the microwave dielectric properties of 95MCT. When the ZnO : Nb2O5 mole ratio was 1.5 and the co-doping content was 0.25 wt.%, the optimal sintering temperature of 95MCT ceramic could be lowered from 1400∘C to 1320∘C and the Qf value could be improved by about 7.7%. The optimal microwave dielectric properties obtained under this condition were Qf = 72730 GHz (6.8 GHz), ɛr = 20.29 and τf = -6.84ppm/∘C, which demonstrated great potential usage in ceramic industry. High values of Qf ceramic were used to design the dielectric cross coupling filter. The dielectric filter measured at 2.35 GHz exhibited a 6.7% bandwidth (insert loss > -3 dB) of center frequency.

Spark plasma sintering of titanium aluminide intermetallics and its composites

NASA Astrophysics Data System (ADS)

Aldoshan, Abdelhakim Ahmed

Titanium aluminide intermetallics are a distinct class of engineering materials having unique properties over conventional titanium alloys. gamma-TiAl compound possesses competitive physical and mechanical properties at elevated temperature applications compared to Ni-based superalloys. gamma-TiAl composite materials exhibit high melting point, low density, high strength and excellent corrosion resistance. Spark plasma sintering (SPS) is one of the powder metallurgy techniques where powder mixture undergoes simultaneous application of uniaxial pressure and pulsed direct current. Unlike other sintering techniques such as hot iso-static pressing and hot pressing, SPS compacts the materials in shorter time (< 10 min) with a lower temperature and leads to highly dense products. Reactive synthesis of titanium aluminide intermetallics is carried out using SPS. Reactive sintering takes place between liquid aluminum and solid titanium. In this work, reactive sintering through SPS was used to fabricate fully densified gamma-TiAl and titanium aluminide composites starting from elemental powders at different sintering temperatures. It was observed that sintering temperature played significant role in the densification of titanium aluminide composites. gamma-TiAl was the predominate phase at different temperatures. The effect of increasing sintering temperature on microhardness, microstructure, yield strength and wear behavior of titanium aluminide was studied. Addition of graphene nanoplatelets to titanium aluminide matrix resulted in change in microhardness. In Ti-Al-graphene composites, a noticeable decrease in coefficient of friction was observed due to the influence of self-lubrication caused by graphene.

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.

Composite scaffolds for osteochondral repair obtained by combination of additive manufacturing, leaching processes and hMSC-CM functionalization.

PubMed

Díaz Lantada, Andrés; Alarcón Iniesta, Hernán; García-Ruíz, Josefa Predestinación

2016-02-01

Articular repair is a relevant and challenging area for the emerging fields of tissue engineering and biofabrication. The need of significant gradients of properties, for the promotion of osteochondral repair, has led to the development of several families of composite biomaterials and scaffolds, using different effective approaches, although a perfect solution has not yet been found. In this study we present the design, modeling, rapid manufacturing and in vitro testing of a composite scaffold aimed at osteochondral repair. The presented composite scaffold stands out for having a functional gradient of density and stiffness in the bony phase, obtained in titanium by means of computer-aided design combined with additive manufacture using selective laser sintering. The chondral phase is obtained by sugar leaching, using a PDMS matrix and sugar as porogen, and is joined to the bony phase during the polymerization of PDMS, therefore avoiding the use of supporting adhesives or additional intermediate layers. The mechanical performance of the construct is biomimetic and the stiffness values of the bony and chondral phases can be tuned to the desired applications, by means of controlled modifications of different parameters. A human mesenchymal stem cell (h-MSC) conditioned medium (CM) is used for improving scaffold response. Cell culture results provide relevant information regarding the viability of the composite scaffolds used. Copyright © 2015 Elsevier B.V. All rights reserved.

Rapid liquid phase sintered Mn doped BiFeO3 ceramics with enhanced polarization and weak magnetization

NASA Astrophysics Data System (ADS)

Kumar, Manoj; Yadav, K. L.

2007-12-01

Single-phase BiFe1-xMnxO3 multiferroic ceramics have been synthesized by rapid liquid phase sintering method to study the influence of Mn substitution on their crystal structure, dielectric, magnetic, and ferroelectric behaviors. From XRD analysis it is seen that Mn substitution does not affect the crystal structure of the BiFe1-xMnxO3 system. An enhancement in magnetization was observed for BiFe1-xMnxO3 ceramics. However, the ferooelectric hysteresis loops were not really saturated, we observed a spontaneous polarization of 10.23μC /cm2 under the applied field of 42kV/cm and remanent polarization of 3.99μC/cm2 for x =0.3 ceramic.

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.

Capillary equilibrium and sintering kinetics in dispersed media and catalysts

NASA Astrophysics Data System (ADS)

Delannay, Francis

2016-06-01

The evolution of an aggregate of particles embedded in a fluid phase, no matter whether a liquid, a vapor, or a mixture of both, is determined by the dependence of the equilibrium interface area on porosity volume fraction. In system with open porosity, this equilibrium can be analyzed using a model representing the particles as a collection of cones of revolution, the number of which is the average particle coordination number. The accuracy of the model has been assessed using in situ X-ray microtomography. The model makes possible the computation of the driving force for sintering, commonly called sintering stress. It allows the mapping of the domains of relative density, coordination number, and dihedral angle that bring about aggregate densification or expansion. The contribution of liquid/vapor interfaces is enlightened, as well as the dependence of the equilibrium fluid phase distribution on particle size. Applied to foams and emulsions, the model provides insight into the relationship between osmotic pressure and coordination. Interface-governed transport mechanisms are considered dominant in the macroscopic viscosity. Both sintering stress and viscosity parameters strongly depend on particle size. The capacity of modeling the simultaneous particle growth is thus essential. The analysis highlights the microstructural parameters and material properties needed for kinetics simulation.

[Development of computer aided forming techniques in manufacturing scaffolds for bone tissue engineering].

PubMed

Wei, Xuelei; Dong, Fuhui

2011-12-01

To review recent advance in the research and application of computer aided forming techniques for constructing bone tissue engineering scaffolds. The literature concerning computer aided forming techniques for constructing bone tissue engineering scaffolds in recent years was reviewed extensively and summarized. Several studies over last decade have focused on computer aided forming techniques for bone scaffold construction using various scaffold materials, which is based on computer aided design (CAD) and bone scaffold rapid prototyping (RP). CAD include medical CAD, STL, and reverse design. Reverse design can fully simulate normal bone tissue and could be very useful for the CAD. RP techniques include fused deposition modeling, three dimensional printing, selected laser sintering, three dimensional bioplotting, and low-temperature deposition manufacturing. These techniques provide a new way to construct bone tissue engineering scaffolds with complex internal structures. With rapid development of molding and forming techniques, computer aided forming techniques are expected to provide ideal bone tissue engineering scaffolds.

Transformation from insulating p-type to semiconducting n-type conduction in CaCu3Ti4O12-related Na(Cu5/2Ti1/2)Ti4O12 ceramics

NASA Astrophysics Data System (ADS)

Li, Ming; Sinclair, Derek C.

2013-07-01

A double doping mechanism of Na+ + 1/2 Ti4+ → Ca2+ + 1/2 Cu2+ on the general formula Ca1-xNax(Cu3-x/2Tix/2)Ti4O12 has been used to prepare a series of isostructural CaCu3Ti4O12 (CCTO)-type perovskites. A complete solid solution exists for 0 ≤ x ≤ 1 and all compositions exhibit incipient ferroelectric behaviour with higher than expected intrinsic relative permittivity. Although CCTO ceramics typically exhibit n-type semiconductivity (room temperature, RT, resistivity of ˜10-100 Ω cm), Na(Cu5/2Ti1/2)Ti4O12 (NCTO) ceramics sintered at 950 °C consist of two insulating bulk phases (RT resistivity > 1 GΩ cm), one p-type and the other n-type. With increasing sintering temperature/period, the p-type phase transforms into the n-type phase. During the transformation, the resistivity and activation energy for electrical conduction (Ea ˜ 1.0 eV) of the p-type phase remain unchanged, whereas the n-type phase becomes increasingly conductive with Ea decreasing from ˜ 0.71 to 0.11 eV with increasing sintering temperature. These changes are attributed to small variations in stoichiometry that occur during high temperature ceramic processing with oxygen-loss playing a crucial role.

Diamond grinding wheels production study with the use of the finite element method.

PubMed

Kundrák, J; Fedorovich, V; Markopoulos, A P; Pyzhov, I; Kryukova, N

2016-11-01

Research results on 3D modeling of the diamond grain and its bearing layer when sintering diamond grinding wheels are provided in this paper. The influence of the main characteristics of the wheel materials and the wheel production process, namely the quantity of metallic phase within diamond grain, coefficient of thermal expansion of the metallic phase, the modulus of elasticity of bond material and sintering temperature, on the internal stresses arising in grains is investigated. The results indicate that the stresses in the grains are higher in the areas around the metallic phase. Additionally, sintering temperature has the greatest impact on the stresses of the grain-metallic phase-bond system regardless of the type of the bond. Furthermore, by employing factorial design for the carried out finite element model, a mathematical model that reflects the impact of these factors on the deflected mode of the diamond grain-metallic phase-bond material system is obtained. The results of the analysis allow for the identification of optimal conditions for the efficient production of improved diamond grinding wheels. More specifically, the smallest stresses are observed when using the metal bond with modulus of elasticity 204 GPa, the quantity of metallic phase in diamond grain of not higher than 7% and coefficient of thermal expansion of 1.32 × 10 -5  1/K or lower. The results obtained from the proposed 3D model can lead to the increase in the diamond grains utilization and improve the overall efficiency of diamond grinding.

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.

Phosphorus as sintering activator in powder metallurgical steels: characterization of the distribution and its technological impact.

PubMed

Krecar, Dragan; Vassileva, Vassilka; Danninger, Herbert; Hutter, Herbert

2004-06-01

Powder metallurgy is a highly developed method of manufacturing reliable ferrous parts. The main processing steps in a powder metallurgical line are pressing and sintering. Sintering can be strongly enhanced by the formation of a liquid phase during the sintering process when using phosphorus as sintering activator. In this work the distribution (effect) of phosphorus was investigated by means of secondary ion mass spectrometry (SIMS) supported by Auger electron spectroscopy (AES) and electron probe micro analysis (EPMA). To verify the influence of the process conditions (phosphorus content, sintering atmosphere, time) on the mechanical properties, additional measurements of the microstructure (pore shape) and of impact energy were performed. Analysis of fracture surfaces was performed by means of scanning electron microscopy (SEM). The concentration of phosphorus differs in the samples from 0 to 1% (w/ w). Samples with higher phosphorus concentrations (1% (w/ w) and above) are also measurable by EPMA, whereas the distributions of P at technically relevant concentrations and the distribution of possible impurities are only detectable (visible) by means of SIMS. The influence of the sintering time on the phosphorus distribution will be demonstrated. In addition the grain boundary segregation of P was measured by AES at the surface of in-situ broken samples. It will be shown that the distribution of phosphorus depends also on the concentration of carbon in the samples.

A microcomputed tomography evaluation of the marginal fit of cobalt-chromium alloy copings fabricated by new manufacturing techniques and alloy systems.

PubMed

Kim, Eun-Ha; Lee, Du-Hyeong; Kwon, Sung-Min; Kwon, Tae-Yub

2017-03-01

Although new digital manufacturing techniques are attracting interest in dentistry, few studies have comprehensively investigated the marginal fit of fixed dental prostheses fabricated with such techniques. The purpose of this in vitro microcomputed tomography (μCT) study was to evaluate the marginal fit of cobalt-chromium (Co-Cr) alloy copings fabricated by casting and 3 different computer-aided design and computer-aided manufacturing (CAD-CAM)-based processing techniques and alloy systems. Single Co-Cr metal crowns were fabricated using 4 different manufacturing techniques: casting (control), milling, selective laser melting, and milling/sintering. Two different commercial alloy systems were used for each fabrication technique (a total of 8 groups; n=10 for each group). The marginal discrepancy and absolute marginal discrepancy of the crowns were determined with μCT. For each specimen, the values were determined from 4 different regions (sagittal buccal, sagittal lingual, coronal mesial, and coronal distal) by using imaging software and recorded as the average of the 4 readings. For each parameter, the results were statistically compared with 2-way analysis of variance and appropriate post hoc analysis (using Tukey or Student t test) (α=.05). The milling and selective laser melting groups showed significantly larger marginal discrepancies than the control groups (70.4 ±12.0 and 65.3 ±10.1 μm, respectively; P<.001), whereas the milling/sintering groups exhibited significantly smaller values than the controls (P=.004). The milling groups showed significantly larger absolute marginal discrepancy than the control groups (137.4 ±29.0 and 139.2 ±18.9 μm, respectively; P<.05). In the selective laser melting and milling/sintering groups, the absolute marginal discrepancy values were material-specific (P<.05). Nonetheless, the milling/sintering groups yielded statistically comparable (P=.935) or smaller (P<.001) absolute marginal discrepancies to the control groups. The findings of this in vitro μCT study showed that the marginal fit values of the Co-Cr alloy greatly depended on the fabrication methods and, occasionally, the alloy systems. Fixed dental prostheses produced by using the milling/sintering technique can be considered clinically acceptable in terms of marginal fit. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Microstructure and Current-Voltage Characteristics of Erbium Oxide Doped Multicomponent Zinc Oxide Varistors

NASA Astrophysics Data System (ADS)

Roy, Samarpita; Kundu Roy, Tapatee; Das, Debdulal

2018-03-01

The present work emphasizes the influence of Er2O3 addition on the microstructure and nonlinear current-voltage characteristics of ZnO based varistors prepared by mixing in a high energy ball mill followed by compaction and sintering at a temperature of 1100 °C for duration ranging from 0.5 to 8 h. Increasing sintering time is found to enhance the size of ZnO grains of the sintered pellets and thereby, degrades the electrical properties. However, Er2O3 addition retards the grain growth of ZnO due to the generation of secondary spinel phases (ErVO4 and Er-rich) at grain boundaries and triple points that restrict the grain boundary migration. Er2O3 modified ZnO varistor sintered at 1100 °C for 0.5 h exhibits considerably improved electrical property with nonlinear exponent and breakdown field of 27 and 3880 V cm-1, respectively.

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.

Microstructural Evolution and Mechanical Properties of Nanointermetallic Phase Dispersed Al65Cu20Ti15 Amorphous Matrix Composite Synthesized by Mechanical Alloying and Hot Isostatic Pressing

NASA Astrophysics Data System (ADS)

Roy, D.; Mitra, R.; Ojo, O. A.; Lojkowski, W.; Manna, I.

2011-08-01

The structure and mechanical properties of nanocrystalline intermetallic phase dispersed amorphous matrix composite prepared by hot isostatic pressing (HIP) of mechanically alloyed Al65Cu20Ti15 amorphous powder in the temperature range 573 K to 873 K (300 °C to 600 °C) with 1.2 GPa pressure were studied. Phase identification by X-ray diffraction (XRD) and microstructural investigation by transmission electron microscopy confirmed that sintering in this temperature range led to partial crystallization of the amorphous powder. The microstructures of the consolidated composites were found to have nanocrystalline intermetallic precipitates of Al5CuTi2, Al3Ti, AlCu, Al2Cu, and Al4Cu9 dispersed in amorphous matrix. An optimum combination of density (3.73 Mg/m3), hardness (8.96 GPa), compressive strength (1650 MPa), shear strength (850 MPa), and Young's modulus (182 GPa) were obtained in the composite hot isostatically pressed ("hipped") at 773 K (500 °C). Furthermore, these results were compared with those from earlier studies based on conventional sintering (CCS), high pressure sintering (HPS), and pulse plasma sintering (PPS). HIP appears to be the most preferred process for achieving an optimum combination of density and mechanical properties in amorphous-nanocrystalline intermetallic composites at temperatures ≤773 K (500 °C), while HPS is most suited for bulk amorphous alloys. Both density and volume fraction of intermetallic dispersoids were found to influence the mechanical properties of the composites.

PTCR characteristics and microstructure of porous (Ba,Sr)TiO3 ceramics prepared by spark plasma sintering

NASA Astrophysics Data System (ADS)

Lee, Ki-Ju; Tang, Dongxu; Park, K.; Cho, Won-Seung

2010-02-01

Porous Y-doped (Ba,Sr)TiO3 ceramics were prepared by the spark plasma sintering of (Ba,Sr)TiO3 powders with different amounts of carbon black, and by subsequently burning out the carbon black acting as a pore precursor. The microstructure, PTCR and gas-sensing characteristics for porous Y-doped (Ba,Sr)TiO3 ceramics were investigated. Spark plasma sintered (Ba,Sr)TiO3 ceramics revealed a very fine microstructure containing submicron-sized grains with a cubic phase and revealed an increased porosity after the carbon black was burned out. As a result of reoxidation treatment, the grain size of the (Ba,Sr)TiO3 ceramics increased to a few μm and the cubic phase transformed into a tetragonal phase. The phase transformation of (Ba,Sr)TiO3 ceramics was affected by grain size. The PTCR jump in the (Ba,Sr)TiO3 ceramics prepared by adding 40 vol.% carbon black showed an excellent value of 4.72 × 106, which was ten times higher than the PTCR jump in (Ba,Sr)TiO3 ceramics. The electrical resistivity of the porous (Ba,Sr)TiO3 ceramics was recovered as the atmosphere changed from a reducing gas (N2) to an oxidizing gas (O2) under consecutive heating and cooling cycles.

Compositional Design of Dielectric, Ferroelectric and Piezoelectric Properties of (K, Na)NbO₃ and (Ba, Na)(Ti, Nb)O₃ Based Ceramics Prepared by Different Sintering Routes.

PubMed

Eiras, José A; Gerbasi, Rosimeire B Z; Rosso, Jaciele M; Silva, Daniel M; Cótica, Luiz F; Santos, Ivair A; Souza, Camila A; Lente, Manuel H

2016-03-08

Lead free piezoelectric materials are being intensively investigated in order to substitute lead based ones, commonly used in many different applications. Among the most promising lead-free materials are those with modified NaNbO₃, such as (K, Na)NbO₃ (KNN) and (Ba, Na)(Ti, Nb)O₃ (BTNN) families. From a ceramic processing point of view, high density single phase KNN and BTNN ceramics are very difficult to sinter due to the volatility of the alkaline elements, the narrow sintering temperature range and the anomalous grain growth. In this work, Spark Plasma Sintering (SPS) and high-energy ball milling (HEBM), following heat treatments (calcining and sintering), in oxidative (O₂) atmosphere have been used to prepare single phase highly densified KNN ("pure" and Cu 2+ or Li 1+ doped), with theoretical densities ρ th > 97% and BTNN ceramics (ρ th - 90%), respectively. Using BTTN ceramics with a P 4 mm perovskite-like structure, we showed that by increasing the NaNbO₃ content, the ferroelectric properties change from having a relaxor effect to an almost "normal" ferroelectric character, while the tetragonality and grain size increase and the shear piezoelectric coefficients ( k 15 , g 15 and d 15 ) improve. For KNN ceramics, the results reveal that the values for remanent polarization as well as for most of the coercive field are quite similar among all compositions. These facts evidenced that Cu 2+ may be incorporated into the A and/or B sites of the perovskite structure, having both hardening and softening effects.

Microstructures and Properties of W-Ti Alloys Prepared Under Different Cooling Conditions

NASA Astrophysics Data System (ADS)

Dai, Weili; Liang, Shuhua; Yang, Qing; Zou, Juntao; Zhuo, Longchao

2016-07-01

W-(10 to 15) wt.% Ti alloys were sintered at 1400 or 1500 °C and cooled under different cooling conditions. The microstructures and properties of W-Ti alloys were affected by the cooling conditions. XRD, SEM, EBSD, and TEM were carried out to investigate the effects of cooling conditions and sintering temperature on the microstructures of W-Ti alloys. The nanohardness and elastic modulus of the alloys were also investigated. The results showed that when the temperature was 1500 °C, the content of Ti-rich phase in W-(10 to 15) wt.% Ti alloys decreased obviously with the increase of cooling rate (the average cooling rate of furnace cooling, air cooling and water cooling was 0.2, 10, and 280 °C/s, respectively). For the W-10 wt.% Ti alloy, the content decreased from 20.5 to 9.7%, and the grain size decreased from 2.33 to 0.67 μm. When the temperature decreased to 1400 °C, the grain size was also decreased sharply with the increase of cooling rate, but there was a little change in the microstructure. Meanwhile, the grain sizes were smaller than those of the alloys sintered at 1500 °C. The nanohardness and elastic modulus increased with the increase of cooling rate, and the alloys sintered at different temperatures had different nanohardness and elastic modulus which depended on the cooling conditions. Sintering at a proper temperature and then cooling at a certain cooling condition was a useful method to fabricate alloy with less Ti-rich phase and high properties.

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

Fabrication of a porous material with a porosity gradient by a pulsed electric current sintering process

NASA Astrophysics Data System (ADS)

Suk, Myung-Jin; Choi, Sung-II; Kim, Ji-Soon; Kim, Young Do; Kwon, Young-Soon

2003-12-01

A porous structure with a porosity gradient can be applied to the preparation of continuous FGM, where liquid or chemical vapor of the second phase is infiltrated into the graded pores. It also has applications in skeletal implant materials and ultrafiltration media. An attempt was made to fabricate a porous material with a porosity gradient by means of a pulsed electric current sintering (PECS) process. The present work describes not only the measured value of the temperature difference between the upper and lower part of the specimen, which brings about a gradual change in pore distribution, but also the sintering characteristics of the porous structure obtained by the pressureless PECS process.

Process for fabricating articles of tungsten-nickel-iron alloy

DOEpatents

Northcutt, Jr., Walter G.; Snyder, Jr., William B.

1976-01-01

A high density W--Ni--Fe alloy of composition 85-96% by weight W and the remainder Ni and Fe in a wt. ratio of 5:5-8:2 having enhanced mechanical properties is prepared by compacting the mixed powders, sintering the compact in reducing atmosphere to near theoretical density followed by further sintering at a temperature where a liquid phase is present, vacuum annealing, and cold working to achieve high uniform hardness.

Mechanisms and mechanics of shape loss during supersolidus liquid-phase sintering

NASA Astrophysics Data System (ADS)

Lal, Anand

Rapid sinter densification of relatively coarse prealloyed powders is possible by exceeding the solidus temperature in an approach termed supersolidus liquid phase sintering (SLPS). However, narrow processing windows for densification without distortion often limit this process. The liquid films at the grain boundaries that are responsible for densification also reduce the structural rigidity of components. Hence, components tend to slump under their own weight. Thus, the present study investigates shape loss during SLPS and rationalizes the processing and material factors with regard to separating densification from distortion. Experiments are performed on various prealloyed powders, including bronze, 316L stainless steel, and T15 tool steel. Differential thermal analysis, dilatometry, and in situ video imaging of sintering compacts are used to follow melting, densification, and distortion, respectively. Further, density and dimensional measurements are performed on sintered compacts. Results indicate a dependence of distortion on the sintering temperature and time, compact size, and melting behavior of the alloy. It is shown that the sintering temperature window, where high-density, precise components are obtained, can be widened for 316L stainless steel by boron addition. For the first time, a beam bending technique is used to measure the macroscopic apparent viscosity of semisolid bronze. The viscosity drops with temperature above the solidus and lies in the range of 108 to 106 Pa-s. Additionally, the in situ transverse rupture strength of bronze is measured to demonstrate the softening above the solidus temperature. Further, microstructural measurements are performed to enable correlation with the slumping behavior and viscosity. A model combining the deformation mechanisms, driving forces, and microstructural characteristics is developed to predict the conditions for densification and distortion onset. The microstructure is also correlated with the magnitude of shape loss and viscosity of a semisolid aggregate. A mechanistic model, based on the semisolid rheological characteristics, is developed to predict the magnitude and nature of shape loss. The model shows good correlation with experimental data for bronze. This study offers critical insight into SLPS and provides processing strategies for fabrication of high-density components without shape loss.

Preparation of long alumina fibers by sol-gel method using tartaric acid

NASA Astrophysics Data System (ADS)

Tan, Hong-Bin

2011-12-01

Long alumina fibers were prepared by sol-gel method. The spinning sol was obtained by mixing aluminum nitrate, tartaric acid, and polyvinylpyrrolidone with a mass ratio of 10:3:1.5. Thermogravimetry-differential scanning calorimetry (TG-DSC), Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD), and scanning electron microscopy (SEM) were used to characterize the properties of the gel and ceramic fibers. A little of α-Al2O3 phase is observed in the alumina precursor gel fibers sintered at 1273 K. The fibers with a uniform diameter can be obtained when sintered at 1473 K, and its main phase is also indentified as α-Al2O3.

Dielectric and Piezoelectric Properties of Barium-substituted Sr1.9Ca0.1NaNb5O15 Ceramics

NASA Astrophysics Data System (ADS)

Xie, Rong-Jun; Akimune, Yoshio; Wang, Ruiping; Hirosaki, Naoto; Nishimura, Toshiyuki

2003-12-01

Highly dense piezoelectric ceramics of tungsten bronze-type (Sr1.9Ca0.1)1-0.5xBaxNaNb5O15 (where x=0.1--0.8) were prepared by spark plasma sintering. The crystallographic parameters, dielectric behaviors and piezoelectric properties of the sintered ceramics were investigated, and the effects of the Ba substitution on these electrical properties were discussed. The structural analysis and the electrical property measurements indicate a morphotropic phase boundary (MPB)-like phenomenon at x=0.4--0.5. In all compositions, a diffuse phase transition and a relaxor behavior are observed. The electrical properties are found to be crystallographically dependent.

A comparative study of the physical properties of Cu-Zn ferrites annealed under different atmospheres and temperatures: Magnetic enhancement of Cu0.5Zn0.5Fe2O4 nanoparticles by a reducing atmosphere

NASA Astrophysics Data System (ADS)

Gholizadeh, Ahmad

2018-04-01

In the present work, the influence of different sintering atmospheres and temperatures on physical properties of the Cu0.5Zn0.5Fe2O4 nanoparticles including the redistribution of Zn2+ and Fe3+ ions, the oxidation of Fe atoms in the lattice, crystallite sizes, IR bands, saturation magnetization and magnetic core sizes have been investigated. The fitting of XRD patterns by using Fullprof program and also FT-IR measurement show the formation of a cubic structure with no presence of impurity phase for all the samples. The unit cell parameter of the samples sintered at the air- and inert-ambient atmospheres trend to decrease with sintering temperature, but for the samples sintered under carbon monoxide-ambient atmosphere increase. The magnetization curves versus the applied magnetic field, indicate different behaviour for the samples sintered at 700 °C with the respect to the samples sintered at 300 °C. Also, the saturation magnetization increases with the sintering temperature and reach a maximum 61.68 emu/g in the sample sintered under reducing atmosphere at 600 °C. The magnetic particle size distributions of samples have been calculated by fitting the M-H curves with the size distributed Langevin function. The results obtained from the XRD and FTIR measurements suggest that the magnetic core size has the dominant effect in variation of the saturation magnetization of the samples.

Enhanced Photoluminescent Properties and Crystalline Morphology of LiBaPO4:Tm3+ Phosphor through Microwave Sintering Method

PubMed Central

Lai, Hsuan-Lin; Weng, Min-Hang; Yang, Ru-Yuan; Chang, Shoou-Jinn

2016-01-01

An investigation of the photoluminescent properties and crystalline morphology of blue emitting LiBa1−xPO4:xTm3+ phosphors with various concentrations (x = 0.005–0.030) of Tm3+ ions were synthesized by microwave sintering. For comparison, the LiBa1−xPO4:xTm3+ powders sintered at the same sintering condition but in a conventional furnace were also investigated. LiBaPO4 without second phase was formed no matter which furnace was used. More uniform grain size distributions are obtained by microwave sintering. When the concentration of Tm3+ ion was x = 0.015, the luminescence intensity reached a maximum value, and then decreased with the increases of the Tm3+ concentration due to concentration quenching effect. The microwave sintering significantly enhanced the emission intensity of LiBa1−xPO4:xTm3+ phosphors. Additionally, the d-d interaction is the key mechanism of concentration quenching for LiBaPO4:Tm3+. The chromaticity (x, y) for all LiBa1−xPO4:xTm3+ phosphors are located at (0.16, 0.05), which will be classified as a blue region. PMID:28773483

Study of the suitability of a commercial hydroxyapatite powder to obtain sintered compacts for medical applications

NASA Astrophysics Data System (ADS)

Palacio, C.; Jaramillo, D.; Correa, S.; Arroyave, M.

2017-06-01

Hydroxyapatite (HA) is a material widely used by the medical community due to its Ca/P ratio is comparable to the Ca/P ratio of bones and teeth, which promotes osteoinduction and osteoconduction processes when in contact with bone tissue, either as volume piece or coating. This work focuses on studying the quality of the commercial HA powder MKnano-#MKN-HXAP-S12 µm, after processing, to obtain sintered compact discs with suitable physical and chemical characteristics for implants applications. The HA powder was processed through calcination, grinding, pressing and sintering to evaluate the effect of such as procedures in the compacts dics quality. The raw powder was characterized by laser diffraction, SEM, XRF, XRD, TGA and DSC while the characteristics of the obtained compact discs were determined by dilatometry and XRD to identify the sintering temperature range, constituent phases, the amorphous content and the crystallinity degree, parameters that allow determining their suitability for implants applications. Although, it was not possible to obtain sintered compacts with the suitable chemical composition and without fractures, this work allowed to identify the parameters that determine the suitability of a HA powder to obtain sintered compacts for medical applications, as well as the characterization protocol that allows the evaluation of such parameters.

Synthesis of Ti-6Al-4V alloy with nano-TiN microstructure via spark plasma sintering technique

NASA Astrophysics Data System (ADS)

E Falodun, O.; Obadele, B. A.; Oke, S. R.; E Maja, M.; Olubambi, P. A.

2017-12-01

The effect of nano-TiN dispersion strengthened Ti-6Al-4V via spark plasma sintering method has been investigated. Ti-6Al-4V with 4 vol. percent of nano-TiN were mixed in a Turbula shaker mixer for 8 h at a speed of 49 rpm and the admixed powders were sintered at sintering temperature range of 1000 - 1100 °C, holding time of 10-30 mins, heating rate of 100 °C/min under an applied pressure of 50 MPa. The morphology of the as-received and sintered compacts was examined by scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS) and phase analysis was done by X-ray diffractometry (XRD). The sintered compacts without nano-TiN reveal lamellar structure while reinforced Ti-6Al-4V with nano-TiN shows a bimodal structure and titanium nitride has a great influence on a grain growth at high temperature. Furthermore, the microstructural formation mechanism was investigated. With the addition of the content of Ti-6Al-4V with 4 vol.% of nano-TiN, the micro-hardness also improved and this was due to homogenous distribution of TiN in Ti-6Al-4V matrix.

Report on in-situ studies of flash sintering of uranium dioxide

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

Raftery, Alicia Marie

Flash sintering is a novel type of field assisted sintering that uses an electric field and current to provide densification of materials on very short time scales. The potential for field assisted sintering techniques to be used in producing nuclear fuel is gaining recognition due to the potential economic benefits and improvements in material properties. The flash sintering behavior has so far been linked to applied and material parameters, but the underlying mechanisms active during flash sintering have yet to be identified. This report summarizes the efforts to investigate flash sintering of uranium dioxide using dilatometer studies at Los Alamosmore » National Laboratory and two separate sets of in-situ studies at Brookhaven National Laboratory’s NSLS-II XPD-1 beamline. The purpose of the dilatometer studies was to understand individual parameter (applied and material) effects on the flash behavior and the purpose of the in-situ studies was to better understand the mechanisms active during flash sintering. As far as applied parameters, it was found that stoichiometry, or oxygen-to-metal ratio, has a significant effect on the flash behavior (time to flash and speed of flash). Composite systems were found to have degraded sintering behavior relative to pure UO 2. The critical field studies are complete for UO 2.00 and will be analyzed against an existing model for comparison. The in-situ studies showed that the strength of the field and current are directly related to the sample temperature, with temperature-driven phase changes occurring at high values. The existence of an ‘incubation time’ has been questioned, due to a continuous change in lattice parameter values from the moment that the field is applied. Some results from the in-situ experiments, which should provide evidence regarding ion migration, are still being analyzed. Some preliminary conclusions can be made from these results with regard to using field assisted sintering to fabricate nuclear fuel. First, the pure UO 2-based system shows promising behavior with flash sintering, but composite systems are likely to show better sintering behavior with spark plasma sintering. Efforts to develop these methods should therefore be tailored towards the likelihood of success. Additionally, modeling is a rapidly developing aspect of current flash sintering research and should be used in parallel with experiments. Ultimately, ongoing flash sintering studies on various materials, like those summarized in this report, are rapidly contributing to the feasibility of controlling this method for use in the future.« less

Emerging Ceramic-based Materials for Dentistry

PubMed Central

Denry, I.; Kelly, J.R.

2014-01-01

Our goal is to give an overview of a selection of emerging ceramics and issues for dental or biomedical applications, with emphasis on specific challenges associated with full-contour zirconia ceramics, and a brief synopsis on new machinable glass-ceramics and ceramic-based interpenetrating phase composites. Selected fabrication techniques relevant to dental or biomedical applications such as microwave sintering, spark plasma sintering, and additive manufacturing are also reviewed. Where appropriate, the authors have added their opinions and guidance. PMID:25274751

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.

Effect of Mg and Si co-substitution on microstructure and strength of tricalcium phosphate ceramics.

PubMed

García-Páez, Ismael H; Carrodeguas, Raúl García; De Aza, Antonio H; Baudín, Carmen; Pena, Pilar

2014-02-01

Magnesium and silicon co-doped tricalcium phosphate (TCP) ceramics with compositions corresponding to 0, 5 and 10wt% CaMg(SiO3)2 in the system Ca3(PO4)2-CaMg(SiO3)2 were obtained by conventional sintering of compacted mixtures of Ca3(PO4)2, MgO, SiO2 and CaCO3 powders at temperatures between 1100 and 1450°C. Microstructural analyses were performed by X-ray diffraction and field emission scanning electron microscopy with energy dispersive spectroscopy. Major phases in the obtained ceramics were β- or α+β-tricalcium phosphate containing Mg and Si in solid solution. Certain amounts of liquid were formed during sintering depending on composition and temperature. There were found significant differences in distributions of strength determined by the diametral compression of disc tests (DCDT). Failure strengths were controlled by microstructural defects associated with phase development. Mg and Si additions were found to be effective to improve densification and associated strength of TCP bioceramics due to the enhancement of sintering by the low viscosity liquids formed. The highest density and strength were obtained for the TCP ceramic containing 5wt% CaMg(SiO3)2 sintered at 1300°C. Cracking and porosity increased at higher temperatures due to grain growth and swelling. © 2013 Published by Elsevier Ltd.

Tailoring of processing parameters for sintering microsphere-based scaffolds with dense-phase carbon dioxide

PubMed Central

Jeon, Ju Hyeong; Bhamidipati, Manjari; Sridharan, BanuPriya; Scurto, Aaron M.; Berkland, Cory J.; Detamore, Michael S.

2015-01-01

Microsphere-based polymeric tissue-engineered scaffolds offer the advantage of shape-specific constructs with excellent spatiotemporal control and interconnected porous structures. The use of these highly versatile scaffolds requires a method to sinter the discrete microspheres together into a cohesive network, typically with the use of heat or organic solvents. We previously introduced subcritical CO2 as a sintering method for microsphere-based scaffolds; here we further explored the effect of processing parameters. Gaseous or subcritical CO2 was used for making the scaffolds, and various pressures, ratios of lactic acid to glycolic acid in poly(lactic acid-co-glycolic acid), and amounts of NaCl particles were explored. By changing these parameters, scaffolds with different mechanical properties and morphologies were prepared. The preferred range of applied subcritical CO2 was 15–25 bar. Scaffolds prepared at 25 bar with lower lactic acid ratios and without NaCl particles had a higher stiffness, while the constructs made at 15 bar, lower glycolic acid content, and with salt granules had lower elastic moduli. Human umbilical cord mesenchymal stromal cells (hUCMSCs) seeded on the scaffolds demonstrated that cells penetrate the scaffolds and remain viable. Overall, the study demonstrated the dependence of the optimal CO2 sintering parameters on the polymer and conditions, and identified desirable CO2 processing parameters to employ in the sintering of microsphere-based scaffolds as a more benign alternative to heat-sintering or solvent-based sintering methods. PMID:23115065

Microstructure and corrosion behavior of porous coatings on titanium alloy by vacuum-brazed method.

PubMed

Lee, T M; Chang, E; Yen, C H

2006-05-01

The microstructural evolution and electrochemical characteristics of brazed porous-coated Ti-6Al-4V alloy were analyzed and compared with respect to the conventionally 1300 degrees C sintering method. The titanium filler metal of low-melting-point (934 degrees C) Ti-15Cu-15Ni was used to braze commercially pure (CP) titanium beads onto the substrate of Ti-6Al-4V alloy at 970 degrees C for 2 and 8 h. Optical microscopy, scanning and transmission electron microscopy, and X-ray diffractometry (XRD) were used to characterize the microstructure and phase of the brazed metal; also, the potentiostat was used for corrosion study. Experimental results indicate that the bead/substrate contact interface of the 970 degrees C brazed specimens show larger contact area and higher radius curvature in comparison with 1300 degrees C sintering method. The microstructure of brazed specimens shows the Widmanstätten structure in the brazed zone and equiaxed alpha plus intergranular beta in the Ti-6Al-4V substrate. The intermetallic Ti2Ni phase existing in the prior filler metal diminishes, while the Ti2Cu phase can be identified for the substrate at 970 for 2 h, but the latter phase decrease with time. In Hank's solution at 37 degrees C, the corrosion rates of the 1300 degrees C sintering and the 970 degrees C brazed samples are similar at corrosion potential (E(corr)) in potentiodynamic test, and the value of E(corr) for the brazed sample is noble to the sintering samples. The current densities of the brazed specimens do not exceed 100 microA/cm2 at 3.5 V (SCE). These results suggest that the vacuum-brazed method exhibits the potentiality to manufacture the porous-coated specimens for biomedical application. (c) 2005 Wiley Periodicals, Inc.

Diffraction, microstructure and thermal stability analysis in a double phase nanocrystalline Al20Mg20Ni20Cr20Ti20 high entropy alloy

NASA Astrophysics Data System (ADS)

Rameshbabu, A. M.; Parameswaran, P.; Vijayan, V.; Panneer, R.

2017-12-01

An effort has been made to develop a new composition of AlMgNiCrTi high entropy alloy (HEA) with a distinct properties includes squat density, intense strength and hardness, superior corrosion resistance, better oxidation resistance, high temperature resistance, fatigue load and crack resistance to congregate the necessity of aircraft applications. The equivalent atomic percentage for the above defined composition is established using analytical correlation for molar and atom renovation by trial and error method. The alloy is synthesized by powder metallurgy technique through mechanical alloying. Succeeding to mechanical alloying it is elucidated that the metal powder is primarily composed of single BCC solid solution with crystallite magnitude <10 nm. It is also observed that the alloy is thermally stable at prominent temperature about 800°C as it is retained its nanostructure which was revealed using differential scanning caloriemetry (DSC). This alloy powder was consolidated and sintered using spark plasma sintering at 800°C with 50 Mpa pressure to a density of 98.83%. Subsequent to sintering, Titanium carbide FCC phase evolved along with the BCC phase. The alloying behavior and phase transformation were studied using X-ray diffraction (XRD) and scanning electron microscope (SEM). The homogeneity of the composition is confirmed by energy dispersive spectroscopy (EDS). The hardness of the alloy is found to be 710±20 HV. The evolutions of the phases and hardness imply that this alloy is apposite for both high strength and high temperature applications.

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.

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.

Characterization of Sintering Dust, Blast Furnace Dust and Carbon Steel Electric Arc Furnace Dust

NASA Astrophysics Data System (ADS)

Chang, Feng; Wu, Shengli; Zhang, Fengjie; Lu, Hua; Du, Kaiping

In order to make a complete understanding of steel plant metallurgical dusts and to realize the goal of zero-waste, a study of their properties was undertaken. For these purposes, samples of two sintering dusts (SD), two blast furnace dusts (BFD), and one electric arc furnace dust (EAFD) taken from the regular production process were subjected to a series of tests. The tests were carried out by using granulometry analysis, chemical analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy via SEM (EDS), and Fourier transform infrared spectroscopy (FTIR). The dominant elements having an advantage of reuse are Fe, K, Cl, Zn, C. The dominant mineralogical phases identified in sintering dust are KCl, Fe2O3, CaCO3, CaMg(CO3)2, NaCl, SiO2. Mineralogical phases exist in blast furnace dust are Fe2O3, Fe3O4, with small amount of KCl and kaolinite coexist. While in electric arc furnace dust, Fe3O4, ZnFe2O4, CaCO3, CaO, Ca(OH)2 are detected.

Phase composition, microstructure, and mechanical properties of porous Ti-Nb-Zr alloys prepared by a two-step foaming powder metallurgy method.

PubMed

Rao, X; Chu, C L; Zheng, Y Y

2014-06-01

Porous Ti-Nb-Zr alloys with different porosities from 6.06 to 62.8% are prepared by a two-step foaming powder metallurgy method using TiH2, Nb, and Zr powders together with 0 to 50wt% of NH4HCO3. The effects of the amounts of Nb and Zr as well as the sintering temperature (1473 to 1673K) on their phase composition, porosity, morphology, and mechanical characteristics are investigated. By controlling the porosity, Nb and Zr concentrations as well as the sintering temperature, porous Ti-Nb-Zr alloys with different mechanical properties can be obtained, for example, the hardness between 290 and 63HV, the compressive strength between 1530.5 and 73.4MPa, and the elastic modulus between 10.8 and 1.2GPa. The mechanical properties of the sintered porous Ti-Nb-Zr alloys can be tailored to match different requirements for the human bones and are thus potentially useful in the hard tissue implants. Copyright © 2014 Elsevier Ltd. All rights reserved.

110K Bi-Sr-Ca-Cu-O superconductor oxide and method for making same

DOEpatents

Veal, B.W.; Downey, J.W.; Lam, D.J.; Paulikas, A.P.

1992-12-22

A superconductor is disclosed consisting of a sufficiently pure phase of the oxides of Bi, Sr, Ca, and Cu to exhibit a resistive zero near 110K resulting from the process of forming a mixture of Bi[sub 2]O[sub 3], SrCO[sub 3], CaCO[sub 3] and CuO into a particulate compact wherein the atom ratios are Bi[sub 2], Sr[sub 1.2-2.2], Ca[sub 1.8-2.4], Cu[sub 3]. Thereafter, heating the particulate compact rapidly in the presence of oxygen to an elevated temperature near the melting point of the oxides to form a sintered compact, and then maintaining the sintered compact at the elevated temperature for a prolonged period of time. The sintered compact is cooled and reground. Thereafter, the reground particulate material is compacted and heated in the presence of oxygen to an elevated temperature near the melting point of the oxide and maintained at the elevated temperature for a time sufficient to provide a sufficiently pure phase to exhibit a resistive zero near 110K. 7 figs.

110K Bi-Sr-Ca-Cu-O superconductor oxide and method for making same

DOEpatents

Veal, Boyd W.; Downey, John W.; Lam, Daniel J.; Paulikas, Arvydas P.

1992-01-01

A superconductor consisting of a sufficiently pure phase of the oxides of Bi, Sr, Ca, and Cu to exhibit a resistive zero near 110K resulting from the process of forming a mixture of Bi.sub.2 O.sub.3, SrCO.sub.3, CaCO.sub.3 and CuO into aparticulate compact wherein the atom ratios are Bi.sub.2, Sr.sub.1.2-2.2, Ca.sub.1.8-2.4, Cu.sub.3. Thereafter, heating the particulate compact rapidly in the presence of oxygen to an elevated temperature near the melting point of the oxides to form a sintered compact, and then maintaining the sintered compact at the elevated temperature for a prolonged period of time. The sintered compact is cooled and reground. Thereafter, the reground particulate material is compacted and heated in the presence of oxygen to an elevated temperature near the melting point of the oxide and maintained at the elevated temperature for a time sufficient to provide a sufficiently pure phase to exhibit a resistive zero near 110K.

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.

Study on Microstructures and Mechanical Properties of Foam Titanium Carbide Ceramics Fabricated by Reaction Sintering Process

NASA Astrophysics Data System (ADS)

Ma, Yana; Bao, Chonggao; Chen, Jie; Song, Suocheng; Han, Longhao

2018-05-01

Foam titanium carbide (TiC) ceramics with a three-dimensional network structure were fabricated by the reaction sintering process, in which polyurethane foam was taken as the template, and TiO2 and phenolic resin were used as the reactants. Phase, microstructures and fracture morphologies of foam TiC ceramics were characterized by x-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The results show that when the mass ratios of phenolic resin and TiO2 (F/T) are (0.8-1.2): 1, foam TiC ceramics with pure TiC phase can be formed. As the F/T ratios increase, crystal lattice parameters of fabricated foam TiC ceramics become bigger. When the value of F/T decreases from 1.2 to 0.8, grain size of TiC grows larger and microstructures get denser; meanwhile, the compressive strength increases from 0.10 to 1.05 MPa. Additionally, either raising the sintering temperatures or extending holding time can facilitate the completion of the reaction process and increase the compressive strength.

Stability of Nanocrystalline Spark Plasma Sintered 3Y-TZP

PubMed Central

Chintapalli, Ravikiran; Mestra, Alvaro; García Marro, Fernando; Yan, Haixue; Reece, Michael; Anglada, Marc

2010-01-01

Spark plasma sintered 3Y-TZP has been investigated with respect to hydrothermal ageing and grinding. The sintering was performed between the temperatures of 1,100 and 1,600 °C for a soaking time of 5 minutes and the resulting materials were obtained with grain sizes between 65 to 800 nm and relative densities between 88.5 to 98.8%. Experiments on hydrothermal ageing in water vapour at 131 °C, 2 bars during 60 hours shows that phase stability is retained, elastic modulus and hardness of near surface region measured by nanoindentation does not change in fine grain (<200 nm) materials, in spite of porosity. In ground specimens, very small amount of transformation was found for all grain sizes studied.

Microstructural study and densification analysis of hot work tool steel matrix composites reinforced with TiB{sub 2} particles

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

Fedrizzi, A., E-mail: anna.fedrizzi@ing.unitn.it; Pellizzari, M.; Zadra, M.

2013-12-15

Hot work tool steels are characterized by good toughness and high hot hardness but are less wear resistant than other tooling materials, such as high speed steel. Metal matrix composites show improved tribological behavior, but not much work has been done in the field of hot work tool steels. In this paper TiB{sub 2}-reinforced hot work tool steel matrix composites were produced by spark plasma sintering (SPS). Mechanical alloying (MA) was proposed as a suited process to improve the composite microstructure. Density measurements and microstructure confirmed that MA promotes sintering and produces a fine and homogeneous dispersion of reinforcing particles.more » X-ray diffraction patterns of the sintered composites highlighted the formation of equilibrium Fe{sub 2}B and TiC, as predicted by thermodynamic calculations using Thermo-Calc® software. Scanning electron microscopy as well as scanning Kelvin probe force microscopy highlighted the reaction of the steel matrix with TiB{sub 2} particles, showing the formation of a reaction layer at the TiB{sub 2}-steel interface. Phase investigations pointed out that TiB{sub 2} is not chemically stable in steel matrix because of the presence of carbon even during short time SPS. - Highlights: • TiB{sub 2} reinforced steel matrix composites were produced by spark plasma sintering. • TiB{sub 2} was successfully dispersed in the steel matrix by mechanical alloying. • Steel and TiB{sub 2} react during sintering forming equilibrium Fe{sub 2}B and TiC. • The new phases were investigated by means of AFM, Volta potential and XRD analyses.« less

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.

Compositional Design of Dielectric, Ferroelectric and Piezoelectric Properties of (K, Na)NbO3 and (Ba, Na)(Ti, Nb)O3 Based Ceramics Prepared by Different Sintering Routes

PubMed Central

Eiras, José A.; Gerbasi, Rosimeire B. Z.; Rosso, Jaciele M.; Silva, Daniel M.; Cótica, Luiz F.; Santos, Ivair A.; Souza, Camila A.; Lente, Manuel H.

2016-01-01

Lead free piezoelectric materials are being intensively investigated in order to substitute lead based ones, commonly used in many different applications. Among the most promising lead-free materials are those with modified NaNbO3, such as (K, Na)NbO3 (KNN) and (Ba, Na)(Ti, Nb)O3 (BTNN) families. From a ceramic processing point of view, high density single phase KNN and BTNN ceramics are very difficult to sinter due to the volatility of the alkaline elements, the narrow sintering temperature range and the anomalous grain growth. In this work, Spark Plasma Sintering (SPS) and high-energy ball milling (HEBM), following heat treatments (calcining and sintering), in oxidative (O2) atmosphere have been used to prepare single phase highly densified KNN (“pure” and Cu2+ or Li1+ doped), with theoretical densities ρth > 97% and BTNN ceramics (ρth ~ 90%), respectively. Using BTTN ceramics with a P4mm perovskite-like structure, we showed that by increasing the NaNbO3 content, the ferroelectric properties change from having a relaxor effect to an almost “normal” ferroelectric character, while the tetragonality and grain size increase and the shear piezoelectric coefficients (k15, g15 and d15) improve. For KNN ceramics, the results reveal that the values for remanent polarization as well as for most of the coercive field are quite similar among all compositions. These facts evidenced that Cu2+ may be incorporated into the A and/or B sites of the perovskite structure, having both hardening and softening effects. PMID:28773304

Synthesis and evaluation of bioceramics for orthopedics and tissue culture applications

NASA Astrophysics Data System (ADS)

Demirkiran, Hande

Hydroxyapatite is the most well known phosphate in the biologically active phosphate ceramic family by virtue of its similarity to natural bone mineral. Among all bioglass compositions BioglassRTM45S5 is one of the most bioactive glasses. This study initially started by adding different amounts (1, 2.5, 5, 10, and 25 wt.%) of BioglassRTM45S5 to synthetic hydroxyapatite in order to improve the bioactivity of these bioceramics. The chemistries formed by sintering and their effect on different material properties including bioactivity were identified by using various techniques, such as powder and thin film x-ray diffraction, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy, X-ray absorption near edge spectroscopy, compression test, and nano indentation. All the results demonstrated that 10 and 25 wt.% BioglassRTM45S5 addition to hydroxyapatite and sintering at 1200°C for 4 hours yield new compositions with main Ca 5(PO4)2SiO4 and Na3Ca 6(PO4)5 crystalline phases dispersed in silicate glassy matrices, respectively. In addition, in vitro bioactivity tests such as bone like apatite formation in simulated body fluid and bone marrow stromal cell culture have shown that the crystalline and amorphous phases have an important role on improving bioactivity of these bioceramic compositions. Besides, compression test and nano indentation has given important information on compression strength and nano structure properties of these newly composed bioceramic materials and the bone like apatite layers formed on them, respectively. Finally, the effect of silicate addition on both formation and bioactivity of Na3Ca6(PO4)5 bioceramics were shown. These findings and different techniques used assisted to develop a phenomenological approach to demonstrate how the novel bioceramic compositions were composed and aid improving bioactivity of known bioceramic materials.

Powder Metallurgy of Uranium Alloy Fuels for TRU-Burning Reactors Final Technical Report

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

McDeavitt, Sean M

2011-04-29

Overview Fast reactors were evaluated to enable the transmutation of transuranic isotopes generated by nuclear energy systems. The motivation for this was that TRU isotopes have high radiotoxicity and relatively long half-lives, making them unattractive for disposal in a long-term geologic repository. Fast reactors provide an efficient means to utilize the energy content of the TRUs while destroying them. An enabling technology that requires research and development is the fabrication metallic fuel containing TRU isotopes using powder metallurgy methods. This project focused upon developing a powder metallurgical fabrication method to produce U-Zr-transuranic (TRU) alloys at relatively low processing temperatures (500ºCmore » to 600ºC) using either hot extrusion or alpha-phase sintering for charecterization. Researchers quantified the fundamental aspects of both processing methods using surrogate metals to simulate the TRU elements. The process produced novel solutions to some of the issues relating to metallic fuels, such as fuel-cladding chemical interactions, fuel swelling, volatility losses during casting, and casting mold material losses. Workscope There were two primary tasks associated with this project: 1. Hot working fabrication using mechanical alloying and extrusion • Design, fabricate, and assemble extrusion equipment • Extrusion database on DU metal • Extrusion database on U-10Zr alloys • Extrusion database on U-20xx-10Zr alloys • Evaluation and testing of tube sheath metals 2. Low-temperature sintering of U alloys • Design, fabricate, and assemble equipment • Sintering database on DU metal • Sintering database on U-10Zr alloys • Liquid assisted phase sintering on U-20xx-10Zr alloys Appendices Outline Appendix A contains a Fuel Cycle Research & Development (FCR&D) poster and contact presentation where TAMU made primary contributions. Appendix B contains MSNE theses and final defense presentations by David Garnetti and Grant Helmreich outlining the beginning of the materials processing setup. Also included within this section is a thesis proposal by Jeff Hausaman. Appendix C contains the public papers and presentations introduced at the 2010 American Nuclear Society Winter Meeting. Appendix A—MSNE theses of David Garnetti and Grant Helmreich and proposal by Jeff Hausaman A.1 December 2009 Thesis by David Garnetti entitled “Uranium Powder Production Via Hydride Formation and Alpha Phase Sintering of Uranium and Uranium-Zirconium Alloys for Advanced Nuclear Fuel Applications” A.2 September 2009 Presentation by David Garnetti (same title as document in Appendix B.1) A.3 December 2010 Thesis by Grant Helmreich entitled “Characterization of Alpha-Phase Sintering of Uranium and Uranium-Zirconium Alloys for Advanced Nuclear Fuel Applications” A.4 October 2010 Presentation by Grant Helmreich (same title as document in Appendix B.3) A.5 Thesis Proposal by Jeffrey Hausaman entitled “Hot Extrusion of Alpha Phase Uranium-Zirconium Alloys for TRU Burning Fast Reactors” Appendix B—External presentations introduced at the 2010 ANS Winter Meeting B.1 J.S. Hausaman, D.J. Garnetti, and S.M. McDeavitt, “Powder Metallurgy of Alpha Phase Uranium Alloys for TRU Burning Fast Reactors,” Proceedings of 2010 ANS Winter Meeting, Las Vegas, Nevada, USA, November 7-10, 2010 B.2 PowerPoint Presentation Slides from C.1 B.3 G.W. Helmreich, W.J. Sames, D.J. Garnetti, and S.M. McDeavitt, “Uranium Powder Production Using a Hydride-Dehydride Process,” Proceedings of 2010 ANS Winter Meeting, Las Vegas, Nevada, USA, November 7-10, 2010 B.4. PowerPoint Presentation Slides from C.3 B.5 Poster Presentation from C.3 Appendix C—Fuel cycle research and development undergraduate materials and poster presentation C.1 Poster entitled “Characterization of Alpha-Phase Sintering of Uranium and Uranium-Zirconium Alloys” presented at the Fuel Cycle Technologies Program Annual Meeting C.2 April 2011 Honors Undergraduate Thesis by William Sames, Research Fellow, entitled “Uranium Metal Powder Production, Particle Distribution Analysis, and Reaction Rate Studies of a Hydride-Dehydride Process"« less

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

Evaluation of marginal fit of single implant-supported metal-ceramic crowns prepared by using presintered metal blocks.

PubMed

Pasali, Baris; Sarac, Duygu; Kaleli, Necati; Sarac, Yakup Sinasi

2018-02-01

Recently, presintered metal blocks for nonprecious and precious metal implant-supported restorations have gained popularity in computer-aided design and computer-aided manufacturing (CAD-CAM) systems. However, few studies have evaluated the marginal discrepancy of implant-supported restorations made with these new alloy systems. The purpose of this in vitro study was to compare the milling-sintering method with the lost-wax and milling methods in terms of the marginal fit of implant-supported metal-ceramic restorations. Thirty implant abutments screwed to implant analogs were embedded into acrylic resin to investigate marginal fit and then divided according to fabrication methods into the following 3 groups (n=10): lost-wax (LW; control group), milling (M), and milling-sintering (MS). Porcelain material was applied to all specimens after completion of the fabrication process. Subsequently, all specimens were cemented to implant abutments for the measurement of marginal discrepancies. Twelve marginal discrepancy measurements were recorded on each implant abutment by using a stereomicroscope. The arithmetic mean of these 12 measurements was considered the mean marginal discrepancy value of each abutment. Data were statistically analyzed by using 1-way ANOVA and Tukey honest significant difference tests (α=.05). The lowest mean marginal discrepancy values (81 ±2 μm) were observed in the M group, which was significantly different (P<.001) from the other methods. The highest mean marginal discrepancy values (99 ±2 μm) were observed in the MS group. The results revealed that restorations prepared by the milling-sintering method provided clinically acceptable results (<120 μm); however, this new technique was not found to be as precise as the milling method in terms of marginal fit. Copyright © 2017 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

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.

Correlative tomography at the cathode/electrolyte interfaces of solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Wankmüller, Florian; Szász, Julian; Joos, Jochen; Wilde, Virginia; Störmer, Heike; Gerthsen, Dagmar; Ivers-Tiffée, Ellen

2017-08-01

This paper introduces a correlative tomography technique. It visualizes the spatial organization of primary and secondary phases at the interface of La0.58Sr0.4Co0.2Fe0.8O3-δ cathode/10 mol% Gadolinia doped Ceria/8 mol% Yttria stabilized Zirconia electrolyte. It uses focused ion beam/scanning electron microscope tomography (FIB/SEM), and combines data sets from Everhart-Thornley and Inlens detector differentiating four primary and two secondary material phases. In addition, grayscale information is correlated to elemental distribution gained by energy dispersive X-ray spectroscopy in a scanning transmission electron microscope. Interdiffusion of GDC into YSZ and SrZrO3 as secondary phases depend (in both amount and spatial organization) on the varied co-sintering temperature of the GDC/YSZ electrolyte. The ion-blocking SrZrO3 forms a continuous layer on top of the temperature-dependent GDC/YSZ interdiffusion zone (ID) at and below a co-sintering temperature of 1200 °C; above it becomes intermittent. 2D FIB/SEM images of primary and secondary phases at 1100, 1200, 1300 and 1400 °C were combined with a 3D FIB/SEM reconstruction (1300 °C). This reveals that ;preferred; oxygen ion transport pathways from the LSCF cathode through GDC and the ID into the YSZ electrolyte only exist in samples sintered above 1200 °C. The applied correlative technique expands our understanding of this multiphase cathode/electrolyte interface region.

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).

Electrical percolation threshold of magnetostrictive inclusions in a piezoelectric matrix under simulated sintering conditions

NASA Astrophysics Data System (ADS)

Bedard, Antoine Joseph; Barbero, Ever J.

2018-03-01

Magnetoelectric (ME) composites can be produced by embedding magnetostrictive H particles in a piezoelectric E matrix derived from a piezoelectric powder precursor. Previously, using a bi-disperse hard-shell model (Barbero and Bedard in Comput Part Mech, 2018. https://doi.org/10.1007/s40571-017-0165-4), it has been shown that the electrical percolation threshold of the conductive H phase can be increased by decreasing the piezoelectric E particle size, relative to the H phase particle size, and by increasing short-range affinity between the E and H particles. This study builds on our previous study by exploring what happens during sintering of the ME composite when either the H or E particles undergo deformation. It was found that deformation of the H particles reduces the percolation threshold, and that deformation of E particles increases inter-phase H-E mechanical coupling, thus contributing to enhancing of ME coupling.

Effect of liquid-phase sintering as a means of quality enhancement of pseudoalloys based on copper

NASA Astrophysics Data System (ADS)

Gordeev, Yu I.; Abkaryan, A. K.; Zeer, G. M.; Lepeshev, A. A.; Zelenkova, E. G.

2017-01-01

The effects of the liquid phase of a metal binder on the microstructure and properties of self-diffusion gradient composite (Cu - Al - ZnO) were investigated. For the compositions considered, it was revealed that at the temperature of about 550 °C, a liquid phase binder forms from nanoparticles Cu - Al. Applying a proper amount of a (Cu - Al) binder appeared to be beneficial for fabricating gradient composites with the desired self-diffusion process. It is also favorable for mass transfer of additives nanoparticles into the volume of a matrix during sintering and for the desired fine microstructure and mechanical properties. For the experimental conditions considered in this study, the best mechanical properties can be obtained when 6 mass % (Cu - Al) of ligature were used, which gave hardness HB at 120, electroerosion wear - 0.092 • 10-6 g / cycle, resistivity - 0.025 mcOm.

Protonic Conduction of BaCe0.85YO. 1503 Doped with SrTiO3

NASA Technical Reports Server (NTRS)

Dynys, Frederick W.; Sayir, Ali

2005-01-01

Reformers based on ceramic membrane technology potentially offer hydrogen production that is comparable to the cost of fossil fuels. Protonic conducting ceramic with the chemical formula AB03 offers the promise of highly selective hydrogen separation at intermediate temperature (400-800 C). Among different perovskite-type oxides, BaCe03 and SrCe03 based compositions show high protonic conductivities but strong resistance to densification. X-ray diffraction studies on sintered specimens of BaCe0.85Y0.1503-6 show multi-phase formation which was found to show dependence upon powder synthesis method. Doping with SrTiO3 suppresses multi-phase formation and enhances grain growth. Conductivity measurements in temperature range of 200 to 1000 C were performed by ac impedance spectroscopy under dry and wet conditions. Sintering behavior, phase formation and conductivity results will be reported.

SPS Fabrication of Tungsten-Rhenium Alloys in Support of NTR Fuels Development

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

Jonathan A. Webb; Indrajit Charit; Cory Sparks

Abstract. Tungsten metal slugs were fabricated via Spark Plasma Sintering (SPS) of powdered metals at temperatures ranging from 1575 K to 1975 K and hold times of 5 minutes to 30 minutes, using powders with an average diameter of 7.8 ?m. Sintered tungsten specimens were found to have relative densities ranging from 83 % to 94 % of the theoretical density for tungsten. Consolidated specimens were also tested for their Vickers Hardness Number (VHN), which was fitted as a function of relative density; the fully consolidated VHN was extrapolated to be 381.45 kg/mm2. Concurrently, tungsten and rhenium powders with averagemore » respective diameters of 0.5 ?m and 13.3 ?m were pre-processed either by High-Energy-Ball-Milling (HEBM) or by homogeneous mixing to yield W-25at.%Re mixtures. The powder batches were sintered at temperatures of 1975 K and 2175 K for hold times ranging from 0 minutes to 60 minutes yielding relative densities ranging from 94% to 97%. The combination of HEBM and sintering showed a significant decrease in the inter-metallic phases compared to that of the homogenous mixing and sintering.« less

Effect of reinforcement phase on the mechanical property of tungsten nanocomposite synthesized by spark plasma sintering

DOE PAGES

Lee, Jin -Kyu; Kim, Song -Yi; Ott, Ryan T.; ...

2015-07-15

Nanostructured tungsten composites were fabricated by spark plasma sintering of nanostructured composite powders. The composite powders, which were synthesized by mechanical milling of tungsten and Ni-based alloy powders, are comprised of alternating layers of tungsten and metallic glass several hundred nanometers in size. The mechanical behavior of the nanostructured W composite is similar to pure tungsten, however, in contrast to monolithic pure tungsten, some macroscopic compressive plasticity accompanies the enhanced maximum strength up to 2.4 GPa by introducing reinforcement. As a result, we have found that the mechanical properties of the composites strongly depend on the uniformity of the nano-grainedmore » tungsten matrix and reinforcement phase distribution.« less

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.

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

Copper-polydopamine composite derived from bioinspired polymer coating

DOE PAGES

Zhao, Yao; Wang, Hsin; Qian, Bosen; ...

2018-04-01

Metal matrix composites with nanocarbon phases, such carbon nanotube (CNT) and graphene, have shown potentials to achieve improved mechanical, thermal, and electrical properties. However, incorporation of these nanocarbons into the metal matrix usually involves complicated processes. Here, this study explored a new processing method to fabricate copper (Cu) matrix composite by coating Cu powder particles with nanometer-thick polydopamine (PDA) thin films and sintering of the powder compacts. For sintering temperatures between 300°C and 750°C, the Cu-PDA composite samples showed higher electrical conductivity and thermal conductivity than the uncoated Cu samples, which is likely related to the higher mass densities ofmore » the composite samples. After being sintered at 950°C, the thermal conductivity of the Cu-PDA sample was approximately 12% higher than the Cu sample, while the electrical conductivity did not show significant difference. On the other hand, Knoop micro-hardness values were comparable between the Cu-PDA and Cu samples sintered at the same temperatures.« less

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloy

NASA Astrophysics Data System (ADS)

Mori, A.; Mamiya, H.; Ohnuma, M.; Ilavsky, J.; Ohishi, K.; Woźniak, Jarosław; Olszyna, A.; Watanabe, N.; Suzuki, J.; Kitazawa, H.; Lewandowska, M.

2018-04-01

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and alloy contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small-angle X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 °C. Sintering at 1000 °C for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128 nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloys

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

Kowalska-Mori, A.; Mamiya, H.; Ohnuma, M.

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 ºC. Sintering at 1000 ºC for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128more » nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.« less

Co-melting technology in resource recycling of sludge derived from stone processing.

PubMed

Hu, Shao-Hua; Hu, Shen-Chih; Fu, Yen-Pei

2012-12-01

Stone processing sludge (SPS) is a by-product of stone-processing wastewater treatment; it is suitable for use as a raw material for making artificial lightweight aggregates (ALWAs). In this study, boric acid was utilized as a flux to lower sintering temperature. The formation of the viscous glassy phase was observed by DTA curve and changes in XRD patterns. Experiments were conducted to find the optimal combination of sintering temperature, sintering time, and boric acid dosage to produce an ALWA of favorable characteristics in terms of water absorption, bulk density, apparent porosity, compressive strength and weight loss to satisfy Taiwan's regulatory requirements for construction and insulation materials. Optimal results gave a sintering temperature of 850 degrees C for 15 min at a boric acid dosage of 15% by weight of SPS. Results for ALWA favorable characteristics were: 0.21% (water absorption), 0.35% (apparent porosity), 1.67 g/cm3 (bulk density), 66.94 MPa (compressive strength), and less than 0.1% (weight loss).

Co-melting technology in resource recycling of sludge derived from stone processing.

PubMed

Hu, Shao-Hua; Hu, Shen-Chih; Fu, Yen-Pei

2012-12-01

Stone processing sludge (SPS) is a by-product of stone-processing wastewater treatment; it is suitable for use as a raw material for making artificial lightweight aggregates (ALWAs). In this study, boric acid was utilized as a flux to lower sintering temperature. The formation of the viscous glassy phase was observed by DTA curve and changes in XRD patterns. Experiments were conducted to find the optimal combination of sintering temperature, sintering time, and boric acid dosage to produce an ALWA of favorable characteristics in terms of water absorption, bulk density, apparent porosity, compressive strength and weight loss to satisfy Taiwan's regulatory requirements for construction and insulation materials. Optimal results gave a sintering temperature of 850 °C for 15 min at a boric acid dosage of 15 % by weight of SPS. Results for ALWA favorable characteristics were: 0.21 % (water absorption), 0.35 %(apparent porosity), 1.67 g/cm3 (bulk density), 66.94 MPa (compressive strength), and less than 0.1% (weight loss). [Box: see text].

Improved silicon nitride for advanced heat engines

NASA Technical Reports Server (NTRS)

Yeh, H. C.; Wimmer, J. M.; Huang, H. H.; Rorabaugh, M. E.; Schienle, J.; Styhr, K. H.

1985-01-01

The AiResearch Casting Company baseline silicon nitride (92 percent GTE SN-502 Si sub 3 N sub 4 plus 6 percent Y sub 2 O sub 3 plus 2 percent Al sub 2 O sub 3) was characterized with methods that included chemical analysis, oxygen content determination, electrophoresis, particle size distribution analysis, surface area determination, and analysis of the degree of agglomeration and maximum particle size of elutriated powder. Test bars were injection molded and processed through sintering at 0.68 MPa (100 psi) of nitrogen. The as-sintered test bars were evaluated by X-ray phase analysis, room and elevated temperature modulus of rupture strength, Weibull modulus, stress rupture, strength after oxidation, fracture origins, microstructure, and density from quantities of samples sufficiently large to generate statistically valid results. A series of small test matrices were conducted to study the effects and interactions of processing parameters which included raw materials, binder systems, binder removal cycles, injection molding temperatures, particle size distribution, sintering additives, and sintering cycle parameters.

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloys

DOE PAGES

Kowalska-Mori, A.; Mamiya, H.; Ohnuma, M.; ...

2018-01-17

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 ºC. Sintering at 1000 ºC for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128more » nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.« less

Copper-polydopamine composite derived from bioinspired polymer coating

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

Zhao, Yao; Wang, Hsin; Qian, Bosen

Metal matrix composites with nanocarbon phases, such carbon nanotube (CNT) and graphene, have shown potentials to achieve improved mechanical, thermal, and electrical properties. However, incorporation of these nanocarbons into the metal matrix usually involves complicated processes. Here, this study explored a new processing method to fabricate copper (Cu) matrix composite by coating Cu powder particles with nanometer-thick polydopamine (PDA) thin films and sintering of the powder compacts. For sintering temperatures between 300°C and 750°C, the Cu-PDA composite samples showed higher electrical conductivity and thermal conductivity than the uncoated Cu samples, which is likely related to the higher mass densities ofmore » the composite samples. After being sintered at 950°C, the thermal conductivity of the Cu-PDA sample was approximately 12% higher than the Cu sample, while the electrical conductivity did not show significant difference. On the other hand, Knoop micro-hardness values were comparable between the Cu-PDA and Cu samples sintered at the same temperatures.« less

Synthesis and Characterization of Hydroxyapatite Powder by Wet Precipitation Method

NASA Astrophysics Data System (ADS)

Cahyaningrum, S. E.; Herdyastuty, N.; Devina, B.; Supangat, D.

2018-01-01

Hydroxyapatite is main inorganic component of the bone with formula Ca10(PO4)6(OH)2. Hydroxyapatite can be used as substituted bone biomaterial because biocompatible, non toxic, and osteoconductive. In this study, hydroxyapatite is synthesized using wet precipitation method from egg shell. The product was sintered at different temperatures of 800°C to 1000°C to improve its crystallinity. The hydroxyapatite was characterized by X-ray analysis, Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FTIR) to reveal its phase content, morphology and types of bond present within it. The analytical results showed hydroxyapatite had range in crystallinity from 85.527 to 98.753%. The analytical functional groups showed that presence of functional groups such as OH, (PO4)3 2-, and CO3 2- that indicated as hydroxyapatite. The result of characterization SEM indicated that hydroxyapatite without sintering and HAp sintering at 800 °C were irregular shape without pore. The best hydroxyapatite with temperature sintering at 900 °C showed oval shaped with pores without agglomerated.

Co-Precipitation Synthesis of Gadolinium Aluminum Gallium Oxide (GAGG) via Different Precipitants

NASA Astrophysics Data System (ADS)

Sun, Yan; Yang, Shenghui; Zhang, Ye; Jiang, Jun; Jiang, Haochuan

2014-02-01

In order to obtain a uniform transparent ceramic scintillator, well-dispersed fine starting powders with high-purity, small grain size, spherical morphology and high sinter-ability are necessary. In this study, Ce3+ doped gadolinium aluminum gallium garnet Gd3Al3Ga2O12 (GAGG) powders were synthesized by the co-precipitation method. NH4OH, NH4HCO3 and the mixed solution of NH4OH and NH4HCO3 were used as precipitants, respectively. The precursor composition, phase formation process, microstructure, morphology, particle size distribution and luminescent properties of obtained GAGG powders were measured. The results show that powders prepared using the mixed precipitant exhibit the best microstructural morphology, good sinter-ability and highest luminescent intensity. Pure GAGG polycrystalline powders could be obtained at about 950°C for 1.5 h and the average size of the particles is about 50 nm. The photoluminescence spectrum shows a strong green-yellow emission near 540 nm.

Mechanical Property Evaluation at Elevated Temperatures of Sintered Beta Silicon Carbide.

DTIC Science & Technology

1986-03-01

a co mercial- sintered product. 1-7 It is fabricated from a submicron (beta) silicon carbide powder with small additions (f-0.5 wtZ each) of goron and...majority of the material-is beta silicon carbide with a small percentage of the alpha phase and a small amount of graphite. In a parallel study being...surface-connected porosity (Figures 12 and 13). This porosity was often an area of small interconnected porosity and not necessarily a discrete void

Anisotropy and Microstructure of High-Coercivity Rare Earth Iron Permanent Magnets

DTIC Science & Technology

1989-06-01

still necessary in order to achieve a high quality permanent magnet with an opera - ting temperature up to 150C. Acces1O, FO" NTIS CRA&i DTIC TAB... China , Crucible Materials and Unocal, USA) under different processing and post-sintering heat treatment conditions. Doped, "two-phase" Nd:0FebaiBe...mation for the nucleation field Ho (8,10). -15- 4.5 Al-substituted magnets These sintered magnets were produced by the Institute of Physics in Bejing

Effect of Annealing Treatments on the Microstructure, Mechanical Properties and Corrosion Behavior of Direct Metal Laser Sintered Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Xu, Yangzi; Lu, Yuan; Sundberg, Kristin L.; Liang, Jianyu; Sisson, Richard D.

2017-05-01

An experimental investigation on the effects of post-annealing treatments on the microstructure, mechanical properties and corrosion behavior of direct metal laser sintered Ti-6Al-4V alloys has been conducted. The microstructure and phase evolution as affected by annealing treatment temperature were examined through scanning electron microscopy and x-ray diffraction. The tensile properties and Vickers hardness were measured and compared to the commercial Grade 5 Ti-6Al-4V alloy. Corrosion behavior of the parts was analyzed electrochemically in simulated body fluid at 37 °C. It was found out that the as-printed parts mainly composed of non-equilibrium α' phase. Annealing treatment allowed the transformation from α' to α phase and the development of β phase. The tensile test results indicated that post-annealing treatment could improve the ductility and decrease the strength. The as-printed Ti-6Al-4V part exhibits inferior corrosion resistance compared to the commercial alloy, and post-annealing treatment can reduce its susceptibility to corrosion by reducing the two-phase interface area.

Effect of oxygen content of Nd-Fe-B sintered magnet on grain boundary diffusion process of DyH2 dip-coating

NASA Astrophysics Data System (ADS)

Bae, Kyoung-Hoon; Lee, Seong-Rae; Kim, Hyo-Jun; Lee, Min-Woo; Jang, Tae-Suk

2015-11-01

We investigated the effect of oxygen content on the microstructural and magnetic properties of a DyH2 dip-coated Nd-Fe-B sintered magnet. When the magnet had a low oxygen content (1500 ppm), the volume and size of the rare-earth-rich oxide (Nd-Dy-O) phase was reduced, and a uniform and continuous thin Nd-rich grain boundary phase (GBP) was well developed. The grain boundary diffusion depth of Dy increased from 200 to 350 μm with decreasing oxygen content from ˜3000 to 1500 ppm. The coercivity of the low-oxygen magnet increased from 19.98 to 23.59 kOe after grain boundary diffusion process (GBDP) while the remanence reduction was minimized. The formation of an fcc-NdOx Nd-rich phase in the high-oxygen magnet hindered the formation of a Nd-rich triple-junction phase and GBP. In contrast, a metallic dhcp-Nd phase, which was closely related to coercivity enhancement after GBDP, was formed in the low-oxygen magnet.

Effects of particle size and forming pressure on pore properties of Fe-Cr-Al porous metal by pressureless sintering

NASA Astrophysics Data System (ADS)

Koo, Bon-Uk; Yi, Yujeong; Lee, Minjeong; Kim, Byoung-Kee

2017-03-01

With increased hydrogen consumption in ammonia production, refining and synthesis, fuel cells and vehicle industries, development of the material components related to hydrogen production is becoming an important factor in industry growth. Porous metals for fabrication of hydrogen are commonly known for their relative excellence in terms of large area, lightness, lower heat capacity, high toughness, and permeability. Fe-Cr-Al alloys not only have high corrosion resistance, heat resistance, and chemical stability but also ductility, excellent mechanical properties. In order to control powder size and sintering temperature effects of Fe-Cr-Al porous metal fabrication, Fe-Cr-Al powder was classified into 25-35 μm, 35-45 μm, 45-75 μm using an auto shaking sieve machine and then classified Fe-Cr-Al powders were pressed into disk shapes using a uniaxial press machine and CIP. The pelletized Fe-Cr-Al specimens were sintered at various temperatures in high vacuum. Properties such as pore size, porosity, and air permeability were evaluated using perm-porosimetry. Microstructure and phase changes were observed with SEM and XRD. Porosity and relative density were proportionated to increasing sintering temperature. With sufficient sintering at increasing temperatures, the pore size is expected to be gradually reduced. Porosity decreased with increasing sintering temperature and gradually increased necking of the powder.

Effects of flux concentrations and sintering temperature on dental porcelain

NASA Astrophysics Data System (ADS)

Ghose, Polash; Gafur, Md. Abdul; Das, Sujan Kumar; Ranjan Chakraborty, Shyamal; Mohsin, Md.; Deb, Arun Kumar; Rakibul Qadir, Md.

2014-02-01

In this study, samples of dental porcelain bodies have been made by using the materials collected from selected deposits employing different mixing proportions of clay, quartz and feldspar. Dental porcelain ceramics have been successfully fabricated by using the sintering technique together with some Na2CO3 additive. The dental porcelain powder has been pressed into pellets at first and subsequently sintered at 700, 800, 900, 1000 and 1100 °C for 2 h. The physical and mechanical properties of the prepared samples have been investigated. The sintering behavior of the fired samples has been evaluated by bulk density, linear shrinkage, water absorption and apparent porosity measurements. This study includes the evaluation of the Vickers's microhardness by microhardness tester. Phase analysis and microstructural study have been performed by XRD and optical microscope respectively. Optical properties have been investigated using UV-visible spectroscopy. Influence of firing conditions on leucite formation, densification and microstructural development of the sintered samples has been investigated. It has been found that the choice of sintering temperature is one of the key factors in controlling leucite crystallization in dental porcelain ceramics. It has also been found that the flux concentration of material and the effect of temperature on preparation of dental porcelain contribute to the firing shrinkage and hardness, which has been found to increase with the increase of treatment temperature.

Improved silicon carbide for advanced heat engines

NASA Technical Reports Server (NTRS)

Whalen, T. J.; Winterbottom, W. L.

1986-01-01

Work performed to develop silicon carbide materials of high strength and to form components of complex shape and high reliability is described. A beta-SiC powder and binder system was adapted to the injection molding process and procedures and process parameters developed capable of providing a sintered silicon carbide material with improved properties. The initial effort has been to characterize the baseline precursor materials (beta silicon carbide powder and boron and carbon sintering aids), develop mixing and injection molding procedures for fabricating test bars, and characterize the properties of the sintered materials. Parallel studies of various mixing, dewaxing, and sintering procedures have been carried out in order to distinguish process routes for improving material properties. A total of 276 MOR bars of the baseline material have been molded, and 122 bars have been fully processed to a sinter density of approximately 95 percent. The material has a mean MOR room temperature strength of 43.31 ksi (299 MPa), a Weibull characteristic strength of 45.8 ksi (315 MPa), and a Weibull modulus of 8.0. Mean values of the MOR strengths at 1000, 1200, and 14000 C are 41.4, 43.2, and 47.2 ksi, respectively. Strength controlling flaws in this material were found to consist of regions of high porosity and were attributed to agglomerates originating in the initial mixing procedures. The mean stress rupture lift at 1400 C of five samples tested at 172 MPa (25 ksi) stress was 62 hours and at 207 MPa (30 ksi) stress was 14 hours. New fluid mixing techniques have been developed which significantly reduce flaw size and improve the strength of the material. Initial MOR tests indicate the strength of the fluid-mixed material exceeds the baseline property by more than 33 percent.

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.

Structural, microstructural, dielectric and ferroelectric properties of lead free Ba0.85Ca0.15Zr0.1Ti0.9O3 ceramic

NASA Astrophysics Data System (ADS)

Sharma, Sarita; Sharma, Hakikat; Negi, N. S.

2018-05-01

Lead free Ba0.85Ca0.15Zr0.1Ti0.9O3(BCTZ) ceramic has been synthesized by sol-gel method. Properties of material are studied at different sintering temperatures for 5 hours. Structural and microstructural properties are analyzed by using X-ray diffractrometer (XRD) and scanning electron microscopy (SEM) at annealing temperature of 850°C and 1050°C XRD pattern confirm the perovskite structure of the material without any unwanted phases crystalinity increased with increase of sintering temperature so as roughness and porosity is decreased as shown by SEM micrographs. There is large improvement in density with rise of sintering temperature which also leads to drastic change in ferroelectric and dielectric properties.

Environmentally benign processing of YAG transparent wafers

NASA Astrophysics Data System (ADS)

Yang, Yan; Wu, Yiquan

2015-12-01

Transparent yttrium aluminum garnet (YAG) wafers were successfully produced via aqueous tape casting and vacuum sintering techniques using a new environmentally friendly binder, a copolymer of isobutylene and maleic anhydride with the commercial name ISOBAM (noted as ISOBAM). Aqueous YAG slurries were mixed by ball-milling, which was followed by de-gassing and tape casting of wafers. The final YAG green tapes were homogenous and flexible, and could be bent freely without cracking. After the drying and sintering processes, transparent YAG wafers were achieved. The microstructures of both the green tape and vacuum-sintered YAG ceramic were observed by scanning electronic microscopy (SEM). Phase compositions were examined by X-ray diffraction (XRD). Optical transmittance was measured in UV-VIS regions with the result that the transmittance is 82.6% at a wavelength of 800 nm.

The impact of sintering temperature on structural, morphological and thermoelectric properties of zinc titanate nanocrystals

NASA Astrophysics Data System (ADS)

Chandrasekaran, P.; Murugu thiruvalluvan, T. M. V.; Arivanandhan, M.; Jayakumari, T.; Anandan, P.

2017-07-01

The effect of sintering temperature and Ti:Zn ratio of precursor solutions on the structural, morphological and thermoelectric properties of Zinc titanate (TZO) nanocrystals have been investigated. TZO nanocrystals were synthesized by changing the molar ratio of precursors of Zn and Ti sources by sol-gel method. The synthesized materials were sintered at different temperatures and the formation of multi phases of TZO were analysed by x-ray diffraction studies. The morphological properties and composition of TZO samples were studied by FESEM, TEM and XPS analysis. The thermoelectric properties of the TZO have been studied by measuring the Seebeck coefficient of the materials at various temperature. It was observed that the Seebeck coefficient of TZO sample increases with increasing Zn content in the sample especially at high temperature.

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

NASA Astrophysics Data System (ADS)

Kapoor, Seema; Batra, Uma; Kohli, Suchita

2011-12-01

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

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.

Osteoblast adhesion on novel machinable calcium phosphate/lanthanum phosphate composites for orthopedic applications.

PubMed

Ergun, Celaletdin; Liu, Huinan; Webster, Thomas J

2009-06-01

Lanthanum phosphate (LaPO(4), LP) was combined with either hydroxyapatite (HA) or tricalcium phosphate (TCP) to form novel composites for orthopedic applications. In this study, these composites were prepared by wet chemistry synthesis and subsequent powder mixing. These HA/LP and TCP/LP composites were characterized in terms of phase stability and microstructure evolution during sintering using X-ray diffraction (XRD) and scanning electron microscopy (SEM). Their machinability was evaluated using a direct drilling test. For HA/LP composites, LP reacted with HA during sintering and formed a new phase, Ca(8)La(2)(PO(4))(6)O(2), as a reaction by-product. However, TCP/LP composites showed phase stability and the formation of a weak interface between TCP and LP machinability when sintered at 1100 degrees C, which is crucial for achieving desirable properties. Thus, these novel TCP/LP composites fulfilled the requirements for machinability, a key consideration for manufacturing orthopedic implants. Moreover, the biocompatibility of these novel LP composites was studied, for the first time, in this paper. In vitro cell culture tests demonstrated that the LP and its composites supported osteoblast (bone-forming cell) adhesion similar to natural bioceramics (such as HA and TCP). In conclusion, these novel LP composites should be further studied and developed for more effectively treating bone related diseases or injuries. 2008 Wiley Periodicals, Inc.

The Influence of Milling and Spark Plasma Sintering on the Microstructure and Properties of the Al7075 Alloy

PubMed Central

Málek, Přemysl; Minárik, Peter; Novák, Pavel; Průša, Filip

2018-01-01

The compact samples of an Al7075 alloy were prepared by a combination of gas atomization, high energy milling, and spark plasma sintering. The predominantly cellular morphology observed in gas atomized powder particles was completely changed by mechanical milling. The continuous-like intermetallic phases present along intercellular boundaries were destroyed; nevertheless, a small amount of Mg(Zn,Cu,Al)2 phase was observed also in the milled powder. Milling resulted in a severe plastic deformation of the material and led to a reduction of grain size from several µm into the nanocrystalline region. The combination of these microstructural characteristics resulted in abnormally high microhardness values exceeding 300 HV. Consolidation through spark plasma sintering (SPS) resulted in bulk samples with negligible porosity. The heat exposition during SPS led to precipitation of intermetallic phases from the non-equilibrium microstructure of both gas atomized and milled powders. SPS of the milled powder resulted in a recrystallization of the severely deformed structure. An ultra-fine grained structure (grain size close to 500 nm) with grains divided primarily by high-angle boundaries was formed. A simultaneous release of stored deformation energy and an increase in the grain size caused a drop of microhardness to values close to 150 HV. This value was retained even after annealing at 425 °C. PMID:29614046

Sintering of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) with/without SrTiO3 Dopant

NASA Technical Reports Server (NTRS)

Dynys, F.; Sayir, A.; Heimann, P. J.

2004-01-01

The perovskite composition, BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta), displays excellent protonic conduction at high temperatures making it a desirable candidate for hydrogen separation membranes. This paper reports on the sintering behavior of BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders doped with SrTiO3. Two methods were used to synthesize BaCe(sub 0.85)Y(sub 0.15)O(sub 3-delta) powders: (1) solid state reaction and (2) wet chemical co-precipitation. Co-precipitated powder crystallized into the perovskite phase at 1000 C for 4 hrs. Complete reaction and crystallization of the perovskite phase by solid state was achieved by calcining at 1200 C for 24 hrs. Solid state synthesis produced a coarser powder with an average particle size of 1.3 microns and surface area of 0.74 sq m/g. Co-precipitation produced a finer powder with a average particle size of 65 nm and surface area of 14.9 sq m/g. Powders were doped with 1, 2, 5, and 10 mole % SrTiO3. Samples were sintered at 1450 C, 1550 C and 1650 C. SrTiO3 enhances sintering, optimal dopant level is different for powders synthesized by solid state and co-precipitation. Both powders exhibit similar grain growth behavior. Dopant levels of 5 and 10 mole % SrTiO3 significantly enhances the grain size.

Copper stabilization in beneficial use of waterworks sludge and copper-laden electroplating sludge for ceramic materials.

PubMed

Tang, Yuanyuan; Chan, Siu-Wai; Shih, Kaimin

2014-06-01

A promising strategy for effectively incorporating metal-containing waste materials into a variety of ceramic products was devised in this study. Elemental analysis confirmed that copper was the predominant metal component in the collected electroplating sludge, and aluminum was the predominant constituent of waterworks sludge collected in Hong Kong. The use of waterworks sludge as an aluminum-rich precursor material to facilitate copper stabilization under thermal conditions provides a promising waste-to-resource strategy. When sintering the mixture of copper sludge and the 900 °C calcined waterworks sludge, the CuAl2O4 spinel phase was first detected at 650 °C and became the predominant product phase at temperatures higher than 850 °C. Quantification of the XRD pattern using the Rietveld refinement method revealed that the weight of the CuAl2O4 spinel phase reached over 50% at 850 °C. The strong signals of the CuAl2O4 phase continued until the temperature reached 1150 °C, and further sintering initiated the generation of the other copper-hosting phases (CuAlO2, Cu2O, and CuO). The copper stabilization effect was evaluated by the copper leachability of the CuAl2O4 and CuO via the prolonged leaching experiments at a pH value of 4.9. The leaching results showed that the CuAl2O4 phase was superior to the CuAlO2 and CuO phases for immobilizing hazardous copper over longer leaching periods. The findings clearly indicate that spinel formation is the most crucial metal stabilization mechanism when sintering multiphase copper sludge with aluminum-rich waterworks sludge, and suggest a promising and reliable technique for reusing both types of sludge waste for ceramic materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

The effect of aging treatment on the fracture toughness and impact strength of injection molded Ni-625 superalloy parts

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

Özgün, Özgür, E-mail: oozgun@bingol.edu.tr; Yılmaz, Ramazan; Özkan Gülsoy, H.

In this study, the effect of aging heat treatment on fracture toughness and impact strength of Ni-625 superalloy fabricated by using powder injection molding (PIM) method was examined. After a feedstock was prepared by mixing the prealloyed Ni-625 superalloy powder, which was fabricated by gas atomisation, with a polymeric binder system and then it was granulated, it was shaped through the use of injection. The molded specimens were sintered at 1300 °C for 3 h after a two-stage debinding process. Once the sintered specimens were treated in the solution at 1150 °C for 2 h, they were quenched. Aging treatmentmore » was performed by keeping specimens at 745 °C for 22 h. Fracture toughness and impact tests were performed on sintered and aged specimens. Microstructure examinations were performed by using optical microscope, scanning electron microscope, and transmission electron microscope. The results revealed that aging heat treatment led to the formation of some carbides and intermetallic phases in the microstructure. While the hardness of the aged specimens increased due to these phases, their fracture toughness and impact strength values decreased. - Highlights: • Ni-625 superalloy components were produced by means of powder injection molding. • The produced components were subjected to aging treatment. • Aging process provided approximately 50% increase in the hardness of components. • Intermetallic precipitates, carbides and TCP phases occurred within the aged parts. • Fracture toughness and impact strength values decreased due to the hard phases.« less

Relation between the microstructure and the electromagnetic properties of BaTiO3/Ni0.5Zn0.5Fe2O4 ceramic composite

NASA Astrophysics Data System (ADS)

Xiao, Bin; Tang, Yu; Ma, Guodong; Ma, Ning; Du, Piyi

2015-06-01

The microstructure-property relation in ferroelectric/ferromagnetic composite is investigated in detail, exemplified by typical sol-gel-derived 0.3BTO/0.7NZFO ceramic composite. The effect of microstructural factors including intergrain connectivity, grain size and interfaces on the dielectric and magnetic properties of the composite prepared by conventional ceramic method and three-step sintering method is discussed both experimentally and theoretically. It reveals that the dielectric behavior of the composite is controlled by a hybrid dielectric process that combines the contribution of Debye-like dipoles and Maxwell-Wagner (M-W or interfacial) polarization. Enhanced dielectric, magnetic and conductive behaviors appear in the composite with better intergrain connectivity and larger grain size derived by sol-gel route and three-step sintering method. The effective permittivity contributed by Debye-like dipoles exhibits a value of ~130,000 in three-step sintered composite, which is almost the same as that in conventionally sintered one, but that contributed by M-W response is much smaller in the former. Compared with conventionally prepared samples, the relaxation time ( τ) is 3.476 × 10-6 s, about one order of magnitude smaller, and the dc electrical conductivity is 3.890 × 10-3 S/m, one order of magnitude higher in three-step sintered composite. The minimum dielectric loss reveals almost the same (~0.2) for all samples, but shows distinguishable difference in low-frequency region. Meanwhile, an initial permeability of 84, twice as large as that of conventionally prepared composite and 56 % the value of single-phased NZFO ferrite (~150), and a saturation magnetization of 63.5 emu/g, 32 % higher than that of conventional one and approximately 84 % the value of single-phased NZFO ferrite (~76 emu/g), appear simultaneously in three-step sintered composite with larger grain size and better intergrain connectivity. It is clear that the discovery is helpful for establishing a more explicit view on the physics of multi-functional composite materials, while the composite with optimized microstructure is beneficial to be used as a high-performance material.

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.)

Understanding proton-conducting perovskite interfaces using atom probe tomography

NASA Astrophysics Data System (ADS)

Clark, Daniel R.

Proton-conducting ceramics are under intense scientific investigation for a number of exciting applications, including fuel cells, electrolyzers, hydrogen separation membranes, membrane reactors, and sensors. However, commercial application requires deeper understanding and improvement of proton conductivity in these materials. It is well-known that proton conductivity in these materials is often limited by highly resistive grain boundaries (GBs). While these conductivity-limiting GBs are still not well understood, it is hypothesized that their blocking nature stems from the formation of a positive (proton-repelling) space-charge zone. Furthermore, it has been observed that the strength of the blocking behavior can change dramatically depending on the fabrication process used to make the ceramic. This thesis applies laser-assisted atom probe tomography (LAAPT) to provide new insights into the GB chemistry and resulting space-charge behavior of BaZr0.9Y0.1O 3--delta (BZY10), a prototypical proton-conducting ceramic. LAAPT is an exciting characterization technique that allows for three-dimensional nm-scale spatial resolution and very high chemical resolution (up to parts-per-million). While it is challenging to quantitatively apply LAAPT to complex, multi-cation oxide materials, this thesis successfully develops a method to accurately quantify the stoichiometry of BZY10 and maintain minimal quantitative cationic deviation at a laser energies of approximately 10--20 pJ. With the analysis technique specifically optimized for BZY10, GB chemistry is then examined for BZY10 samples prepared using four differing processing methods: (1) spark plasma sintering (SPS), (2) conventional sintering using powder prepared by solid-state reaction followed by high-temperature annealing (HT), (3) conventional sintering using powder prepared by solid-state reaction with NiO used as a sintering aid (SSR-Ni), and (4) solid-state reactive sintering directly from BaCO3, ZrO2, and Y2O3 precursor powders with 1 wt. % NiO as a reactive sintering aid (SSRS-Ni). It is observed that oxygen depletion (oxygen-vacancy accumulation) occurs at all GBs. Segregation of the constituent cations, Ba, Zr, and Y, is found to be variable across all samples although zirconium depletion and yttrium accumulation are most prevalent. Additionally, impurities such as Al, Fe, Mg, Ni, Si, and Sr are shown to generally accumulate at the GBs. Finally, LAAPT-derived GB chemistry data is combined with electrostatic modeling to examine the electronic structure of a BZY10 GB, revealing significant non-uniformity in the space charge region at the GB with an average space-charge potential of approximately 580 mV, extending 5--7 nm in width from the GB core. This result demonstrates how LAAPT can not only be used to further understand the role of GB chemistry within oxide materials, but can also be used to examine the electronic structure, allowing for the possibility of engineering these interfaces to improve their electrochemical performance.

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

Formation of Fine B2/ β + O Structure and Enhancement of Hardness in the Aged Ti2AlNb-Based Alloys Prepared by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Li, Mengchen; Cai, Qi; Liu, Yongchang; Ma, Zongqing; Wang, Zumin; Huang, Yuan; Li, Huijun

2017-09-01

Ti2AlNb-based alloys synthesized at 1223 K (950 °C) by spark plasma sintering were aged at 973 K, 1023 K, 1073 K, and 1123 K (700 °C, 750 °C, 800 °C, and 850 °C), respectively. Phase composition, microstructure, and microhardness of the aged alloys were investigated in this study. Equiaxed O grains and Widmanstätten B2/ β + O laths were formed in the aged alloys, and the microhardness was improved in contrast with the spark plasma-sintered alloy without aging. The microhardness relies largely on the O-phase content, as well as the length and width of the O laths. In particular, complete Widmanstätten B2/ β + O laths, with locally finely dispersed β precipitates, were obtained in the alloy aged at 1073 K (800 °C), and the alloy exhibited the best microhardness performance. Such fine structure is due to the temperature-dependent transformations Oequiaxed→Oprimary + B2/ β primary, Oprimary→Osecondary + B2/ β secondary, and B2/ β primary→O.

Rapidly sintering of interconnected porous Ti-HA biocomposite with high strength and enhanced bioactivity.

PubMed

Zhang, L; He, Z Y; Zhang, Y Q; Jiang, Y H; Zhou, R

2016-10-01

In this work, interconnected porous Ti-HA biocomposites with enhanced bioactivity, high porosity and compressive strength were prepared by spark plasma sintering (SPS) and space holder method. Pore characteristics, mechanical properties, corrosion behaviors and in vitro bioactivity of the porous Ti-HA were investigated. Results showed that porous Ti-HA with 5-30wt% HA contents possessed not only low elastic modulus of 8.2-15.8GPa (close to that of human bone) but also high compressive strength (86-388MPa). Although the HA partially decomposed and formed secondary phases, the sintered porous Ti-HA can still be good bioactivity. The homogeneity and the thickness of apatite layer increased significantly with the increase of HA. But with the thickness of apatite layer increased, micro-cracks appeared on the surface of porous Ti-30%HA. A model was built to discuss the current distribution and sintering mechanism of HA on Ti matrix during SPS process. It indicated that the excessive addition of HA would deteriorate the sintering quality, thus decreasing the mechanical properties and corrosion resistance. However, the combination of interconnected pore characteristics, low elastic modulus, high compressive strength and enhanced bioactivity might make porous Ti-HA biocomposites prepared by SPS a promising candidate for hard tissue implants. Copyright © 2016 Elsevier B.V. All rights reserved.

Sintering and Microstructure of BaTiO3 Nano Particles Synthesized by Molten Salt Method.

PubMed

Lee, Chang-Hyun; Shin, Hyo-Soon; Yeo, Dong-Hun; Ha, Gook-Hyun; Nahm, Sahn

2016-05-01

In order to establish thinner dielectric layers in thick film electronic components such as MLCC (Multilayer ceramic capacitor), BaTiO3 nanoparticles have been utilized. However, studies on the synthesis of nanoparticles smaller than 20 nm, the characteristics of the BaTiO3 powder, and the powder's sintering are lacking. Therefore, this paper aims to synthesize BaTiO3 particles smaller than 20 nm by using the molten salt method and evaluate the microstructure and dielectric properties by varying the sintering temperature from 750 degrees C to 1200 degrees C. Through the molten salt method and by using KOH-KCl mixed salt, 20 nm BaTiO3 powder was synthesized at a low temperature of 150 degrees C. Sintering the pellets formed from the synthesized 20 nm BaTiO3 nano powder led to the observation of an unusual phenomenon where the particles grew to approximate sizes below 850 degrees C where densification progressed. At sintering temperatures above 950 degrees C, particles that expanded into rod shapes were observed and these particles were identified to be unreacted TiO2 based on the results of the EDX (Energy Dispersive X-ray Spectroscopy) analysis and phase analysis results.

Influence of Sintering Temperature on Mechanical and Physical properties of Mill Scale based Bipolar Plates for PEMFC

NASA Astrophysics Data System (ADS)

Khaerudini, Deni S.; Berliana, Rina; Prakoso, Gatra B.; Insiyanda, Dita R.; Alva, Sagir

2018-03-01

This work concerns the utilization of mill scale, a by-product of iron and steel formed during the hot rolling of steel, as a potential material for use as bipolar plates in proton exchange membrane fuel cells (PEMFCs). On the other hand, mill scale is considered a very rich in iron source having characteristic required such as for current collector in bipolar plate and would significantly contribute to lower the overall cost of PEMFC based fuel cell systems. In this study, the iron reach source of mill scale powder, after sieving of 150 mesh, was mechanically alloyed with the aluminium source containing 30 wt.% using a shaker mill for 3 h. The mixed powders were then pressed at 300 MPa and sintered at various temperatures of 400, 450 and 500 °C for 1 h under inert gas atmosphere. The structural changes of powder particles during mechanical alloying and after sintering were studied by x-ray diffractometry, scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX), microhardness measurement, and density - porosity analysis. The details of the performance variation of three different sintering conditions can be preliminary explained by the metallographic and crystallographic structure and phase analysis as well as sufficient mechanical strength of the sintered materials was presented in this report.

The Influence of Sintering Temperature on the Microstructure and Thermoelectric Properties of n-Type Bi2Te3- x Se x Nanomaterials

NASA Astrophysics Data System (ADS)

Du, Y.; Cai, K. F.; Li, H.; An, B. J.

2011-05-01

Pure Bi2Te3 and Bi2Se3 nanopowders were hydrothermally synthesized, and n-type Bi2Te3- x Se x bulk samples were prepared by hot pressing a mixture of Bi2Te3 and Bi2Se3 nanopowders at 623 K, 648 K or 673 K and 80 MPa in vacuum. The phase composition of the powders and bulk samples were characterized by x-ray diffraction. The morphology of the powders was examined by transmission electron microscopy. The microstructure and composition of the bulk samples were characterized by field-emission scanning electron microscopy and energy-dispersive x-ray spectroscopy, respectively. The density of the samples increased with sintering temperature. The samples were somewhat oxidized, and the amount of oxide (Bi2TeO5) present increased with sintering temperature. The samples consisted of sheet-like grains with a thickness less than 100 nm. Seebeck coefficient, electrical conductivity, and thermal conductivity of the samples were measured from room temperature up to 573 K. Throughout the temperature range investigated, the sample sintered at 623 K had a higher power factor than the samples sintered at 648 K or 673 K.

Processing, characterization, and in vitro/in vivo evaluations of powder metallurgy processed Ti-13Nb-13Zr alloys.

PubMed

Bottino, Marco C; Coelho, Paulo G; Henriques, Vinicius A R; Higa, Olga Z; Bressiani, Ana H A; Bressiani, José C

2009-03-01

This article presents details of processing, characterization and in vitro as well as in vivo evaluations of powder metallurgy processed Ti-13Nb-13Zr samples with different levels of porosity. Sintered samples were characterized for density, crystalline phases (XRD), and microstructure (SEM and EDX). Samples sintered at 1000 degrees C showed the highest porosity level ( approximately 30%), featuring open and interconnected pores ranging from 50 to 100 mum in diameter but incomplete densification. In contrast, samples sintered at 1300 and 1500 degrees C demonstrated high densification with 10% porosity level distributed in a homogeneous microstructure. The different sintering conditions used in this study demonstrated a coherent trend that is increase in temperature lead to higher sample densification, even though densification represents a drawback for bone ingrowth. Cytotoxicity tests did not reveal any toxic effects of the starting and processed materials on surviving cell percentage. After an 8-week healing period in rabbit tibias, the implants were retrieved, processed for nondecalcified histological evaluation, and then assessed by backscattered electron images (BSEI-SEM) and EDX. Bone growth into the microstructure was observed only in samples sintered at 1000 degrees C. Overall, a close relation between newly formed bone and all processed samples was observed. (c) 2008 Wiley Periodicals, Inc.

Cold sintering and electrical characterization of lead zirconate titanate piezoelectric ceramics

NASA Astrophysics Data System (ADS)

Wang, Dixiong; Guo, Hanzheng; Morandi, Carl S.; Randall, Clive A.; Trolier-McKinstry, Susan

2018-01-01

This paper describes a cold sintering process for Pb(Zr,Ti)O3 ceramics and the associated processing-property relations. Pb(Zr,Ti)O3 has a very small, incongruent solubility that is a challenge during cold sintering. To circumvent this, a Pb(NO3)2 solution was used as the transient liquid phase. A bimodal lead zirconate titanate powder was densified to a relative density of 89% by cold sintering at 300 °C and 500 MPa. After the cold sintering step, the permittivity was 200, and the dielectric loss was 2.0%. A second heat-treatment involving a 3 h anneal at 900 °C increased the relative density to 99%; the resulting relative dielectric permittivity was 1300 at room temperature and 100 kHz. The samples showed well-defined ferroelectric hysteresis loops, having a remanent polarization of 28 μC/cm2. On poling, the piezoelectric coefficient d33 was ˜200 pC/N. With a 700 °C 3 h post-annealing, samples show a lower room temperature relative permittivity (950 at 100 kHz), but a 24 h hold time at 700 °C produces ceramics where there is an improved relative dielectric constant (1050 at 100 kHz).

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

Synthesis and characterization of nanocrystalline Nd{sup 3+}-doped gadolinium scandium aluminum garnet powders by a gel-combustion method

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

Su, Jing, E-mail: zlj007@126.com; Miao, Ju-hong; Xu, Lin-hua

2012-07-15

Graphical abstract: The graph shows the emission spectra (λ{sub ex} = 808 nm) of 1 at.% Nd:GSAG powders sintered at different temperatures for 3 h. Compared with the powder sintered at 900 °C, the PL intensity of the powder sintered at 1000 °C decreased significantly. The changes in the PL intensity should mainly due to the crystallinity and dispersion of the powders. Highlights: ► We synthesized Nd:GSAG nano-powders by gel-combustion method successfully. ► We analyzed the structure and the morphology of the heat-treated products. ► We studied the optical characteristics of Nd:GSAG nano-powders. -- Abstract: Nd{sup 3+}-doped gadolinium scandium aluminummore » garnet (Nd:GSAG) precursor was synthesized by a gel combustion method using metal nitrates and citric acid as raw materials. The structure and morphology of the precursor and the sintered powders were studied by means of X-ray diffraction (XRD), infrared spectroscopy (IR) and transmission electron microscopy (TEM). The results showed that the precursor transformed into pure GSAG polycrystalline phase at about 800 °C, and the powders sintered at 800–1000 °C were well-dispersed with average particle sizes in the range of 30–80 nm. Optical properties of Nd:GSAG nano-powders were characterized by using photoluminescence spectroscopy. The highest photoluminescence intensity was achieved for the powder sintered at 900 °C.« less

Mechanical properties of {beta}-SiC pressureless sintered with Al{sub 2}O{sub 3} additions

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

Mulla, M.A.; Krstic, V.D.

1994-01-01

Mechanical properties of pressureless sintered SiC with Al{sub 2}O{sub 3}addition were measured. The increase in fracture toughness and strength is attributed to the presence of a liquid phase which results in the formation of platelets of an {alpha}-SiC. The highest values for flexural strength and toughness were measured on samples with {approximately}10%Al{sub 2}O{sub 3} addition. Pull out, crack bridging and crack deflection are identified as the major strengthening and toughening mechanisms.

Processing, Microstructures and Properties of a Dual Phase Precipitation-Hardening PM Stainless Steel

NASA Astrophysics Data System (ADS)

Schade, Christopher

To improve the mechanical properties of PM stainless steels in comparison with their wrought counterparts, a PM stainless steel alloy was developed which combines a dual-phase microstructure with precipitation-hardening. The use of a mixed microstructure of martensite and ferrite results in an alloy with a combination of the optimum properties of each phase, namely strength and ductility. The use of precipitation hardening via the addition of copper results in additional strength and hardness. A range of compositions was studied in combination with various sintering conditions to determine the optimal thermal processing to achieve the desired microstructure. The microstructure could be varied from predominately ferrite to one containing a high percentage of martensite by additions of copper and a variation of the sintering temperature before rapid cooling. Mechanical properties (transverse rupture strength (TRS), yield strength, tensile strength, ductility and impact toughness) were measured as a function of the v/o ferrite in the microstructure. A dual phase alloy with the optimal combination of properties served as the base for introducing precipitation hardening. Copper was added to the base alloy at various levels and its effect on the microstructure and mechanical properties was quantified. Processing at various sintering temperatures led to a range of microstructures; dilatometry was used utilized to monitor and understand the transformations and the formation of the two phases. The aging process was studied as a function of temperature and time by measuring TRS, yield strength, tensile strength, ductility, impact toughness and apparent hardness. It was determined that optimum aging was achieved at 538°C for 1h. Aging at slightly lower temperatures led to the formation of carbides, which contributed to reduced hardness and tensile strength. As expected, at the peak aging temperature, an increase in yield strength and ultimate tensile strength as well as apparent hardness was found. Aging also lead to an unexpected and concurrent increase in ductility and impact toughness. The alloys also showed an increase in strain hardening on aging. The increase in ductility varied with the v/o martensite in the microstructure and was shown to occur after short time intervals at the optimum aging temperature. Compressive strength measurements revealed that the increase in ductility was due to the relaxation of residuals stresses that occur when the high temperature austenite transforms to martensite in the dual phase microstructure. The specific volume of martensite is much larger than that of austenite so that when the transformation takes place, a compressive stress is induced in the ferrite. In the sintered state, the residual stress leads to a higher work hardening rate in tension. When the alloy is aged, the work hardening rate is reduced and the ductility is increased compared with the sintered state, even though aging increases the strength and apparent hardness.

Subcritical CO2 Sintering of Microspheres of Different Polymeric Materials to Fabricate Scaffolds for Tissue Engineering

PubMed Central

Bhamidipati, Manjari; Sridharan, BanuPriya; Scurto, Aaron M; Detamore, Michael S.

2013-01-01

The aim of this study was to use CO2 at sub-critical pressures as a tool to sinter 3D, macroporous, microsphere-based scaffolds for bone and cartilage Tissue Engineering Porous scaffolds composed of ~200 µm microspheres of either poly(lactic-co-glycolic acid) (PLGA) or polycaprolactone (PCL) were prepared using dense phase CO2 sintering, which were seeded with rat bone marrow mesenchymal stromal cells (rBMSCs), and exposed to either osteogenic (PLGA, PCL) or chondrogenic (PLGA) conditions for 6 weeks. Under osteogenic conditions, the PLGA constructs produced over an order of magnitude more calcium than the PCL constructs, whereas the PCL constructs had far superior mechanical and structural integrity (125 times stiffer than PLGA constructs) at week 6, along with twice the cell content of the PLGA constructs. Chondrogenic cell performance was limited in PLGA constructs, perhaps as a result of the polymer degradation rate being too high. The current study represents the first long-term culture of CO2-sintered microsphere-based scaffolds, and has established important thermodynamic differences in sintering between the selected formulations of PLGA and PCL, with the former requiring adjustment of pressure only, and the latter requiring the adjustment of both pressure and temperature. Based on more straightforward sintering conditions and more favorable cell performance, PLGA may be the material of choice for microspheres in a CO2 sintering application, although a different PLGA formulation with the encapsulation of growth factors, extracellular matrix-derived nanoparticles, and/or buffers in the microspheres may be advantageous for achieving a more superior cell performance than observed here. PMID:24094202

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

Lee, Min Ho; Rhyee, Jong-Soo, E-mail: jsrhyee@khu.ac.kr

We investigated the thermoelectric properties of PbTe/Ag{sub 2}Te bulk composites, synthesized by hand milling, mixing, and hot press sintering. From x-ray diffraction and energy dispersive x-ray spectroscopy measurements, we observed Ag{sub 2}Te phase separation in the PbTe matrix without Ag atom diffusion. In comparison with previously reported pseudo-binary (PbTe){sub 1−x}(Ag{sub 2}Te){sub x} composites, synthesized by high temperature phase separation, the PbTe/Ag{sub 2}Te bulk composites fabricated with a low temperature phase mixing process give rise to p-type conduction of carriers with significantly decreased electrical conductivity. This indicates that Ag atom diffusion in the PbTe matrix changes the sign of the Seebeckmore » coefficient to n-type and also increases the carrier concentration. Effective p-type doping with low temperature phase separation by mixing and hot press sintering can enhance the thermoelectric performance of PbTe/Ag{sub 2}Te bulk composites, which can be used as a p-type counterpart of n-type (PbTe){sub 1−x}(Ag{sub 2}Te){sub x} bulk composites.« less

Sinter-vein correlations at Buckskin Mountain, National district, Humboldt County, Nevada

USGS Publications Warehouse

Vikre, P.G.

2007-01-01

At Buckskin Mountain (elev 2,650 m, 8,743 ft), Humboldt County, Nevada, a hydrothermal system, imposed on a middle Miocene volcanic sequence with contrasting permeabilities and tensile strengths, produced alteration assemblages controlled by elevation, from Hg-mineralized sinter to subjacent precious metal veins over a vertical distance exceeding 790 m. Sinter and epiclastic deposits, interpreted to be remnant paleosurface basinal strata enclosed by 16.6 to 16.1 Ma rhyolites, overlie older volcaniclastic basinal deposits and were part of a regional fluvial-lacustrine system developed among ca. 16 to 12 Ma basalt-rhyolite eruptive centers throughout the northern Great Basin. Because of contrasting erosional resistance among altered and unaltered rocks, Buckskin Mountain represents inverse topography with sinter and silicified epiclastic deposits at the summit. Sinter and veins, correlated by common elements, similar mineralogy, age constraints, textures, S isotope compositions, and fluid inclusion microthermometry, were deposited by sinter-vein fluid, the first of two sequential hydrothermal fluid regimes that evolved in response to magmatism, tectonism, hydrology, and topography. Thermal quenching of distally derived sinter-vein fluid in planar conduits caused deposition of banded quartz-silicate-selenide-sulfide veins ???270 to > 440 m below sinter at 16.1 Ma; vei??ns were initially enveloped by zoned selvages of proximal K-feldspar + K-mica + quartz + pyrite and distal illite + chlorite + calcite + pyrite. Mixing of sinter-vein fluid with local meteoric water in saturated basinal deposits caused deposition of silica, Hg-Se-S-Cl minerals, and precious metals in sinter and epiclastic deposits. Elevated ???Se/???S in sinter-vein fluid, and the relatively large stability fields of reduced aqueous selenide species in the temperature range of 250?? to <100??C, enabled (but was not the cause of) codeposition of selenide-sulfide minerals and common element associations in veins and sinter. Acid-sulfate fluid of the second fluid regime was derived from oxidation of H2S and other volatiles exsolved from sinter-vein fluid. Acid-sulfate fluid produced (1) a subhorizontal zone of partially leached basinal deposits and rhyolite from the paleosurface to a depth of ???60 m, and (2) laterally pervasive zones, ???100 to 200 m thick, of quartz + alunite ?? hematite and quartz + kaolinite + pyrite in volcaniclastic deposits immediately beneath partially leached rocks, but this fluid did not decompose selenide-sulfide-precious metal phases in sinter. Paragenetically late vein and wall-rock assemblages, including marcasite + pyrite, calcite, and kaolinite-replaced K minerals, record deeper transition of sinter-vein fluid into acid-sulfate fluid in vein conduits. This transition occurred as regional subsidence, manifested by the Goosey Lake depression immediately east of Buckskin Mountain, lowered the pieziometric surface at Buckskin Mountain, terminated sinter deposition, and caused boiling and/or degassing of sinter-vein fluid. The timing of subsidence is recorded by a decrease in alunite ages, from ca. 15.8 to 15.6 Ma, with depth below sinter. Lateral replacement of sinter and partially leached epiclastic deposits and rhyolite by opal-A marks the termination of the two hydrothermal regimes that lasted ???0.5 m.y. and followed rhyolitic volcanism of similar duration. Veins and sinter display textures that attest to plastic deformation, spalling, and gravitational settling, and indicate fluid-flow direction, velocity, and density stratification which, with conduit topology, may have influenced precious metal tenor in the veins. Components of sinter and veins were transported as colloids, formed in supersaturated sinter-vein fluid, that aggregated or coagulated as incompetent gelatinous layers in shallow pools and in underlying, near-vertical conduits in rhyolite and initially crystallized as opal and chalcedony. The low thermal conductivity of ho

Oxidation resistant slurry coating for carbon-based materials

NASA Technical Reports Server (NTRS)

Smialek, J. L.; Rybicki, G. C. (Inventor)

1985-01-01

An oxidation resistant coating is produced on carbon-base materials, and the same processing step effects an infiltration of the substrate with silicon containing material. The process comprises making a slurry of nickel and silicon powders in a nitrocellulose lacquer, spraying onto the graphite or carbon-carbon substrate, and sintering in vacuum to form a fused coating that wets and covers the surface as well as penetrates into the pores of the substrate. Optimum wetting and infiltration occurs in the range of Ni-60 w/o Si to Ni-90 w/o Si with deposited thicknesses of 25-100 mg/sq. cm. Sintering temperatures of about 1200 C to about 1400 C are used, depending on the melting point of the specific coating composition. The sintered coating results in Ni-Si intermetallic phases and SiC, both of which are highly oxidation resistant.

Spinel formation for stabilizing simulated nickel-laden sludge with aluminum-rich ceramic precursors.

PubMed

Shih, Kaimin; White, Tim; Leckie, James O

2006-08-15

The feasibility of stabilizing nickel-laden sludge from commonly available Al-rich ceramic precursors was investigated and accomplished with high nickel incorporation efficiency. To simulate the process, nickel oxide was mixed alternatively with gamma-alumina, corundum, kaolinite, and mullite and was sintered from 800 to 1480 degrees C. The nickel aluminate spinel (NiAl2O4) was confirmed as the stabilization phase for nickel and crystallized with efficiencies greater than 90% for all precursors above 1250 degrees C and 3-h sintering. The nickel-incorporation reaction pathways with these precursors were identified, and the microstructure and spinel yield were investigated as a function of sintering temperature with fixed sintering time. This study has demonstrated a promising process for forming nickel spinel to stabilize nickel-laden sludge from a wide range of inexpensive ceramic precursors, which may provide an avenue for economically blending waste metal sludges via the building industry processes to reduce the environmental hazards of toxic metals. The correlation of product textures and nickel incorporation efficiencies through selection of different precursors also provides the option of tailoring property-specific products.

Room Temperature Electrochemical Sintering of Zn Microparticles and Its Use in Printable Conducting Inks for Bioresorbable Electronics.

PubMed

Lee, Yoon Kyeung; Kim, Jeonghyun; Kim, Yerim; Kwak, Jean Won; Yoon, Younghee; Rogers, John A

2017-10-01

This study describes a conductive ink formulation that exploits electrochemical sintering of Zn microparticles in aqueous solutions at room temperature. This material system has relevance to emerging classes of biologically and environmentally degradable electronic devices. The sintering process involves dissolution of a surface passivation layer of zinc oxide in CH 3 COOH/H 2 O and subsequent self-exchange of Zn and Zn 2+ at the Zn/H 2 O interface. The chemical specificity associated with the Zn metal and the CH 3 COOH/H 2 O solution is critically important, as revealed by studies of other material combinations. The resulting electrochemistry establishes the basis for a remarkably simple procedure for printing highly conductive (3 × 10 5 S m -1 ) features in degradable materials at ambient conditions over large areas, with key advantages over strategies based on liquid phase (fusion) sintering that requires both oxide-free metal surfaces and high temperature conditions. Demonstrations include printed magnetic loop antennas for near-field communication devices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microstructure and microwave magnetic properties of Low-Firing Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4 ferrite

NASA Astrophysics Data System (ADS)

Xie, Fei; Jia, Lijun; Shen, Qihang; Qiu, Hua; Zhang, Huaiwu

2018-03-01

Low firing temperature and excellent gyromagnetic properties such as high remanence square ratio and narrow ferromagnetic resonance line width are required for the application in nonreciprocal microwave ferrite devices based on low temperature cofired ceramics (LTCC) technology. In this research, Bi2O3-Li2CO3 mixture was introduced as the sintering agent to lower the sintering temperature of Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4 ferrite. The influence of Bi2O3-Li2CO3 mixture upon the phase composition, composite microstructures and gyromagnetic properties of LiZnTiMn ferrite sintered at low temperature has been investigated for LTCC integration applications. With a proper amount of Bi2O3-Li2CO3 mixture, the sintering temperature of LiZnTiMn ferrite successfully reduced to below 900°C from 1100°C without degradation of magnetic properties, meanwhile, both of saturation flux density and remanence square ratio were increased.

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.

Compaction and sintering behaviors of a Nd-Fe-B permanent magnet alloy

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

Chin, T.; Hung, M.; Tsai, D.

1988-11-15

Extensive x-ray diffraction (XRD) and magnetic measurements were done on Nd/sub 15/ Fe/sub 77/ B/sub 8/ magnet alloy green compacts after cold isostatic pressing following a pulsed 2-T field (CIP) and die-pressing under a static 1.2-T perpendicular field (DP1) or parallel field (DP2), and on those after sintering. An alignment factor F, through the calculation of the integrated diffraction intensity ratio of the XRD patterns, was adopted as the effectiveness of magnetic alignment. At the green compact state, DP1 has the best alignment while CIP the worst. However, after sintering the alignment factor was such that CIP>DPI>DP2, the same ordermore » as the magnetic properties. Three mechanisms were proposed for the evolution of the alignment factor at different stages of sintering, i.e., that both the appearance of a liquid phase at low temperatures and preferred grain growth at high temperatures enhance F, while recrystallization at intermediate temperatures deteriorates F. CIP results in less-defect green compact, hence less recrystallization, leading to better resultant alignment« less

Enhancement of structural and magnetic properties of M-type hexaferrite permanent magnet based on synthesis temperature

NASA Astrophysics Data System (ADS)

Anjum, Safia; Sehar, Fatima; Mustafa, Zeeshan; Awan, M. S.

2018-01-01

The main purpose of this research work is to develop the single domain magnetic particles of M-type barium hexaferrite (BaFe12O19) using oxide precursors employing conventional powder metallurgy technique. The phase formation and magnetic performance of the powders and magnets will be optimized by adjusting calcination and sintering temperatures. The synthesis of M-type barium hexaferrite was carried out in two sections. A series of four samples have been prepared by initial wet mixed powders calcined at different temperatures, i.e., 750, 850, 950 and 1050 °C. On the basis of structural analysis, the sample calcined at 950 °C has been selected and further divided into four parts to sintered them at 1100, 1150, 1200 and 1250 °C. The structural measurements depict the confirmation of M-type barium hexaferrite structure. SEM micrographs show the hexagonal-shaped grains. The abrupt decrease in coercivity for the sample sintered at 1250 °C has been seen which may be due to high sintering temperature, at which the particles have multi-domain properties.

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.

Nickel/ruthenium catalyst and method for aqueous phase reactions

DOEpatents

Elliott, D.C.; Sealock, J.L.

1998-09-29

A method of hydrogenation is described using a catalyst in the form of a plurality of porous particles wherein each particle is a support having nickel metal catalytic phase or reduced nickel deposited thereon in a first dispersed phase and an additional ruthenium metal deposited onto the support in a second dispersed phase. The additional ruthenium metal is effective in retarding or reducing agglomeration or sintering of the nickel metal catalytic phase thereby increasing the life time of the catalyst during hydrogenation reactions. 2 figs.

Nickel/ruthenium catalyst and method for aqueous phase reactions

DOEpatents

Elliott, Douglas C.; Sealock, John L.

1998-01-01

A method of hydrogenation using a catalyst in the form of a plurality of porous particles wherein each particle is a support having nickel metal catalytic phase or reduced nickel deposited thereon in a first dispersed phase and an additional ruthenium metal deposited onto the support in a second dispersed phase. The additional ruthenium metal is effective in retarding or reducing agglomeration or sintering of the nickel metal catalytic phase thereby increasing the life time of the catalyst during hydrogenation reactions.

Catalyst and method for aqueous phase reactions

DOEpatents

Elliott, Douglas C.; Hart, Todd R.

1999-01-01

The present invention is a catalyst in the form of a plurality of porous particles wherein each particle is a support having nickel metal catalytic phase or reduced nickel deposited thereon in a first dispersed phase and an additional metal deposited onto the support in a second dispersed phase. The additional metal is effective in retarding or reducing agglomeration or sintering of the nickel metal catalytic phase without substantially affecting the catalytic activity, thereby increasing the life time of the catalyst.

Solution-derived sodalite made with Si- and Ge-ethoxide precursors for immobilizing electrorefiner salt

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

Riley, Brian J.; Lepry, William C.; Crum, Jarrod V.

Chlorosodalite has the general form of Na8(AlSiO4)6Cl2 and this paper describes experiments conducted to synthesize sodalite to immobilize a mixed chloride salt using solution-based techniques. Sodalites were made using different Group IV contributions from either Si(OC2H5)4 or Ge(OC2H5)4, NaAlO2, and a simulated spent electrorefiner salt solution containing a mixture of alkali, alkaline earth, and lanthanide chlorides. Additionally, 6 glass binders at low loadings of 5 mass% were evaluated as sintering aids for the consolidation process. The approach of using the organic Group IV additives can be used to produce large quantities of sodalite at room temperature and shows promise overmore » a method where colloidal silica is used as the silica source. However, the small particle sizes inhibited densification during pressure-less sintering.« less

Nanophase materials assembled from clusters

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

Siegel, R.W.

1992-02-01

The preparation of metal and ceramic atom clusters by means of the gas-condensation method, followed by their in situ collection and consolidation under high-vacuum conditions, has recently led to the synthesis of a new class of ultrafine-grained materials. These nanophase materials, with typical average grain sizes of 5 to 50 nm and, hence, a large fraction of their atoms in interfaces, exhibit properties that are often considerably improved relative to those of conventional materials. Furthermore, their synthesis and processing characteristics should enable the design of new materials with unique properties. Some examples are ductile ceramics that can be formed andmore » sintered to full density at low temperatures without the need for binding or sintering aids, and metals with dramatically increased strength. The synthesis of these materials is briefly described along with what is presently known of their structure and properties. Their future impact on materials science and technology is also considered.« less

Improved silicon nitride for advanced heat engines

NASA Technical Reports Server (NTRS)

Yeh, H. C.; Wimmer, J. M.

1986-01-01

Silicon nitride is a high temperature material currently under consideration for heat engine and other applications. The objective is to improve the net shape fabrication technology of Si3N4 by injection molding. This is to be accomplished by optimizing the process through a series of statistically designed matrix experiments. To provide input to the matrix experiments, a wide range of alternate materials and processing parameters was investigated throughout the whole program. The improvement in the processing is to be demonstrated by a 20 percent increase in strength and a 100 percent increase in the Weibull modulus over that of the baseline material. A full characterization of the baseline process was completed. Material properties were found to be highly dependent on each step of the process. Several important parameters identified thus far are the starting raw materials, sinter/hot isostatic pressing cycle, powder bed, mixing methods, and sintering aid levels.

Improved Tubulars for Better Economics in Deep Gas Well Drilling using Microwave Technology

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

Dinesh Agrawal; Paul Gigl; Mahlon Dennis

2006-02-01

The objective of the research program has been to improve the rate-of-penetration in deep hostile environments by improving the life cycle and performance of coiled-tubing, an important component of a deep well drilling system for oil and gas exploration. The current process of the manufacture long tubular steel products consists of shaping the tube from flat strip, welding the seam and sections into lengths that can be miles long, and coiling onto reels. However, the welds, that are a weak point, now limit the performance of the coil tubing. This is not only from a toughness standpoint but also frommore » a corrosion standpoint. By utilizing the latest developments in the sintering of materials with microwave energy and powder metal extrusion technology for the manufacture of seamless coiled tubing and other tubular products, these problems can be eliminated. The project is therefore to develop a continuous microwave process to sinter continuously steel tubulars and butt-join them using microwave/induction process. The program started about three years ago and now we are in the middle of Phase II. In Phase I (which ended in February 2005) a feasibility study of the extrusion process of steel powder and continuously sinter the extruded tubing was conducted. The research program has been based on the development of microwave technology to process tubular specimens of powder metals, especially steels. The existing microwave systems at the Materials Research Laboratory (MRL) and Dennis Tool Company (DTC) were suitably modified to process tubular small specimens. The precursor powder metals were either extruded or cold isostatically pressed (CIP) to form tubular specimens. After conducting an extensive and systematic investigation of extrusion process for producing long tubes, it was determined that there were several difficulties in adopting extrusion process and it cannot be economically used for producing thousands of feet long green tubing. Therefore, in the Phase II the approach was modified to the microwave sintering combined with Cold Isostatic Press (CIP) and joining (by induction or microwave). This process can be developed into a semi-continuous sintering process if the CIP can produce parts fast enough to match the microwave sintering rates. This report summarizes the progress made to-date in this new approach. The final steel composition matching with the Quality tubing's QT-16Cr80 was short listed and used for all experiments. Bonding experiments using 4 different braze powders were conducted and the process optimized to obtain high degree of bonding strength. For fabrication of green tubulars a large CIP unit was acquired and tested. This equipment is located at the Dennis Tool facility in Houston. Microwave sintering experiments for continuous processing of the CIPed tubes are under progress in order to identify the optimum conditions. There have been some reproducibility problems and we are at present working to resolve these problems.« less

Effect of processing conditions on microstructural features in Mn–Si sintered steels

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

Oro, Raquel, E-mail: raqueld@chalmers.se; Hryha, Eduard, E-mail: hryha@chalmers.se; Campos, Mónica, E-mail: campos@ing.uc3m.es

2014-09-15

Sintering of steels containing oxidation sensitive elements is possible if such elements are alloyed with others which present lower affinity for oxygen. In this work, a master alloy powder containing Fe–Mn–Si–C, specifically designed to create a liquid phase during sintering, has been used for such purpose. The effect of processing conditions such as sintering temperature and atmosphere was studied with the aim of describing the microstructural evolution as well as the morphology and distribution of oxides in the sintered material, evaluating the potential detrimental effect of such oxides on mechanical properties. Chemical analyses, metallography and fractography studies combined with X-raymore » photoelectron spectroscopy analyses on the fracture surfaces were used to reveal the main mechanism of fracture and their correlation with the chemical composition of the different fracture surfaces. The results indicate that the main mechanism of failure in these steels is brittle fracture in the surrounding of the original master alloy particles due to degradation of grain boundaries by the presence of oxide inclusions. Mn–Si oxide inclusions were observed on intergranular decohesive facets. The use of reducing atmospheres and high sintering temperatures reduces the amount and size of such oxide inclusions. Besides, high heating and cooling rates reduce significantly the final oxygen content in the sintered material. A model for microstructure development and oxide evolution during different stages of sintering is proposed, considering the fact that when the master alloy melts, the liquid formed can dissolve some of the oxides as well as the surface of the surrounding iron base particles. - Highlights: • Oxide distribution in steels containing oxidation-sensitive elements • Mn, Si introduced in a master alloy powder, mixed with a base iron powder • Selective oxidation of Mn and Si on iron grain boundaries • Decohesive fracture caused by degradation of grain boundaries by oxide inclusions • Reducing agents efficient at low temperatures critical for avoiding oxide inclusions.« less

The Effect of MnO2 Content and Sintering Atmosphere on The Electrical Properties of Iron Titanium Oxide NTC Thermistors using Yarosite

NASA Astrophysics Data System (ADS)

Wiendartun; Gustaman Syarif, Dani

2017-02-01

The effect of MnO2 content and sintering atmosphere on the characteristics of Fe2TiO5 ceramics for Negative Thermal Coefficient (NTC) thermistors by using Fe2O3 derived from yarosite has been studied. The ceramics were produced by pressing a homogeneous mixture of Fe2O3, TiO2 and MnO2 (0-2.0 w/o) powders in appropriate proportions to produce Fe2TiO5 based ceramics and sintering the pressed powder at 1100-1200°C for 3 hours in air, O2 and N2 gas. Electrical characterization was done by measuring electrical resistivity of the sintered ceramics at various temperatures from 30°C to 200°C. Microstructure and structural analyses were also carried out by using an scanning electron microscope (SEM) and x-ray diffraction (XRD). The XRD data showed that the pellets crystallize in orthorhombic. The presence of second phase could not be identified from the XRD analyses. The SEM images showed that the grain size of pellet ceramics increase with increasing of MnO2 addition, and the grains size of the ceramic sintered in oxygen gas is smaller than sintered in nitrogen gas. Electrical data showed that the value of room temperature resistance (RRT) tend to decrease with respect to the increasing of MnO2 addition and the pellet ceramics sintered in oxygen gas had the largest thermistor constant (B), activation energy (Ea), sensitivity (α) and room temperature resistance (RRT), compared to the sintered in nitrogen gas. From the electrical characteristics data, it was known that the electrical characteristics of the Fe2TiO5 pellet ceramics followed the NTC characteristic. The fabricated Fe2TiO5 ceramics have thermistor constants (B = 2207-7145K). This can be applied as temperature sensor, and will fulfill the market requirement.

Investigating the addition of SiO₂-CaO-ZnO-Na₂O-TiO₂ bioactive glass to hydroxyapatite: Characterization, mechanical properties and bioactivity.

PubMed

Yatongchai, Chokchai; Placek, Lana M; Curran, Declan J; Towler, Mark R; Wren, Anthony W

2015-11-01

Hydroxyapatite (Ca10(PO4)6(OH)2) is widely investigated as an implantable material for hard tissue restoration due to its osteoconductive properties. However, hydroxyapatite in bulk form is limited as its mechanical properties are insufficient for load-bearing orthopedic applications. Attempts have been made to improve the mechanical properties of hydroxyapatite, by incorporating ceramic fillers, but the resultant composite materials require high sintering temperatures to facilitate densification, leading to the decomposition of hydroxyapatite into tricalcium phosphate, tetra-calcium phosphate and CaO phases. One method of improving the properties of hydroxyapatite is to incorporate bioactive glass particles as a second phase. These typically have lower softening points which could possibly facilitate sintering at lower temperatures. In this work, a bioactive glass (SiO2-CaO-ZnO-Na2O-TiO2) is incorporated (10, 20 and 30 wt%) into hydroxyapatite as a reinforcing phase. X-ray diffraction confirmed that no additional phases (other than hydroxyapatite) were formed at a sintering temperature of 560 ℃ with up to 30 wt% glass addition. The addition of the glass phase increased the % crystallinity and the relative density of the composites. The biaxial flexural strength increased to 36 MPa with glass addition, and there was no significant change in hardness as a function of maturation. The pH of the incubation media increased to pH 10 or 11 through glass addition, and ion release profiles determined that Si, Na and P were released from the composites. Calcium phosphate precipitation was encouraged in simulated body fluid with the incorporation of the bioactive glass phase, and cell culture testing in MC-3T3 osteoblasts determined that the composite materials did not significantly reduce cell viability. © The Author(s) 2015.

Spark plasma sintering synthesis of Ni1-xZnxFe2O4 ferrites: Mössbauer and catalytic study

NASA Astrophysics Data System (ADS)

Velinov, Nikolay; Manova, Elina; Tsoncheva, Tanya; Estournès, Claude; Paneva, Daniela; Tenchev, Krassimir; Petkova, Vilma; Koleva, Kremena; Kunev, Boris; Mitov, Ivan

2012-08-01

Nickel-zinc ferrite nanoparticles, Ni1-xZnxFe2O4 (x = 0, 0.2, 0.5, 0.8, 1.0) were prepared by combination of chemical precipitation and spark plasma sintering (SPS) techniques and conventional thermal treatment of the obtained precursors. The phase composition and structural properties of the obtained materials were investigated by X-ray diffraction and Mössbauer spectroscopy and their catalytic activity in methanol decomposition was tested. A strong effect of reaction medium leading to the transformation of ferrites to a complex mixture of different iron containing phases was detected. A tendency of formation of Fe-carbide was found for the samples synthesized by SPS, while predominantly iron-nickel alloys ware registered in TS obtained samples. The catalytic activity and selectivity in methanol decomposition to CO and methane depended on the current phase composition of the obtained ferrites, which was formed by the influence of the reaction medium.

Phase Structures and Magnetic Properties of Graphite Nanosheets and Ni-Graphite Nanocomposite Synthesized by Electrical Explosion of Wire in Liquid

NASA Astrophysics Data System (ADS)

Nguyen, Minh-Thuyet; Kim, Jin-Hyung; Lee, Jung-Goo; Kim, Jin-Chun

2018-03-01

The present work studied on phases and magnetic properties of graphite nanosheets and Ni-graphite nanocomposite synthesized using the electrical explosion of wire (EEW) in ethanol. X-ray diffraction and field emission scanning electron microscope were used to investigate the phases and the morphology of the nanopowders obtained. It was found that graphite nanosheets were absolutely fabricated by EEW with a thickness of 29 nm and 3 μm diameter. The as-synthesized Ni-graphite composite powders had a Ni-coating on the surfaces of graphite sheets. The hysteresis loop of the as-exploded, the hydrogen-treated composite nanopowders and the sintered samples were examined with a vibrating sample magnetometer at room temperature. The Ni-graphite composite exposed the magnetic behaviors which are attributed to Ni component. The magnetic properties of composite had the improvement from 10.2 emu/g for the as-exploded powders to 15.8 emu/g for heat-treated powders and 49.16 emu/g for sintered samples.

Method of melting metals to reduce contamination from crucibles

DOEpatents

Banker, John G.; Wigginton, Hubert L.

1977-01-01

Contamination of metals from crucible materials during melting operations is reduced by coating the interior surface of the crucible with a ceramic non-reactive with the metallic charge and disposing a metal liner formed from a portion of the metallic charge within the coated crucible. The liner protects the ceramic coating during loading of the remainder of the charge and expands against the ceramic coating during heat-up to aid in sintering the coating.

The effect of spark plasma sintering on lithium disilicate glass-ceramics.

PubMed

Al Mansour, Fatima; Karpukhina, Natalia; Grasso, Salvatore; Wilson, Rory M; Reece, Mike J; Cattell, Michael J

2015-10-01

To evaluate the effects of spark plasma sintering (SPS) on the microstructure of lithium disilicate glass-ceramics. IPS e.max CAD glass-ceramic samples were processed using spark plasma sintering (SPS) and conventionally sintered (CS) as a comparison. Specimens were sintered at varying temperatures (T1: 840°C, T2: 820°C, T3: 800°C), heating rates (HR1: 150°C/min, HR2: 300°C/min, HR3: 500°C/min) and pressures (P1: 15MPa, P2: 50MPa, P3: 70MPa). IPS e.max Press glass powder samples were densified at 750 and 800°C (50 or 200MPa pressure). Samples were characterized using XRD, HTXRD, and SEM and quantitative image analysis. There was a significant increase in median crystal size (MCS) between the CS and the SPS T1 groups. A statistical difference (p>0.05) in MCS between SPS T1 and SPS T2 groups was observed. The SPS HR3 sample produced a smaller MCS than the CS, SPS HR1 and HR2 groups (p<0.05). The SPS P3 sample had a reduction in MCS compared with the CS group (p<0.05). XRD of the SPS samples revealed major lithium disilicate/lithium metasilicate phases and minor lithium orthophosphate and cristobalite/quartz phases. Densified IPS e.max Press glass samples resulted in fine fibrils or graduated lithium disilicate crystals. The effects of SPS were used to refine the microstructure of IPS e.max CAD lithium disilicate glass-ceramics. Densification by SPS of IPS e.max Press glass resulted in textured and fine nano-crystalline microstructures. SPS generated glass-ceramic microstructures may have unique properties and could be useful in the production of CAD/CAM materials for dentistry. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Structure and Electrical Properties of Mn-Cu-O Spinels

NASA Astrophysics Data System (ADS)

Bobruk, M.; Durczak, K.; Dąbek, J.; Brylewski, T.

2017-04-01

The study presents the results of structural and electrical conductivity investigations of a Cu1.3Mn1.7O4 spinel obtained using EDTA gel processes. An amorphous gel was synthesized and calcinated for 5 h in air at temperatures of 673, 773, 873, and 973 K. When calcinating the gel at temperatures below 973 K, the obtained powders consisted of two phases—the regular Cu1.5Mn1.5O4 spinel and manganese(III) oxide. At 973 K, Mn2O3 was no longer observed, but a new Mn3O4 phase appeared in addition to the Cu1.5Mn1.5O4 spinel. Green bodies prepared from these powders were sintered for 2 h in air at 1393 K. The obtained sinters had a porosity of around 12% and were composed predominantly of the spinel phase, with minor amounts of Mn3O4 and, in the case of three of four sinters—CuO. Electrical conductivity measurements were taken over the temperature range of 300-1073 K. A change in the character of conductivity of the studied sinters was observed in the range of 400-430 K, and it was associated with an increase in activation energy from 0.20 to 0.56 eV. The electrical conductivity of the studied sinters ranged from 74.8 to 88.4 S cm-1, which makes the Cu1.3Mn1.7O4 material suitable for application as a protective-conducting coating in IT-SOFC ferritic stainless steel interconnects.

Effect of Nd doping on structural, dielectric and thermodynamic properties of PZT (65/35) ceramic

NASA Astrophysics Data System (ADS)

Mohiddon, Md Ahamad; Kumar, Abhishek; Yadav, K. L.

2007-05-01

The influence of neodymium (Nd) addition on the phase formation and dielectric properties of Pb(Zr 0.65Ti 0.35)O 3 composition prepared from mixed oxide method was analyzed. Pellets were sintered in air and PbZrO 3 (PZ) atmosphere separately. Non-perovskite ZrO 2 phase was observed in samples which were sintered in air, also grain size was found to decrease with Nd doping in non-PZ environment samples. Decrease in transition temperature by 80 °C with increasing Nd concentration was observed in both set of samples. Maximum dielectric constant and dielectric losses are found to decrease with Nd doping. Complex impedance analysis revealed that grain boundary resistance increases with Nd doping. Thermodynamic parameters such as change in enthalpy, free energy and change in entropy were studied.

Hydrogen-enabled microstructure and fatigue strength engineering of titanium alloys

NASA Astrophysics Data System (ADS)

Paramore, James D.; Fang, Zhigang Zak; Dunstan, Matthew; Sun, Pei; Butler, Brady G.

2017-02-01

Traditionally, titanium alloys with satisfactory mechanical properties can only be produced via energy-intensive and costly wrought processes, while titanium alloys produced using low-cost powder metallurgy methods consistently result in inferior mechanical properties, especially low fatigue strength. Herein, we demonstrate a new microstructural engineering approach for producing low-cost titanium alloys with exceptional fatigue strength via the hydrogen sintering and phase transformation (HSPT) process. The high fatigue strength presented in this work is achieved by creating wrought-like microstructures without resorting to wrought processing. This is accomplished by generating an ultrafine-grained as-sintered microstructure through hydrogen-enabled phase transformations, facilitating the subsequent creation of fatigue-resistant microstructures via simple heat treatments. The exceptional strength, ductility, and fatigue performance reported in this paper are a breakthrough in the field of low-cost titanium processing.

Hydrogen-enabled microstructure and fatigue strength engineering of titanium alloys

DOE PAGES

Paramore, James D.; Fang, Zhigang Zak; Dunstan, Matthew; ...

2017-02-01

Traditionally, titanium alloys with satisfactory mechanical properties can only be produced via energy-intensive and costly wrought processes, while titanium alloys produced using low-cost powder metallurgy methods consistently result in inferior mechanical properties, especially low fatigue strength. Herein, we demonstrate a new microstructural engineering approach for producing low-cost titanium alloys with exceptional fatigue strength via the hydrogen sintering and phase transformation (HSPT) process. The high fatigue strength presented in this work is achieved by creating wroughtlike microstructures without resorting to wrought processing. This is accomplished by generating an ultrafine-grained as-sintered microstructure through hydrogen-enabled phase transformations, facilitating the subsequent creation of fatigue-resistantmore » microstructures via simple heat treatments. Finally, the exceptional strength, ductility, and fatigue performance reported in this paper are a breakthrough in the field of low-cost titanium processing.« less

Hydrogen-enabled microstructure and fatigue strength engineering of titanium alloys

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

Paramore, James D.; Fang, Zhigang Zak; Dunstan, Matthew

Traditionally, titanium alloys with satisfactory mechanical properties can only be produced via energy-intensive and costly wrought processes, while titanium alloys produced using low-cost powder metallurgy methods consistently result in inferior mechanical properties, especially low fatigue strength. Herein, we demonstrate a new microstructural engineering approach for producing low-cost titanium alloys with exceptional fatigue strength via the hydrogen sintering and phase transformation (HSPT) process. The high fatigue strength presented in this work is achieved by creating wroughtlike microstructures without resorting to wrought processing. This is accomplished by generating an ultrafine-grained as-sintered microstructure through hydrogen-enabled phase transformations, facilitating the subsequent creation of fatigue-resistantmore » microstructures via simple heat treatments. Finally, the exceptional strength, ductility, and fatigue performance reported in this paper are a breakthrough in the field of low-cost titanium processing.« less

Feasible Recycling of Industrial Waste Coal Gangue for Preparation of Mullite Based Ceramic Proppant

NASA Astrophysics Data System (ADS)

Li, Guomin; Ma, Haiqiang; Tian, Yuming; Wang, Kaiyue; Zhou, Yi; Wu, Yaqiao; Zou, Xinwei; Hao, Jianying; Bai, Pinbo

2017-09-01

Industrial waste coal gangue was successfully utilized to prepare the mullite-based ceramic proppants. The experiments involved the pelletizing technology of proppant through intensive mixer and following the sintering process under different temperatures. The crystalline phase, microstructure, density and breakage ratio of the proppants were investigated. The results showed that with the increasing of sintering temperature, the crystalline phases were transformed to rod-like mullite, which formed the cross-linked structure, improving the densification of proppants. Consequently, the breakage ratio under the closure pressure of 35 MPa exhibited declining trend and reached the minimum value of 6.8% at 1450 °C. Owing to the easy preparation, feasible design, low cost and moderate breakage ratio, the mullite-based ceramic proppant prepared by coal gangue and bauxite is promising candidate for fracturing proppants in future applications.

Hydrogen-enabled microstructure and fatigue strength engineering of titanium alloys

PubMed Central

Paramore, James D.; Fang, Zhigang Zak; Dunstan, Matthew; Sun, Pei; Butler, Brady G.

2017-01-01

Traditionally, titanium alloys with satisfactory mechanical properties can only be produced via energy-intensive and costly wrought processes, while titanium alloys produced using low-cost powder metallurgy methods consistently result in inferior mechanical properties, especially low fatigue strength. Herein, we demonstrate a new microstructural engineering approach for producing low-cost titanium alloys with exceptional fatigue strength via the hydrogen sintering and phase transformation (HSPT) process. The high fatigue strength presented in this work is achieved by creating wrought-like microstructures without resorting to wrought processing. This is accomplished by generating an ultrafine-grained as-sintered microstructure through hydrogen-enabled phase transformations, facilitating the subsequent creation of fatigue-resistant microstructures via simple heat treatments. The exceptional strength, ductility, and fatigue performance reported in this paper are a breakthrough in the field of low-cost titanium processing. PMID:28145527

Metal stabilization mechanism of incorporating lead-bearing sludge in kaolinite-based ceramics.

PubMed

Lu, Xingwen; Shih, Kaimin

2012-02-01

The feasibility and mechanism of incorporating simulated lead-laden sludge into low-cost ceramic products was investigated by observing the reaction of lead with two kaolinite-based precursors under sintering conditions. To investigate the phase transformation process of lead, lead oxide (PbO) mixed with a kaolinite or mullite precursor were fired at 500-950°C for 3h. Detailed X-ray diffraction analysis of sintered products revealed that both precursors had crystallochemically incorporated lead into the lead feldspar (PbAl(2)Si(2)O(8)) crystalline structure. By mixing lead oxide with kaolinite, lead feldspar begins to crystallize at 700°C; maximum incorporation of lead into this structure occurred at 950°C. However, two intermediate phases, Pb(4)Al(4)Si(3)O(16) and a polymorph of lead feldspar, were detected at temperatures between 700 and 900°C. By sintering lead oxide with the mullite precursor, lead feldspar was detected at temperatures above 750°C, and an intermediate phase of Pb(4)Al(4)Si(3)O(16) was observed in the temperature range of 750-900°C. This study compared the lead leachabilities of PbO and lead feldspar using a prolonged leaching test (at pH 2.9 for 23d) modified from the toxicity characteristic leaching procedure. The results indicate the superiority of lead feldspar in stabilizing lead and suggest a promising and reliable strategy to stabilize lead in ceramic products. Copyright © 2011 Elsevier Ltd. All rights reserved.

Nanostructural Characters of β-SiC Nanoparticles Prepared from Indonesian Natural Resource using Sonochemical Method

NASA Astrophysics Data System (ADS)

Fuad, A.; Kultsum, U.; Taufiq, A.; Hartatiek; Latifah, E.

2018-04-01

Silicon carbide (SiC) nanoparticles become one of the interesting non-oxide ceramics due to their physical and chemical properties. For an extended period, SiC nanoparticles have been prepared by several methods that usually performed at high temperatures ranging from 1200 - 2000 °C from inexpensive commercial precursors. In this work, we prepared SiC nanoparticles from the low priced precursor of Indonesia natural resource using the sonochemical method at a temperature that is lower than 1000 °C. To produce samples with particular characters, we varied the sintering holding time (1, 10, and 20 hours) and the sintering temperatures (850, 950, and 1050 °C) during the synthesis. The samples were then characterized using XRD, SEM-EDX, TEM, and FTIR. The XRD data analysis showed that the samples have a dominant phase of SiC in the form of β-SiC with a 3C-SiC structure and SiO2 phase in a low composition within a good agreement with the EDX characterization. Interestingly, the sample prepared at the sintering temperature of 850 °C for 1 hour showed a non-crystallite phase. Using a Scherer’s equation, the particles of the samples sized from 13 to 18 nm, which were validated by SEM and TEM images. Furthermore, the FT-IR spectra presented several peaks, i.e., at wavenumbers of 482.2 and 1150 cm-1 representing Si-O-Si bonding and also at 798.5 cm-1 regarding with Si-C bonding.

Effect of grinding and aging on subcritical crack growth of a Y-TZP ceramic.

PubMed

Amaral, Marina; Weitzel, Isabela Sandim Souza Leite; Silvestri, Tais; Guilardi, Luis Felipe; Pereira, Gabriel Kalil Rocha; Valandro, Luiz Felipe

2018-01-01

This study aimed to investigate slow crack growth (SCG) behavior of a zirconia ceramic after grinding and simulated aging with low-temperature degradation (LTD). Complementary analysis of hardness, surface topography, crystalline phase transformation, and roughness were also measured. Disc-shaped specimens (15 mm Ø × 1.2 mm thick, n = 42) of a full-contour Y-TZP ceramic (Zirlux FC, Amherst) were manufactured according to ISO:6872-2008, and then divided into: Ctrl - as-sintered condition; Ctrl LTD - as-sintered after aging in autoclave (134°C, 2 bar, 20 h); G - ground with coarse diamond bur (grit size 181 μm); G LTD - ground and aged. The SCG parameters were measured by a dynamic biaxial flexural test, which determines the tensile stress versus stress rate under four different rates: 100, 10, 1 and 0.1 MPa/s. LTD led to m-phase content increase, as well as grinding (m-phase content: Ctrl - 0%; G - 12.3%; G LTD - 59.9%; Ctrl LTD - 81%). Surface topography and roughness analyses showed that grinding created an irregular surface (increased roughness) and aging did not promote any relevant surface change. There was no statistical difference on surface hardness among different conditions. The control group presented the lowest strength values in all tested rates. Regarding SCG, ground conditions were less susceptible to SCG, delaying its occurrence. Aging (LTD) caused an increase in SCG susceptibility for the as-sintered condition (i.e. G < G LTD < Ctrl < Ctrl LTD).

The effect of Bi substitution on the microstructure and magnetic properties of the Sr0.4Ba0.3La0.3Fe12-xBixO19 hexagonal ferrites

NASA Astrophysics Data System (ADS)

Yang, Yujie; Wang, Fanhou; Liu, Xiansong; Shao, Juxiang; Feng, Shuangjiu; Huang, Duohui; Li, Mingling

2017-01-01

Bi3+ ions doped M-type hexaferrites, Sr0.4Ba0.3La0.3Fe12-xBixO19 (0≤x≤0.7), were prepared by the ceramic process. The phase components of the magnetic powders were investigated by X-ray diffraction. The results show that a single magnetoplumbite phase is obtained for the magnetic powders with x from 0 to 0.2, and BiFeO3 as a second phase appears when Bi content (x)≥0.3. The micrographs of the sintered magnets were observed by a field emission scanning electron microscopy. The sintered magnets are formed of hexagonal-shaped crystals. The magnetic properties of the sintered magnets were measured at room temperature by a permanent magnetic measuring system. The remanence (Br) first increases with x from 0 to 0.2, and then decreases when Bi content (x)≥0.2. The intrinsic coercivity (Hcj) and magnetic induction coercivity (Hcb) firstly decrease quickly with x from 0 to 0.1, and then increase linearly when Bi content (x)≥0.1. The maximum energy product [(BH)max] increases with x from 0 to 0.3, and then decreases when Bi content (x)≥0.3. The ratio Hk/Hcj ratio first increases with Bi content (x) from 0 to 0.4. And the Hk/Hcj ratio decreases when x≥0.4.

Use of free silicon in liquid phase sintering of silicon nitrides and sialons

DOEpatents

Raj, R.; Baik, S.

1985-11-12

This invention relates to the production of improved high density nitrogen based ceramics by liquid-phase densification of silicon nitride or a compound of silicon-nitrogen-oxygen-metal, e.g. a sialon. In the process and compositions of the invention minor amounts of finely divided silicon are employed together with the conventional liquid phase producing additives to enhance the densification of the resultant ceramic. 4 figs.

Use of free silicon in liquid phase sintering of silicon nitrides and sialons

DOEpatents

Raj, Rishi; Baik, Sunggi

1985-11-12

This invention relates to the production of improved high density nitrogen based ceramics by liquid-phase densification of silicon nitride or a compound of silicon-nitrogen-oxygen-metal, e.g. a sialon. In the process and compositions of the invention minor amounts of finely divided silicon are employed together with the conventional liquid phase producing additives to enhance the densification of the resultant ceramic.

CHEMICALLY ACTIVE FLUID-BED PROCESS FOR SULPHUR REMOVAL DURING GASIFICATION OF HEAVY FUEL OIL - SECOND PHASE

EPA Science Inventory

The report describes the second phase of studies on the CAFB process for desulfurizing gasification of heavy fuel oil in a bed of hot lime. The first continuous pilot plant test with U.S. limestone BCR 1691 experienced local stone sintering and severe production of sticky dust du...

High energy X-ray diffraction study of a dental ceramics–titanium functional gradient material prepared by field assisted sintering technique

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

Witte, K., E-mail: kerstin.witte@uni-rostock.de; Bodnar, W.; Schell, N.

A functional gradient material with eleven layers composed of a dental ceramics and titanium was successfully consolidated using field assisted sintering technique in a two-step sintering process. High energy X-ray diffraction studies on the gradient were performed at High Energy Material Science beamline at Desy in Hamburg. Phase composition, crystal unit edges and lattice mismatch along the gradient were determined applying Rietveld refinement procedure. Phase analysis revealed that the main crystalline phase present in the gradient is α-Ti. Crystallinity increases stepwisely along the gradient with a decreasing increment between every next layer, following rather the weight fraction of titanium. Themore » crystal unit edge a of titanium remains approximately constant with a value of 2.9686(1) Å, while c is reduced with increasing amount of titanium. In the layer with pure titanium the crystal unit edge c is constant with a value of 4.7174(2) Å. The lattice mismatch leading to an internal stress was calculated over the whole gradient. It was found that the maximal internal stress in titanium embedded in the studied gradient is significantly smaller than its yield strength, which implies that the structure of titanium along the whole gradient is mechanically stable. - Highlights: • High energy XRD studies of dental ceramics–Ti gradient material consolidated by FAST. • Phase composition, crystallinity and lattice parameters are determined. • Crystallinity increases stepwisely along the gradient following weight fraction of Ti. • Lattice mismatch leading to internal stress is calculated over the whole gradient. • Internal stress in α-Ti embedded in the gradient is smaller than its yield strength.« less