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.

[Influence of compaction pressure and pre-sintering temperature on the machinability of zirconia ceramic].

PubMed

Huang, Huil; Li, Jing; Zhang, Fuqiang; Sun, Jing; Gao, Lian

2011-10-01

In order to make certain the compaction pressure as well as pre-sintering temperature on the machinability of the zirconia ceramic. 3 mol nano-size 3 mol yttria partially stabilized zirconia (3Y-TZP) powder were compacted at different isostatic pressure and sintered at different temperature. The cylindrical surface was traversed using a hard metal tool. Surface and edge quality were checked visually using light stereo microscopy. Pre-sintering temperature had the obviously influence on the machinability of 3Y-TZP. The cutting surface was smooth, and the integrality of edge was better when the pre-sintering temperature was chosen between 800 degrees C to 900 degrees C. Compaction pressure showed only a weak influence on machinability of 3Y-TZP blanks, but the higher compaction pressure result in the poor surface quality. The best machinability of pre-sintered zirconia body was found for 800-900 degrees C pre-sintering temperature, and 200-300 MPa compaction pressure.

Method of forming and assembly of parts

DOEpatents

Ripley, Edward B.

2010-12-28

A method of assembling two or more parts together that may be metal, ceramic, metal and ceramic parts, or parts that have different CTE. Individual parts are formed and sintered from particles that leave a network of interconnecting porosity in each sintered part. The separate parts are assembled together and then a fill material is infiltrated into the assembled, sintered parts using a method such as capillary action, gravity, and/or pressure. The assembly is then cured to yield a bonded and fully or near-fully dense part that has the desired physical and mechanical properties for the part's intended purpose. Structural strength may be added to the parts by the inclusion of fibrous materials.

Bulk superhard B-C-N nanocomposite compact and method for preparing thereof

DOEpatents

Zhao, Yusheng; He, Duanwei

2004-07-06

Bulk, superhard, B-C-N nanocomposite compact and method for preparing thereof. The bulk, superhard, nanocomposite compact is a well-sintered compact and includes nanocrystalline grains of at least one high-pressure phase of B-C-N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compact has a Vicker's hardness of about 41-68 GPa. It is prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture, and sintering the encapsulated ball-milled mixture at a pressure of about 5-25 GPa and at a temperature of about 1000-2500 K.

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

Consolidation and densification methods for fibrous monolith processing

DOEpatents

Sutaria, Manish P.; Rigali, Mark J.; Cipriani, Ronald A.; Artz, Gregory J.; Mulligan, Anthony C.

2006-06-20

Methods for consolidation and densification of fibrous monolith composite structures are provided. Consolidation and densification of two- and three-dimensional fibrous monolith components having complex geometries can be achieved by pressureless sintering. The fibrous monolith composites are formed from filaments having at least a first material composition generally surrounded by a second material composition. The composites are sintered at a pressure of no more than about 30 psi to provide consolidated and densified fibrous monolith composites.

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.

Fabrication and characterization of powder metallurgy tantalum components prepared by high compaction pressure technique

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

Kim, Youngmoo; Agency for Defense Development, Yuseong, P.O. Box 35, Yuseong-gu, Daejeon 34186, Republic of Korea.; Lee, Dongju

2016-04-15

The present study has investigated the consolidation behaviors of tantalum powders during compaction and sintering, and the characteristics of sintered components. For die compaction, the densification behaviors of the powders are simulated by finite element analyses based on the yield function proposed by Shima and Oyane. Accordingly, the green density distribution for coarser particles is predicted to be more uniform because they exhibits higher initial relative tap density owing to lower interparticle friction. It is also found that cold isostatic pressing is capable of producing higher dense compacts compared to the die pressing. However, unlike the compaction behavior, the sinteredmore » density of smaller particles is found to be higher than those of coarser ones owing to their higher specific surface area. The maximum sintered density was found to be 0.96 of theoretical density where smaller particles were pressed isostatically at 400 MPa followed by sintering at 2000 °C. Moreover, the effects of processing conditions on grain size and texture were also investigated. The average grain size of the sintered specimen is 30.29 μm and its texture is less than 2 times random intensity. Consequently, it is concluded that the higher pressure compaction technique is beneficial to produce high dense and texture-free tantalum components compared to hot pressing and spark plasma sintering. - Highlights: • Higher Ta density is obtained from higher pressure and sintering temperature. • High compaction method enables P/M Ta to achieve the density of 16.00 g·cm{sup −3}. • A P/M Ta component with fine microstructure and random orientation is developed.« less

Spark plasma sintering and porosity studies of uranium nitride

NASA Astrophysics Data System (ADS)

Johnson, Kyle D.; Wallenius, Janne; Jolkkonen, Mikael; Claisse, Antoine

2016-05-01

In this study, a number of samples of UN sintered by the SPS method have been fabricated, and highly pure samples ranging in density from 68% to 99.8%TD - corresponding to an absolute density of 14.25 g/cm3 out of a theoretical density of 14.28 g/cm3 - have been fabricated. By careful adjustment of the sintering parameters of temperature and applied pressure, the production of pellets of specific porosity may now be achieved between these ranges. The pore closure behaviour of the material has also been documented and compared to previous studies of similar materials, which demonstrates that full pore closure using these methods occurs near 97.5% of relative density.

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.

Mechanisms of Superplastic Deformation of Nanocrystalline Silicon Carbide Ceramics

DTIC Science & Technology

2012-08-01

These included the following: standard hot isostatic pressing (HIP), spark plasma sintering , ultra-high pressure HIP, and a multianvil pressure...96.8 2270 Multianvil apparatus 1200 3000 94.8 1130 Note: SPS = spark plasma sintering . 2 Figure 1. Ultra-high pressure HIP; 1600 °C, 980...strain rate sensitivity and flow stress. 15. SUBJECT TERMS silicon carbide, nanostructure, sintering , hot isostatic pressing, hardness 16. SECURITY

Effects of pressure and temperature on sintering of Cr-doped Al2O3 by pulsed electric current sintering process

NASA Astrophysics Data System (ADS)

Dang, K. Q.; Nanko, M.

2011-03-01

The aluminium oxide crystal, Al2O3, which contains a small amount of chromium, Cr, is called ruby. Pulsed electric current sintering (PECS) was applied to sinter ruby polycrystals. Cr2O3-Al2O3 powder mixture prepared by drying an aqueous slurry containing amounts of Al2O3 and Cr(NO3)3 was consolidated by PECS process. The PECS process was performed in vacuum at sintering temperature raging from 1100 to 1300°C with heating rate of 2 K/min under applied uniaxial pressure varied from 40 to 100 MPa. This study found that highly densified and transparent Cr-doped Al2O3 can be obtained by the PECS process with the high applied pressure at sintering temperature of 1200°C.

Consolidation and densification methods for fibrous monolith processing

DOEpatents

Sutaria, Manish P.; Rigali, Mark J.; Cipriani, Ronald A.; Artz, Gregory J.; Mulligan, Anthony C.

2004-05-25

Methods for consolidation and densification of fibrous monolith composite structures are provided. Consolidation and densification of two- and three-dimensional fibrous monolith components having complex geometries can be achieved by pressureless sintering. The fibrous monolith composites are formed from filaments having at least a first material composition generally surrounded by a second material composition. The composites are sintered in an inert gas or nitrogen gas at a pressure of no more than about 30 psi to provide consolidated and densified fibrous monolith composites.

Electric Discharge Sintering and Joining of Tungsten Carbide—Cobalt Composite with High-Speed Steel Substrate

NASA Astrophysics Data System (ADS)

Grigoryev, Evgeny G.

2011-01-01

Simultaneous electro discharge sintering of high strength structure of tungsten carbide—cobalt composite and connection it with high-speed steel substrate is investigated and suitable operating parameters are defined. Tungsten carbide—cobalt and high-speed steel joining was produced by the method of high voltage electrical discharge together with application of mechanical pressure to powder compact. It was found that the density and hardness of composite material reach its maximum values at certain magnitudes of applied pressure and high voltage electrical discharge parameters. We show that there is an upper level for the discharge voltage beyond which the powder of composite material disintegrates like an exploding wire. Due to our results it is possible to determine optimal parameters for simultaneous electro discharge sintering of WC-Co and bonding it with high-speed steel substrate.

Injection molding of silicon carbide capable of being sintered without pressure

NASA Technical Reports Server (NTRS)

Muller-Zell, A.; Schwarzmeier, R.

1984-01-01

The most suitable SiC mass for injection molding of SiC articles (for subsequent pressureless sintering) consisted of beta SiC 84, a wax mixture 8, and polyethylene or polystyrene 8 parts. The most effective method for adding the binders was by dissolving them in a solvent and subsequent evaporation. The sequence of component addition was significant, and all parameters were optimized together rather than individually.

Sintering Behavior of Nanocrystalline Silicon Carbide Using a Plasma Pressure Compaction System: Master Sintering Curve Analysis

NASA Astrophysics Data System (ADS)

Bothara, Manish G.; Atre, Sundar V.; Park, Seong-Jin; German, Randall M.; Sudarshan, T. S.; Radhakrishnan, R.

2010-12-01

Nanostructured ceramics offer significant improvements in properties over corresponding materials with larger grain sizes on the order of tens to hundreds of micrometers. Silicon carbide (SiC) samples with grain sizes on the order of 100 nm can result in improved strength, chemical resistance, thermal stability, and tailored electrical resistivity. In this study, nanocrystalline SiC was processed in a plasma pressure compaction (P2C) system at a temperature of 1973 K (1700 °C) that was much lower than the temperatures reported for other sintering techniques. Microstructure of the resulting samples was studied and the hardness and the fracture toughness were measured. The grain sizes were on the order of 700 nm, the hardness between 22 and 24 GPa, and the toughness between 5 and 6.5 MPa·m1/2. The master sintering curve (MSC) analysis was used to model the densification behavior of SiC powder sintered by the P2C method. The apparent activation energies for three different pressures of 10, 30, and 50 MPa were obtained to be 1666, 1034, and 1162 kJ/mol, respectively. Although densification occurs via diffusion, the activation energies were higher than those associated with self-diffusion in SiC (between 570 and 920 kJ/mol). A validation study of the MSC was also conducted and the variation in observed density from the density predicted by the MSC was found to range from 1 to 10 pct.

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.

Densification and Electrical Properties of Zinc Oxide Varistors Microwave-Sintered Under Different Oxygen Partial Pressures

NASA Astrophysics Data System (ADS)

Lin, Cong; Wang, Bo; Xu, Zheng; Peng, Hu

2012-11-01

ZnO varistors were prepared by microwave sintering under different oxygen partial pressures. The temperature profile and the densification behavior in different atmospheres were investigated. It was found that the density of ZnO varistors during sintering was the key factor affecting the absorption of microwave energy. The electrical properties, including the nonlinear properties and capacitance-voltage ( C- V) characteristics, were also carefully studied. The results showed that the oxygen partial pressure has significant effects on the electrical properties of ZnO varistors by changing the concentration of defects through a series of reactions involving oxygen during sintering.

Vacuum Compatibility of Laser-Sintered Metals

NASA Astrophysics Data System (ADS)

Rivera, W. F.; Romero-Talamas, C. A.; Bates, E. M.; Birmingham, W. J.; Quinley, M.; Woodruff, S.; Stuber, J. E.; Sieck, P. E.; Melnik, P. A.

2016-10-01

We present the design and results of a mass spectrometry system used to assess vacuum compatibility of selective laser-sintered parts. The parts are disks with a thickness of 0.20 cm and a diameter of 8.25 cm, and are made of aluminum, stainless steel, inconel, and titanium. From preliminary results, titanium had the lowest partial pressure for hydrogen. Outgassing from laser-sintered parts is compared against parts with similar surface area that are manufactured with traditional methods. Outgassing is also measured while the part is heated, emulating the conditions at the edge of high temperature plasma confinement chambers. Each part is placed on a heated container that can vary in temperature inside the mass spectrometer's vacuum chamber. The partial pressures of elements up to 200 atomic mass units are analyzed to obtain outgassing data from each sample. This work supported under DOE SBIR Grant DE SC0011858.

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

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

Tyrpekl, V., E-mail: vaclav.tyrpekl@ec.europa.eu, E-mail: vaclav.tyrpekl@gmail.com; Berkmann, C.; Holzhäuser, M.

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

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.

Method of producing improved microstructure and properties for ceramic superconductors

DOEpatents

Singh, Jitendra P.; Guttschow, Rob A.; Dusek, Joseph T.; Poeppel, Roger B.

1996-01-01

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). 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 approximately 4 .mu.m. Such a microstructure results in reduced microcracking, strengths as high as 191 MPa and high critical current density capacity.

Method of producing improved microstructure and properties for ceramic superconductors

DOEpatents

Singh, J.P.; Guttschow, R.A.; Dusek, J.T.; Poeppel, R.B.

1996-06-11

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}). 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 approximately 4 {micro}m. Such a microstructure results in reduced microcracking, strengths as high as 191 MPa and high critical current density capacity. 20 figs.

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

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.

Behavior of oxide film at the interface between particles in sintered Al powders by pulse electric-current sintering

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Song, Minghui; Furuya, Kazuo; Noda, Tetsuji

2003-03-01

The microstructure of the bonding interfaces between particles in aluminum (Al) powder sintered specimens by the pulse electric-current sintering (PECS) process was observed, using conventional transmission electron microscopy (CTEM) and high-resolution transmission electron microscopy (HRTEM). The behavior of oxide film at the interface between Al particles and its effect on properties of the sintered specimens were investigated. The results showed there were two kinds of bonding interfaces in the sintered specimens, namely, the direct metal/metal bonding and the metal/oxide film layer/metal bonding interface. By increasing the fraction of the direct metal/metal bonding interfaces, the tensile strength of the sintered specimens increased, and the electrical resistivity decreased. By increasing the loading pressure at higher sintering temperatures or increasing the sintering temperature under loading pressure, the breakdown of oxide film was promoted. The broken oxide film debris was dispersed in aluminum metal near the bonding interfaces between particles.

Effect of heat wave at the initial stage in spark plasma sintering.

PubMed

Zhang, Long; Zhang, Xiaomin; Chu, Zhongxiang; Peng, Song; Yan, Zimin; Liang, Yuan

2016-01-01

Thermal effects are important considerations at the initial stage in spark plasma sintering of non-conductive Al2O3 powders. The generalized thermo-elastic theory is introduced to describe the influence of the heat transport and thermal focusing caused by thermal wave propagation within a constrained space and transient time. Simulations show that low sintering temperature can realize high local temperature because of the superposition effect of heat waves. Thus, vacancy concentration differences between the sink and the cross section of the particles increase relative to that observed during pressure-less and hot-pressure sintering. Results show that vacancy concentration differences are significantly improved during spark plasma sintering, thereby decreasing the time required for sintering.

UO2 fuel pellets fabrication via Spark Plasma Sintering using non-standard molybdenum die

NASA Astrophysics Data System (ADS)

Papynov, E. K.; Shichalin, O. O.; Mironenko, A. Yu; Tananaev, I. G.; Avramenko, V. A.; Sergienko, V. I.

2018-02-01

The article investigates spark plasma sintering (SPS) of commercial uranium dioxide (UO2) powder of ceramic origin into highly dense fuel pellets using non-standard die instead of usual graphite die. An alternative and formerly unknown method has been suggested to fabricate UO2 fuel pellets by SPS for excluding of typical problems related to undesirable carbon diffusion. Influence of SPS parameters on chemical composition and quality of UO2 pellets has been studied. Also main advantages and drawbacks have been revealed for SPS consolidation of UO2 in non-standard molybdenum die. The method is very promising due to high quality of the final product (density 97.5-98.4% from theoretical, absence of carbon traces, mean grain size below 3 μm) and mild sintering conditions (temperature 1100 ºC, pressure 141.5 MPa, sintering time 25 min). The results are interesting for development and probable application of SPS in large-scale production of nuclear ceramic fuel.

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.

Ultra-high Strength Nanostructured Mg

DTIC Science & Technology

2014-03-31

27709-2211 Nanostructured Mg and Mg alloys, Mg metallic glass, Cryomilling, Powder consolidation, Spark plasma sintering , Deformation mechanisms REPORT...mechanically milled powder and high pressure on spark plasma sintering of Mg-Cu-Gd metallic glasses; (9) microstructure and mechanical behavior of Mg-10Li-3Al...pressure on spark plasma sintering of Mg– Cu–Gd metallic glasses, Acta Materialia , (07 2013): 4414. doi: Baolong Zheng, Ying Li, Weizong Xu

Fabrication of highly dense SiN4 ceramics without additives by high pressure sintering

NASA Technical Reports Server (NTRS)

Takatori, K.; Shimade, M.; Koizumi, M.

1984-01-01

Silicon nitride (Si3N4) is one of candidate materials for the engineering ceramics which is used at high temperatures. The mechanical strengths of hot pressed or sintered Si2N4 ceramics containing some amount of additives, however, are deteriorated at elevated temperatures. To improve the high temperature strength of Si3N4 ceramics, an attempt to consolidate Si3N4 without additives was made by high pressure sintering technique. Scanning electron micrographs of fracture surfaces of the sintered bodies showed the bodies had finely grained and fully self-bonded sintered bodies were 310N sq m at room temperature and 174N/sq m at 1200 C.

Stress-dislocation interaction mechanism in low-temperature thermo-compression sintering of Ag NPs

NASA Astrophysics Data System (ADS)

Wang, Fuliang; Tang, Zikai; He, Hu

2018-04-01

The sintering of metal nanoparticles (NPs) has been widely studied in the field of nanotechnology, and low-temperature sintering has become the industry standard. In this study, a molecular dynamics (MD) model was established to study the sintering behaviour of silver NPs during low-temperature thermo-compression. Primarily, we studied the sintering process, in which the ratio of neck radius to particle radius (x/r) changes. Under a uniaxial pressure, the maximum ratio in the temperature range 420-425 K was 1. According to the change of x/r, the process can be broken down into three stages: the neck-formation stage, neck-growth stage, and neck-stability stage. In addition, the relationship between potential energy, internal stress, and dislocation density during sintering is discussed. The results showed that cycling internal stress played an important role in sintering. Under the uniaxial pressure, the stress-dislocation interaction was found to be the major mechanism for thermo-compression sintering because the plastic deformation product dislocation intensified the diffusion of atoms. Also, the displacement vector, the mean square displacement, and the changing crystal structure during sintering were studied.

LIQUID PHASE SINTERING OF METALLIC CARBIDES

DOEpatents

Hammond, J.; Sease, J.D.

1964-01-21

An improved method is given for fabricating uranium carbide composites, The method comprises forming a homogeneous mixture of powdered uranium carbide, a uranium intermetallic compound which wets and forms a eutectic with said carbide and has a non-uranium component which has a relatively high vapor pressure at a temperature in the range 1200 to 1500 deg C, and an organic binder, pressing said mixture to a composite of desired green strength, and then vacuum sintering said composite at the eutectic forming temperature for a period sufficient to remove at least a portion of the non-uranium containing component of said eutectic. (AEC)

The investigation of die-pressing and sintering behavior of ITP CP-Ti and Ti-6Al-4V powders

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

Chen, Wei; Yamamoto, Yukinori; Peter, William H

This paper investigated the die-pressing and sintering behavior of the low-cost CP-Ti and Ti-6Al- 4V powders made by the Armstrong Process . The Armstrong powders have an irregular coral like, dendritic morphology, with a dendrite size of approximately 2-5 m. As-received as well as milled powders were uniaxially pressed at designated pressures up to 690 MPa to form disk samples with different aspect ratios. In the studied pressure range, an empirical powder compaction equation was applied to linearize the green density pressure relationship, and powder compaction parameters were obtained. The Armstrong Ti-64 powder exhibited a significantly higher sinterability than themore » CP-Ti powder. This was explained to be due to the higher diffusivity of V at the sintering temperature. The Ti-64 samples with a green density of 71.0% increased to 99.6% after sintering at 1300oC for 1 hour. An ex-situ technique was used to track the powder morphology change before and after sintering.« less

Improved compaction of ZnO nano-powder triggered by the presence of acetate and its effect on sintering.

PubMed

Dargatz, Benjamin; Gonzalez-Julian, Jesus; Guillon, Olivier

2015-04-01

The retention of nanocrystallinity in dense ceramic materials is still a challenge, even with the application of external pressure during sintering. The compaction behavior of high purity and acetate enriched zinc oxide (ZnO) nano-powders was investigated. It was found that acetate in combination with water plays a key role during the compaction into green bodies at moderate temperatures. Application of constant pressure resulted in a homogeneous green body with superior packing density (86% of theoretical value) at moderate temperature (85 °C) in the presence of water. In contrast, no improvement in density could be achieved if pure ZnO powder was used. This compaction behavior offers superior packing of the particles, resulting in a high relative density of the consolidated compact with negligible coarsening. Dissolution accompanying creep diffusion based matter transport is suggested to strongly support reorientation of ZnO particles towards densities beyond the theoretical limit for packing of ideal monosized spheres. Finally, the sintering trajectory reveals that grain growth is retarded compared to conventional processing up to 90% of theoretical density. Moreover, nearly no radial shrinkage was observed after sinter-forging for bodies performed with this advanced processing method.

Improved compaction of ZnO nano-powder triggered by the presence of acetate and its effect on sintering

PubMed Central

Gonzalez-Julian, Jesus; Guillon, Olivier

2015-01-01

The retention of nanocrystallinity in dense ceramic materials is still a challenge, even with the application of external pressure during sintering. The compaction behavior of high purity and acetate enriched zinc oxide (ZnO) nano-powders was investigated. It was found that acetate in combination with water plays a key role during the compaction into green bodies at moderate temperatures. Application of constant pressure resulted in a homogeneous green body with superior packing density (86% of theoretical value) at moderate temperature (85 °C) in the presence of water. In contrast, no improvement in density could be achieved if pure ZnO powder was used. This compaction behavior offers superior packing of the particles, resulting in a high relative density of the consolidated compact with negligible coarsening. Dissolution accompanying creep diffusion based matter transport is suggested to strongly support reorientation of ZnO particles towards densities beyond the theoretical limit for packing of ideal monosized spheres. Finally, the sintering trajectory reveals that grain growth is retarded compared to conventional processing up to 90% of theoretical density. Moreover, nearly no radial shrinkage was observed after sinter-forging for bodies performed with this advanced processing method. PMID:27877777

Effect of surface oxide films on the properties of pulse electric-current sintered metal powders

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Yamaguchi, Norio; Wang, Airu

2003-11-01

Metallic powders with various thermodynamic stability oxide films (Ag, Cu, and Al powders) were sintered using a pulse electric-current sintering (PECS) process. Behavior of oxide films at powder surfaces and their effect on the sintering properties were investigated. The results showed that the sintering properties of metallic powders in the PECS process were subject to the thermodynamic stability of oxide films at particles surfaces. The oxide films at Ag powder surfaces are decomposed during sintering with the contact region between the particles being metal/metal bond. The oxide films at Cu powder surfaces are mainly broken via loading pressure at a low sintering temperature. At a high sintering temperature, they are mainly dissolved in the parent metal, and the contact regions turn into the direct metal/metal bonding. Excellent sintering properties can be received. The oxide films at Al powder surfaces are very stable, and cannot be decomposed and dissolved, but broken by plastic deformation of particles under loading pressure at experimental temperatures. The interface between particles is partially bonded via the direct metal/metal bonding making it difficult to achieve good sintered properties.

Synthesis and mechanical/magnetic properties of nano-grained iron-oxides prepared with an inert gas condensation and pulse electric current sintering process

NASA Astrophysics Data System (ADS)

Choa, Yong-Ho; Nakayama, Tatachika; Sekino, Tohru; Niihara, Koichi

1999-04-01

Nanocrystalline iron-oxide powder was fabricated with an inert gas condensation (IGC) method combined with evaporation, and in-situ oxidation techniques. The particle size of iron-oxide powder was controlled by varying the helium gas pressure between 0.1 and 10 Torr, with the smallest one =10 nm at 0.1 Torr. The nanostructure was characterized by TEM. Nanocrystalline iron-oxide powder was sintered with the pulse electric current sintering (PECS) method to obtain densified γ-Fe2O3 materials, and suitably densified nano-grained γ-Fe2O3 materials (≈ 40 nm) of great hardness were obtained. The correlation between the nanostructure and magnetic properties of nanocrystalline powder and densified γ-Fe2O3 materials was also investigated.

Study of phenomena related to the sintering process of silicon nitride at atmospheric pressure

NASA Technical Reports Server (NTRS)

Bertani, A.

1982-01-01

A procedure was perfected for the production of components used in engineering applications of silicon nitride. Particles of complex geometry that combine remarkable mechanical properties with a high density are obtained. The process developed, in contrast to the "hot pressing" method, does not use external pressures, and in contrast to the reaction bonding method, final densities close to the theoretical value are obtained.

Manufacture of dense sintered bodies containing silicon nitride

NASA Technical Reports Server (NTRS)

Hirota, K.; Hasegawa, Y.; Ogura, K.; Yashima, Y.

1985-01-01

Sintered bodies containing 1-32.5 Si oxide and 1.5 wt.% SiC (Si oxide/SiC wt. ratio 3/2) are prepared and kept in a 10-3000 kg/2 sq. cm. N (g) atmosphere at 1500-2300 degrees, while simultaneously maintaining the CO (g) partial pressure around the body lower than the nitrogenation equil. pressure to give a dense sintered body. The prepared dense sintered body has high strength at high temperatures. Thus, SiC 40, oxide 30 and Si3N4 30 wt% were fired to a body which was kept in 1500 kg/sq. cm. N (g) for 20 h at 2000 degrees to give a dense sintered body having high bending strength at high temperatures.

High pressure sintering of non-oxide materials. [hot pressing AIN, TiC, and alpha-Si3N4

NASA Technical Reports Server (NTRS)

Shimado, M.; Ogawa, N.; Koizumi, M.

1979-01-01

Pure materials of AIN, alpha-Si3N4 and TiC, without additives were sintered at 800 C to 1400 C under the pressures of 30 kbar and 50 kbar for 0.5 hours. The maximum density of sintered bodies for the cited materials was nearly 100% for AIN, 98% for TiC and 96% for alpha-Si3N4.

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.

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

PubMed

Mangialardi, T

2001-10-12

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

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.

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.

Enhanced thermal diffusivity of copperbased composites using copper-RGO sheets

NASA Astrophysics Data System (ADS)

Kim, Sangwoo; Kwon, Hyouk-Chon; Lee, Dohyung; Lee, Hyo-Soo

2017-11-01

The synthesis of copper-reduced graphene oxide (RGO) sheets was investigated in order to control the agglutination of interfaces and develop a manufacturing process for copper-based composite materials based on spark plasma sintering. To this end, copper-GO (graphene oxide) composites were synthesized using a hydrothermal method, while the copper-reduced graphene oxide composites were made by hydrogen reduction. Graphene oxide-copper oxide was hydrothermally synthesized at 80 °C for 5 h, and then annealed at 800 °C for 5 h in argon and hydrazine rate 9:1 to obtain copper-RGO flakes. The morphology and structure of these copper-RGO sheets were characterized using scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and Raman spectroscopy. After vibratory mixing of the synthesized copper-RGO composites (0-2 wt%) with copper powder, they were sintered at 600 °C for 5 min under100 MPa of pressure by spark plasma sintering process. The thermal diffusivity of the resulting sintered composite was characterized by the laser flash method at 150 °C.

Role of air on local water retention behavior in the shallow heterogeneous vadose zone

NASA Astrophysics Data System (ADS)

Sakaki, T.; Limsuwat, A.; Illangasekare, T. H.

2009-12-01

In the presence of a subsurface source, air flowing through the unsaturated soil can transport toxic vapor into subsurface structures due to pressure gradients created by, e.g., a pressure drop within the building. Development of dynamic air pathways in the subsurface are largely controlled by the geological heterogeneity and the spatial and temporal distribution of soil moisture. To better understand how these air pathways are developed, it is crucial to know how water is retained in heterogeneous medium at spatial resolutions that are finer than those adopted in typical hydrologic and soil physics applications. Although methods for soil water pressure measurement can be readily found in literature, a technique for measuring “air pressure” in wet soil is not well-established or documented. Hydrophobic porous ceramic cups have been used to measure non-wetting NAPL phase pressure in two-phase systems. However, our preliminary tests using the hydrophobic ceramic cups installed in highly wet soil showed that under conditions of fast drainage of the wetting fluid that is replaced by air, it typically took some time before the cups responded to register the air pressure. Therefore, an attempt was made to develop a more robust method where the time lag is minimized. The tested materials were; 1) ceramic porous cups, 2) sintered stainless steel cups, 3) porous glass discs, and 4) non-woven PTFE fabric. The ceramic cups, sintered stainless steel cups and sintered porous glass discs required hydrophobic treatment, whereas the non-woven PTFE fabric is hydrophobic by itself. To treat the ceramic porous cups, the method proposed by Parker and Lenhard [1988] was adopted. The sintered porous stainless steel cups and porous glass discs were treated by a commercially available water repellant compound. For those four materials, contact angle, water entry pressure, and time lag to respond to an imposed pressure were measured. The best performing material was then tested in a simple heterogeneous column. The column was packed using two sands to form three layers where the coarser sand was sandwitched by two layers of a finer sand. In each layer, soil moisture, water pressure and air pressure were monitored. The soil was initially saturated and suction at the bottom was gradually increased to induce wetting fluid drainage, and followed by a wetting cycle. In the drainage cycle, the coarse middle layer did not drain until air front reached the bottom of the top fine layer. Once the air front reached the fine-coarse interface, air was quickly pulled into the coarse layer. The results showed that the newly developed hydrophobic material showed very small time lag and captured the abrupt air pressure change in the wet soil. In the wetting cycle, we observed positive air pressure which indicated entrapment of air and its compression as wetting proceeded. This behavior cannot be evaluated properly without the rapid measurement of air pressure. The method is currently being applied in a large 2D vertical aquifer with a structured heterogeneity to investigate how air pathways are formed under various flux/temperature conditions at the soil surface.

Hydrothermal Cold Sintering

NASA Astrophysics Data System (ADS)

Kang, Xiaoyu

Solid state sintering transforms particle compact to a physically robust and dense polycrystalline monolith driven by reduction of surface energy and curvature. Since bulk diffusion is required for neck formation and pore elimination, sintering temperature about 2/3 of melting point is needed. It thus places limitations for materials synthesis and integration, and contributes to significant energy consumption in ceramic processing. Furthermore, since surface transport requires lower temperature than bulk processes, grain growth is often rapid and can be undesired for physical properties. For these reasons, several techniques have been developed including Liquid Phase Sintering (LPS), Hot Pressing (HP) and Field Assisted Sintering Technique (FAST), which introduce either viscous melt, external pressure or electric field to speed up densification rates at lower temperature. However, because of their inherent reliability on bulk diffusion, temperatures required are often too high for integrating polymers and non-noble metals. Reduction of sintering temperature below 400 °C would require a different densification mechanism that is based on surface transport with external forces to drive volume shrinkage. Densification method combining uniaxial pressure and solution under hydrothermal condition was first demonstrated by Kanahara's group at Kochi University in 1986 and was brought to our attention by the work of Kahari, etc, from University of Oulu on densification of Li2MoO 4 in 2015. This relatively new process showed promising ultra-low densification temperature below 300 °C, however little was known about its fundamental mechanism and scope of applications, which became the main focus of this dissertation. In this work, a uniaxial hydraulic press, a standard stainless steel 1/2 inch diameter die with heating band were utilized in densifying metal oxides. Applied pressure and sintering temperature were between 100 MPa and 700 MPa and from room temperature to 300 °C, respectively. Process variables were defined and effects of individual parameters were studied systematically through control variable method with Li2MoO4-water system. Crystalline structure, fractured surface morphology and chemical bonding information of the cold sintered pellets were studied with X-ray diffraction (XRD), field effect scanning electron microscopy (FE-SEM) and Raman spectroscopy, etc. Densification mechanism studies were conducted on ZnO. Through comparison experiments, it was found that the Zn2+ concentration in the solution is critical for densification, while dissolution of grains only serves as a means to the former. Through pressure dependent studies, a critical value was found, which correlated well with the hydrostatic pressure keeping liquid water from thermal expansion. These results confirmed establishment of hydrothermal condition that would be important for mass transport in densification. Densification rate variations with process time was estimated and similar time dependence to Kingery's model was found. The densification process was proposed to be consist of three consecutive stages, which are quick initial compaction, grain rearrangement and dissolution-reprecipitation events. Binary metal oxides with different acidities were subjected to cold sintering with various aqueous solutions in establishing a criteria for material selection. It was found that in general materials with high solubility at around neutral pH, high dissolution kinetics and similar free energy to their hydroxides or hydrates at ambient would be more likely for full densification with high phase purity. The anions in solution should also be wisely selected to avoid stable compound or complex formation. To extend the applicable material list for full densification, non-aqueous solvent of dimethyl sulfoxide (DMSO) based solution was studied for cold sintering. Both improvement of pellet density and suppression of hydroxide formation were achieved for MnO by using DMSO-HOAc solution. With this strategy, densification of other metal oxides with strong hydroxide formation may also be improved, for example oxides of alkaline earth and many transition metals. Finally, the author's previous work on Zn1-xMg xO thin films is included in Chapter 7.

Citrate gel-combustion synthesis and sintering of nanocrystalline ThO2 powders

NASA Astrophysics Data System (ADS)

Sanjay Kumar, D.; Ananthasivan, K.; Amirthapandian, S.; Dasgupta, Arup; Jogeswara Rao, G.

2017-12-01

A systematic study of the influence of citric acid to nitrate mole (R) ratio (R = 0 to 0.50) on the citrate gel-combustion synthesis of nanocrystalline (nc) ThO2 in bulk quantities (30 g) by using citrate gel-combustion was carried out. The nc-ThO2 powders were characterized for their bulk density, size distribution of particles, specific surface area, carbon residue and X-ray crystallite size. All these powders were compacted at pressures varying from 60 to 353 MPa and sintered by using the "two-step sintering" method. Powders prepared from a mixture with an "R" value of 0.125 compacted at 243 MPa yielded a maximum sintered density of 98.8 ± 0.3% T.D. For nc-ThO2, this is the highest sintered density reported so far. The microstructural investigations on nc-ThO2 powders were carried out by using both scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM images of the sintered thoria monoliths revealed faceted grains with well defined grain boundaries. Shrinkage anisotropy factor (α) revealed that the compacts prepared from the powders obtained from starting mixtures with R values of 0.125-0.50 had undergone uniform sintering (near isotropic shrinkage).

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.

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.

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)

Characterizations of Rapid Sintered Nanosilver Joint for Attaching Power Chips

PubMed Central

Feng, Shuang-Tao; Mei, Yun-Hui; Chen, Gang; Li, Xin; Lu, Guo-Quan

2016-01-01

Sintering of nanosilver paste has been extensively studied as a lead-free die-attach solution for bonding semiconductor power chips, such as the power insulated gated bipolar transistor (IGBT). However, for the traditional method of bonding IGBT chips, an external pressure of a few MPa is reported necessary for the sintering time of ~1 h. In order to shorten the processing duration time, we developed a rapid way to sinter nanosilver paste for bonding IGBT chips in less than 5 min using pulsed current. In this way, we firstly dried as-printed paste at about 100 °C to get rid of many volatile solvents because they may result in defects or voids during the out-gassing from the paste. Then, the pre-dried paste was further heated by pulse current ranging from 1.2 kA to 2.4 kA for several seconds. The whole procedure was less than 3 min and did not require any gas protection. We could obtain robust sintered joint with shear strength of 30–35 MPa for bonding 1200-V, 25-A IGBT and superior thermal properties. Static and dynamic electrical performance of the as-bonded IGBT assemblies was also characterized to verify the feasibility of this rapid sintering method. The results indicate that the electrical performance is comparable or even partially better than that of commercial IGBT modules. The microstructure evolution of the rapid sintered joints was also studied by scanning electron microscopy (SEM). This work may benefit the wide usage of nanosilver paste for rapid bonding IGBT chips in the future. PMID:28773686

Characterizations of Rapid Sintered Nanosilver Joint for Attaching Power Chips.

PubMed

Feng, Shuang-Tao; Mei, Yun-Hui; Chen, Gang; Li, Xin; Lu, Guo-Quan

2016-07-12

Sintering of nanosilver paste has been extensively studied as a lead-free die-attach solution for bonding semiconductor power chips, such as the power insulated gated bipolar transistor (IGBT). However, for the traditional method of bonding IGBT chips, an external pressure of a few MPa is reported necessary for the sintering time of ~1 h. In order to shorten the processing duration time, we developed a rapid way to sinter nanosilver paste for bonding IGBT chips in less than 5 min using pulsed current. In this way, we firstly dried as-printed paste at about 100 °C to get rid of many volatile solvents because they may result in defects or voids during the out-gassing from the paste. Then, the pre-dried paste was further heated by pulse current ranging from 1.2 kA to 2.4 kA for several seconds. The whole procedure was less than 3 min and did not require any gas protection. We could obtain robust sintered joint with shear strength of 30-35 MPa for bonding 1200-V, 25-A IGBT and superior thermal properties. Static and dynamic electrical performance of the as-bonded IGBT assemblies was also characterized to verify the feasibility of this rapid sintering method. The results indicate that the electrical performance is comparable or even partially better than that of commercial IGBT modules. The microstructure evolution of the rapid sintered joints was also studied by scanning electron microscopy (SEM). This work may benefit the wide usage of nanosilver paste for rapid bonding IGBT chips in the future.

Thermoset recycling via high-pressure high-temperature sintering: Revisiting the effect of interchange chemistry

NASA Astrophysics Data System (ADS)

Morin, Jeremy Edward

In 1844 Charles Goodyear obtained U.S. Patent #3,633 for his "Gum Elastic Composition". In a published circular, which describes his patent for the sulfur vulcanization of gum elastic composition, he stated: "No degree of heat, without blaze, can melt it (rubber)... It resists the most powerful chemical reagents. Aquafortis (nitric acid), sulphuric acid, essential and common oils, turpentine and other solvents... ..." Goodyear's sulfur vulcanization of rubber fueled much of the industrial revolution and made transportation possible, as it exists today. In doing so, Goodyear created one of the most difficult materials to recycle. Rubber will not melt, dissolve, or lend itself to the usual methods of chemical decomposition. Ironically, Goodyear recognized this problem and in 1853 he patented the process of adding ground rubber to virgin material, now currently known as regrind blending. Today, scrap tires represent one of the most serious sources of pollution in the world. Studies estimate that there are roughly 2 billion scrap tires in U.S. landfills and more are being added at a rate of over 273 million tires per year. Current methods of recycling waste tires are crude, ineffective, and use rubber powder as a low cost filler instead of a new rubber. The groundwork for a very simple and effective method of producing high-quality rubber goods using 100% scrap rubber was discovered in 1944 by A. V. Tobolsky et al. This application, however, was not recognized until recently in our laboratory. The process as studied to date represents a method of creating quality, high-value added rubber goods with nothing other than heat and pressure. High pressure is required to obtain a void-free compaction of the rubber particles by forcing all of the free surfaces into intimate contact. High temperature then activates the chemical rearrangement, scission, and reformation of the chemical bonds thus providing new bridges between the once fractured interfaces. This occurs both within and between particles. The technique of high-pressure high-temperature sintering has worked on all types of thermoset materials. Typical mechanical properties for sintered SBR powder rubber are as follows: 1.3 MPa 100% Modulus, 12.0 MPa Tensile Strength and 300% Elongation at Break. The goal of this research is two-fold. First, to gain an understanding of the variables that control the process of high-pressure high-temperature sintering. Second, to study the factors governing the mechanism of fusion with the hope of controlling and exploiting this process so that tires can be recycled to produce high quality and high-value added products.

Study on acoustical properties of sintered bronze porous material for transient exhaust noise of pneumatic system

NASA Astrophysics Data System (ADS)

Li, Jingxiang; Zhao, Shengdun; Ishihara, Kunihiko

2013-05-01

A novel approach is presented to study the acoustical properties of sintered bronze material, especially used to suppress the transient noise generated by the pneumatic exhaust of pneumatic friction clutch and brake (PFC/B) systems. The transient exhaust noise is impulsive and harmful due to the large sound pressure level (SPL) that has high-frequency. In this paper, the exhaust noise is related to the transient impulsive exhaust, which is described by a one-dimensional aerodynamic model combining with a pressure drop expression of the Ergun equation. A relation of flow parameters and sound source is set up. Additionally, the piston acoustic source approximation of sintered bronze silencer with cylindrical geometry is presented to predict SPL spectrum at a far-field observation point. A semi-phenomenological model is introduced to analyze the sound propagation and reduction in the sintered bronze materials assumed as an equivalent fluid with rigid frame. Experiment results under different initial cylinder pressures are shown to corroborate the validity of the proposed aerodynamic model. In addition, the calculated sound pressures according to the equivalent sound source are compared with the measured noise signals both in time-domain and frequency-domain. Influences of porosity of the sintered bronze material are also discussed.

Laminated composite of magnetic alloy powder and ceramic powder and process for making same

DOEpatents

Moorhead, Arthur J.; Kim, Hyoun-Ee

1999-01-01

A laminated composite structure of alternating metal powder layers, and layers formed of an inorganic bonding media powder, and a method for manufacturing same are discosed. The method includes the steps of assembling in a cavity alternating layers of a metal powder and an inorganic bonding media of a ceramic, glass, and glass-ceramic. Heat, with or without pressure, is applied to the alternating layers until the particles of the metal powder are sintered together and bonded into the laminated composite structure by the layers of sintered inorganic bonding media to form a strong composite structure. The method finds particular application in the manufacture of high performance magnets wherein the metal powder is a magnetic alloy powder.

Laminated composite of magnetic alloy powder and ceramic powder and process for making same

DOEpatents

Moorhead, A.J.; Kim, H.

1999-08-10

A laminated composite structure of alternating metal powder layers, and layers formed of an inorganic bonding media powder, and a method for manufacturing same are disclosed. The method includes the steps of assembling in a cavity alternating layers of a metal powder and an inorganic bonding media of a ceramic, glass, and glass-ceramic. Heat, with or without pressure, is applied to the alternating layers until the particles of the metal powder are sintered together and bonded into the laminated composite structure by the layers of sintered inorganic bonding media to form a strong composite structure. The method finds particular application in the manufacture of high performance magnets wherein the metal powder is a magnetic alloy powder. 9 figs.

Method of forming and assembly of metal and ceramic parts

DOEpatents

Ripley, Edward B

2014-04-22

A method of forming and assembling at least two parts together that may be metal, ceramic, or a combination of metal and ceramic parts. Such parts may have different CTE. Individual parts that are formed and sintered from particles leave a network of interconnecting porosity in each sintered part. The separate parts are assembled together and then a fill material is infiltrated into the assembled parts using a method such as capillary action, gravity, and/or pressure. The assembly is then cured to yield a bonded and fully or near-fully dense part that has the desired physical and mechanical properties for the part's intended purpose. Structural strength may be added to the parts by the inclusion of fibrous materials.

Method of forming and assembly of metal parts and ceramic parts

DOEpatents

Ripley, Edward B [Knoxville, TN

2011-11-22

A method of forming and assembling at least two parts together that may be metal, ceramic, or a combination of metal and ceramic parts. Such parts may have different CTE. Individual parts that are formed and sintered from particles leave a network of interconnecting porosity in each sintered part. The separate parts are assembled together and then a fill material is infiltrated into the assembled parts using a method such as capillary action, gravity, and/or pressure. The assembly is then cured to yield a bonded and fully or near-fully dense part that has the desired physical and mechanical properties for the part's intended purpose. Structural strength may be added to the parts by the inclusion of fibrous materials.

A pilot study for determining the optimal operation condition for simultaneously controlling the emissions of PCDD/Fs and PAHs from the iron ore sintering process.

PubMed

Chen, Yu-Cheng; Tsai, Perng-Jy; Mou, Jin-Luh; Kuo, Yu-Chieh; Wang, Shih-Min; Young, Li-Hao; Wang, Ya-Fen

2012-09-01

In this study, the cost-benefit analysis technique was developed and incorporated into the Taguchi experimental design to determine the optimal operation combination for the purpose of providing a technique solution for controlling both emissions of PCDD/Fs and PAHs, and increasing both the sinter productivity (SP) and sinter strength (SS) simultaneously. Four operating parameters, including the water content, suction pressure, bed height, and type of hearth layer, were selected and all experimental campaigns were conducted on a pilot-scale sinter pot to simulate various sintering operating conditions of a real-scale sinter plant. The resultant optimal combination could reduce the total carcinogenic emissions arising from both emissions of PCDD/Fs and PAHs by 49.8%, and increase the sinter benefit associated with the increase in both SP and SS by 10.1%, as in comparison with the operation condition currently used in the real plant. The ANOVA results indicate that the suction pressure was the most dominant parameter in determining the optimal operation combination. The above result was theoretically plausible since the higher suction pressure provided more oxygen contents leading to the decrease in both PCDD/F and PAH emissions. But it should be noted that the results obtained from the present study were based on pilot scale experiments, conducting confirmation tests in a real scale plant are still necessary in the future. Copyright © 2012 Elsevier Ltd. All rights reserved.

Influence of spark plasma sintering parameters on magnetic properties of FeCo alloy

NASA Astrophysics Data System (ADS)

Albaaji, Amar J.; Castle, Elinor G.; Reece, Mike J.; Hall, Jeremy P.; Evans, Sam L.

2018-04-01

Equiatomic FeCo alloys with average particle size of 24 μm were sintered using spark plasma sintering (SPS) system at sintering temperatures of 1100, 800, and 850 °C for heating rates 50, 100, 300 °C/min by applying pressure of 50 MPa instantly at room temperature for sintering time of 5 and 15 minutes. The highest saturation induction was achieved at SPS conditions of 50 MPa, 50 °C/min, 1100 °C, without dwelling, of value 2.39 T. The saturation induction was improved with extending sintering time, the coercivity was higher in samples sintered at a fast heating rate in comparison to the slowest heating rate.

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.

Effects of sintering process on wear and mechanical behavior properties of titanium carbide/hexagonal boron nitrid/steel 316L base nanocomposites

NASA Astrophysics Data System (ADS)

Sadooghi, Ali; Payganeh, Gholamhassan

2018-02-01

Powder metallurgy process is one of the approaches to manufacture nanocomposite samples, in which the product quality depends upon the pressure, temperature, and sintering time. In this manuscript, steel is selected as the base material together with 2% carbon-based reinforcing TiC particles, and 2% hBN particles as the self-lubricant material. The powders were mixed for 5 h in high ball milling, and compacted with two pressures of 350 and 450 MPa, sintered in the furnace for 2 and 4 h, and sintering temperatures of 1350 and 1450 °C were utilized. SEM, XRD, and EDX tests are performed to identify the nanocomposite structure, and DTA tests are carried out to specify the temperature graph of the material. Finally, hardness, wear, and bending tests are done to find the corresponding mechanical properties of the samples. As a result, the optimum process parameters, including pressure, temperature and sintering duration is achieved. Results show that adding the reinforcing particles into a steel matrix increase the hardness, as well as flexural strength of the nanocomposite product. Also, coefficient of friction shows a decreases.

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 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.

Fabrication of thermoelectric modules with Mg2Si and SrRuO3 by the spark plasma sintering method

NASA Astrophysics Data System (ADS)

Nishio, Keishi; Sawada, Yukie; Arai, Koya; Sakamoto, Tatsuya; Kogo, Yasuo; Iida, Tsutomu

2012-06-01

Thermoelectric (TE) modules with a π structure were fabricated by the spark plasma sintering method. The modules were composed of SrRuO3 for the p-type semiconductor, Mg2Si for the n-type semiconductor, and Ni for the electrodes. The SrRuO3 powder was synthesized using the metal-citric-acid complex decomposition method. Mg2Si bulk prepared by meltquenching was ground into powder and sieved to a particle size of 75 μm or less. To obtain the sintered body of SrRuO3, the powder was sintered using spark plasma sintering (SPS). For SPS, the precursor powder was placed in a graphite die and kept at that temperature under a uni-axial pressure of 50 MPa and in vacuum conditions (less than 7 Pa). After sintering by SPS, the ceramic sample was annealed at 1573K in air because the SrRuO3 was slightly reduced during the SPS process in the graphite die. These TE sintered bodies were cut and polished. The dimensions of the samples used for fabrication of the p-type parts of the TE modules were 4.50×9.50×7.45 mm3 and those for the n-type parts were 5.50×11.45×7.45 mm3. Pressed Ni powder was put between these TE materials and the Ni electrodes in order to connect them together, and electrical power was passed through the electrodes from the SPS equipment. The output power under temperature differences ΔT ranging from 100 to 500 K was measured. The open-circuit voltage, maximum output current and maximum output power increased with increasing temperature difference ΔT. The open-circuit voltage of the single module was 91.0 mV, and the maximum output current and maximum output power were 5000 mA and 110 mW at ΔT=500 K, respectively.

CALCIUM OXIDE SINTERING IN ATMOSPHERES CONTAINING WATER AND CARBON DIOXIDE

EPA Science Inventory

The paper gives results of measurements of the effects of water vapor and CO2 on the sintering rate of nascent CaO, as a function of partial pressure and temperature using CaO prepared by rapid decomposition of CaCO3 and CA(OH)2. Each gas strongly catalyzed the sintering process ...

Compositions Comprising Nickel-Titanium, Methods Manufacture Thereof and Articles Comprising the Same

NASA Technical Reports Server (NTRS)

DellaCorte, Christopher (Inventor); Glennon, Glenn N. (Inventor)

2016-01-01

Disclosing herein is a method for manufacturing nickel-titanium compositions. The method includes disposing a powdered composition in a mold; the powdered composition comprising nickel and titanium; the titanium being present in an amount of about 38 to about 42 wt % and the nickel being present in an amount of about 58 to about 62 wt %; sintering the powdered composition to produce a sintered preform; compacting the preform; machining the preform to form an article; heat treating the article; the annealing being conducted at a temperature of about 1650.degree. F. to about 1900.degree. F. at a pressure of about 3 Torr to about 5 Kg-f/cm.sup.2 for a time period of about 10 minutes to about 5 hours; and quenching the article.

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

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

Thomas Zwitter; Phillip Nash; Xiaoyan Xu

2011-03-31

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

Manufacture of sintered silicon nitrides

NASA Technical Reports Server (NTRS)

Iwai, T.

1985-01-01

Sintered silicon nitrides are manufactured by sintering Si3N powder containing 2 to 15% in wt of a powder mixture composed of nitride powder of lanthanide or Y 100 parts and AIN powder less than 100 parts at 1500 to 1900 deg. temperature under a pressure of less than 200 Kg/sq. cm. The sintered Si3N has high mechanical strength in high temperature. Thus, Si3N4 93.0, Y 5.0 and AlN 2.0% in weight were wet mixed in acetone in N atom, molded and sintered at 1750 deg. and 1000 Kg/sq. cm. to give a sintered body having high hardness.

Ceramic synthesis of 0.08BiGaO3-0.90BaTiO3-0.02LiNbO3 under high pressure and high temperature

NASA Astrophysics Data System (ADS)

Hui, Jin; Yong, Li; Mou-Sheng, Song; Lin, Chen; Xiao-Peng, Jia; Hong-An, Ma

2016-07-01

In this paper, the preparation of 0.08BiGaO3-0.90BaTiO3-0.02LiNbO3 is investigated at pressure 3.8 GPa and temperature 1100-1200 °C. Experimental results indicate that not only is the sintered rate more effective, but also the sintered temperature is lower under high pressure and high temperature than those of under normal pressure. It is thought that the adscititious pressure plays the key role in this process, which is discussed in detail. The composition and the structure of the as-prepared samples are recorded by XRD patterns. The result shows that the phases of BaTiO3, BaBiO2.77, and Ba2Bi4Ti5O18 with piezoelectric ceramic performance generate in the sintered samples. Furthermore, the surface morphology characteristics of the typical samples are also investigated using a scanning electron microscope. It indicates that the grain size and surface structure of the samples are closely related to the sintering temperature and sintering time. It is hoped that this study can provide a new train of thought for the preparation of lead-free piezoelectric ceramics with excellent performance. Project supported by the National Natural Science Foundation of China (Grant No. 51172089), the Natural Science Foundation of Education Department of Guizhou Province, China (Grant Nos. KY [2013]183 and LH [2015]7232), and the Research Fund for the Doctoral Program of Tongren University, China (Grant No. DS1302).

Can the use of pulsed direct current induce oscillation in the applied pressure during spark plasma sintering?

PubMed Central

Salamon, David; Eriksson, Mirva; Nygren, Mats; Shen, Zhijian

2012-01-01

The spark plasma sintering (SPS) process is known for its rapid densification of metals and ceramics. The mechanism behind this rapid densification has been discussed during the last few decades and is yet uncertain. During our SPS experiments we noticed oscillations in the applied pressure, related to a change in electric current. In this study, we investigated the effect of pulsed electrical current on the applied mechanical pressure and related changes in temperature. We eliminated the effect of sample shrinkage in the SPS setup and used a transparent quartz die allowing direct observation of the sample. We found that the use of pulsed direct electric current in our apparatus induces pressure oscillations with the amplitude depending on the current density. While sintering Ti samples we observed temperature oscillations resulting from pressure oscillations, which we attribute to magnetic forces generated within the SPS apparatus. The described current–pressure–temperature relations might increase understanding of the SPS process. PMID:27877472

JPRS Report, Science and Technology Japan, 3rd Microelectronics Symposium

DTIC Science & Technology

1990-04-20

Electric Power Insulating Substrate; Degree of Sintering, Thermal Conductivity of Aluminum Nitride Ultrafine Particles ; Effect of Baking Pressure on AlN Sintering; Thick Film Resistor for Use in AlN Ceramics.

Fabrication of lead-free piezoelectric Li2CO3-added (Ba,Ca)(Ti,Sn)O3 ceramics under controlled low oxygen partial pressure and their properties

NASA Astrophysics Data System (ADS)

Noritake, Kouta; Sakamoto, Wataru; Yuitoo, Isamu; Takeuchi, Teruaki; Hayashi, Koichiro; Yogo, Toshinobu

2018-02-01

Reduction-resistant lead-free (Ba,Ca)(Ti,Sn)O3 piezoceramics with high piezoelectric constants were fabricated by optimizing the amount of Li2CO3 added. Oxygen partial pressure was controlled during the sintering of (Ba,Ca)(Ti,Sn)O3 ceramics in a reducing atmosphere using H2-CO2 gas. Enhanced grain growth and a high-polarization state after poling treatment were achieved by adding Li2CO3. Optimizing the amount of Li2CO3 added to (Ba0.95Ca0.05)(Ti0.95Sn0.05)O3 ceramics sintered under a low oxygen partial pressure resulted in improved piezoelectric properties while maintaining the high sintered density. The prepared Li2CO3-added ceramic samples had homogeneous microstructures with a uniform dispersion of each major constituent element. However, the residual Li content in the 3 mol % Li2CO3-added (Ba0.95Ca0.05)(Ti0.95Sn0.05)O3 ceramics after sintering was less than 0.3 mol %. Sintered bodies of this ceramic prepared in a CO2 (1.5%)-H2 (0.3%)/Ar reducing atmosphere (PO2 = 10-8 atm at 1350 °C), exhibited sufficient electrical resistivity and a piezoelectric constant (d 33) exceeding 500 pC/N. The piezoelectric properties of this nonreducible ceramic were comparable or superior to those of the same ceramic sintered in air.

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

The effect of various sintering temperature on used refractory towards its physical properties

NASA Astrophysics Data System (ADS)

Sudibyo; Wulandari, Y. R.; Amin, M.; Azhar

2018-01-01

The used magnesia refractory from the kiln of cement industry was successfully recycled to new refractory using Kaolin as an adhesive. In this work, the temperatures of sintering were varied from 1000°C to 1500°C. The result shows that the increment temperature effects in sintering process will enhance refractory physical properties such as bulk density, cold crushing strength or pressure strength and thermal conductivity. Meanwhile, the porosity was decreased as the increase of the sintering temperature.

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

[Effect of two-step sintering method on properties of zirconia ceramic].

PubMed

Huang, Hui; Wei, Bin; Zhang, Fu-Qiang; Sun, Jing; Gao, Lian

2008-04-01

To study the influence of two-step sintering method on the sintering property, mechanical properties and microstructure of zirconia ceramic. The nano-size zirconia powder were compacted and divided into two groups, one group for one-step sintering method, another group for two-step sintering method. All samples sintered at different temperature. The relative density, three-bend strength, HV hardness, fracture toughness and microstructure of sintered block were investigated. Two-step sintering method influenced the sintering property and mechanical properties of zirconia ceramic. The maximal relative density was 98.49% at 900 degrees C/1,450 degrees C sintering temperature. There were significant difference of mechanical properties between one-step sintering and two-step sintering, the three-bend strength and fracture toughness declined, hardness increased at two-step sintering. The three-bend strength, HV hardness and fracture toughness reached to maximum value as 1,059.08 MPa +/- 75.24 MPa, 1,377.00 MPa +/- 16.37 MPa and 5.92 MPa x m1/2 +/- 0.37 MPa x m1/2 at 900 degrees C/1,450 degrees C sintering temperature respectively. Microscopy revealed the relationship between the porosity and shapes of grains was correlated to strength of the zirconia ceramics. Despite of the two-step sintering method influences the properties of zirconia, it also is a promising esthetic all-ceramic dental material.

Sintered composite medium and filter

DOEpatents

Bergman, Werner

1987-01-01

A particulate filter medium is formed of a sintered composite of 0.5 micron diameter quartz fibers and 2 micron diameter stainless steel fibers. A preferred composition is about 40 vol. % quartz and about 60 vol. % stainless steel fibers. The media is sintered at about 1100.degree. C. to bond the stainless steel fibers into a cage network which holds the quartz fibers. High filter efficiency and low flow resistance are provided by the smaller quartz fibers. High strength is provided by the stainless steel fibers. The resulting media has a high efficiency and low pressure drop similar to the standard HEPA media, with tensile strength at least four times greater, and a maximum operating temperature of about 550.degree. C. The invention also includes methods to form the composite media and a HEPA filter utilizing the composite media. The filter media can be used to filter particles in both liquids and gases.

Sintered composite filter

DOEpatents

Bergman, W.

1986-05-02

A particulate filter medium formed of a sintered composite of 0.5 micron diameter quartz fibers and 2 micron diameter stainless steel fibers is described. Preferred composition is about 40 vol.% quartz and about 60 vol.% stainless steel fibers. The media is sintered at about 1100/sup 0/C to bond the stainless steel fibers into a cage network which holds the quartz fibers. High filter efficiency and low flow resistance are provided by the smaller quartz fibers. High strength is provided by the stainless steel fibers. The resulting media has a high efficiency and low pressure drop similar to the standard HEPA media, with tensile strength at least four times greater, and a maximum operating temperature of about 550/sup 0/C. The invention also includes methods to form the composite media and a HEPA filter utilizing the composite media. The filter media can be used to filter particles in both liquids and gases.

Transport properties of undoped and Br-doped PbTe sintered at high-temperature and pressure >=4.0 GPa

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

Dong, Yongkwan; McGuire, Michael A.; Malik, Abds-Sami, E-mail: abds-sami.malik@diamondinnovations.co

2009-10-15

The thermoelectric properties of nominally undoped PbTe and Br doped PbTe materials sintered at high-pressure and high-temperature (HPHT) have been studied. All samples show n-type semiconducting behavior with negative thermopower. For undoped PbTe, four different HPHT treatments were performed at pressures between 4.0 and 6.5 GPa. PbTe doped with Br at 0.5, 1.0, 2.0, 3.0x10{sup 19} cm{sup -3} was HPHT treated at 4.0 GPa and 1045 deg. C. As the dopant concentration increases, the absolute thermopower decreases, thermal conductivity increases, and electrical resistivity decreases. At a nominal dopant concentration of 1.0x10{sup 19} cm{sup -3}, carrier mobility of 1165 cm{sup 2}/Vmore » s and dimensionless thermoelectric figure-of-merit, ZT, of around 0.27 at 300 K were obtained. These results demonstrate that HPHT post-processing is a viable and controllable way of tuning the thermoelectric properties of PbTe-based materials. - Abstract: The effect, on thermoelectric properties, of sintering undoped and Br doped PbTe at pressures >=4.0 GPa and 1045 deg. C are reported and compared with conventionally sintered materials. Display Omitted« less

Field assisted sintering of refractory carbide ceramics and fiber reinforced ceramic matrix composites

NASA Astrophysics Data System (ADS)

Gephart, Sean

The sintering behaviors of silicon carbide (SiC) and boron carbide (B4C) based materials were investigated using an emerging sintering technology known as field assisted sintering technology (FAST), also known as spark plasma sintering (SPS) and pulse electric current sintering (PECS). Sintering by FAST utilizes high density electric current, uniaxial pressure, and relatively high heating rate compared to conventional sintering techniques. This effort investigated issues of scaling from laboratory FAST system (25 ton capacity) to industrial FAST system (250 ton capacity), as well as exploring the difference in sintering behavior of single phase B4C and SiC using FAST and conventional sintering techniques including hot-pressing (HP) and pressure-less sintering (PL). Materials were analyzed for mechanical and bulk properties, including characterization of density, hardness, fracture toughness, fracture (bend) strength, elastic modulus and microstructure. A parallel investigation was conducted in the development of ceramic matrix composites (CMC) using SiC powder impregnation of fiber compacts followed by FAST sintering. The FAST technique was used to sinter several B4C and SiC materials to near theoretical density. Preliminary efforts established optimized sintering temperatures using the smaller 25 ton laboratory unit, targeting a sample size of 40 mm diameter and 8 mm thickness. Then the same B4C and SiC materials were sintered by the larger 250 ton industrial FAST system, a HP system, and PL sintering system with a targeted dense material geometry of 4 x 4 x 0.315 inches3 (101.6 x 101.6 x 8 mm3). The resulting samples were studied to determine if the sintering dynamics and/or the resulting material properties were influenced by the sintering technique employed. This study determined that FAST sintered ceramic materials resulted in consistently higher averaged values for mechanical properties as well as smaller grain size when compared to conventionally sintered materials. While FAST sintered materials showed higher average values, in general they also showed consistently larger variation in the scattered data and consequently larger standard deviation for the resulting material properties. In addition, dynamic impact testing (V50 test) was conducted on the resulting materials and it was determined that there was no discernable correlation between observed mechanical properties of the ceramic materials and the resulting dynamic testing. Another study was conducted on the sintering of SiC and carbon fiber reinforced SiC ceramic matrix composites (CMC) using FAST. There has been much interest recently in fabricating high strength, low porosity SiC CMC.s for high temperature structural applications, but the current methods of production, namely chemical vapor infiltration (CVI), melt infiltration (MI), and polymer infiltration and pyrolysis (PIP), are considered time consuming and involve material related shortcomings associated with their respective methodologies. In this study, SiC CMC.s were produced using the 25 ton laboratory unit with a target sample size of 40 mm diameter and 3 mm thickness, as well as on the larger 250 ton industrial FAST system targeting a sample size of 101.6 x 101.6 x 3 mm3 to investigate issues associated with scaling. Several sintering conditions were explored including: pressure of 35-65 MPa, temperature of 1700-1900°C, and heating rates between 50-400°C/min. The SiC fibers used in this study were coated using chemical vapor deposition (CVD) with boron nitride (BN) and pyrolytic carbon to act as a barrier layer and preserve the integrity of the fibers during sintering. Then the barrier coating was coated by an outer layer of SiC to enhance the bonding between the fibers and the SiC matrix. Microstructures of the sintered samples were examined by FE-SEM. Mechanical properties including flexural strength-deflection and stress-strain were characterized using 4-point bend testing. Tensile testing was performed on the larger 101.6 x 101.6 x 3 mm samples. The microstructures of samples sintered using the 25 ton laboratory FAST system showed a reduction in porosity and good adhesion between the fiber-fiber and fiber-matrix interface. The microstructures of samples sintered on the 250 ton industrial FAST system showed a reduction in porosity, but there was visible reaction of the fiber and fiber coatings with the surrounding matrix. Additionally, there was significant radial cracking of the fibers visible in the microstructures. There is gap in the understanding of sintering behavior between laboratory and industrial scale FAST systems. The vast majority of publications on FAST sintering have been primarily focused on small sample geometries (20 mm diameter, less than 3 mm thick). A study was coordinated to investigate the thermal properties during heating and cooling using a 250 ton industrial FAST system at 900°C using B4C and SiC materials inside the graphite die assembly. The thermal properties were then compared to the resulting material properties of the identically sintered B4C and SiC to approximately 94% relative density, at a temperature of 1950°C, pressure of 45 MPa, 10 minute hold, and heated at a rate of 100°C/min. The study determined that at 900°C there were significant thermal gradients within the system for the examined materials, and that these gradients correlated well with the material property difference of the samples sintered at higher temperatures where the gradients are presumably larger due to an increase in radiative heat loss. The observed temperatures throughout the graphite were significantly different between B4C and SiC. These temperatures also correlated well with the material properties of the sintered products which showed more substantial variation for B4C when compared to SiC which was overall less affected by thermal gradients. This was attributed to the intrinsic thermal conductivity difference between the two subject materials which was manifested as thermal gradients throughout the material and graphite die assembly. Additionally, both the observed temperature gradients throughout the graphite die assembly and the difference in temperature reading between the optical pyrometer and thermocouples were significantly larger for the 250 ton FAST system than previous publications have demonstrated experimentally or via modeling of smaller laboratory scale systems. The findings from this work showed that relative to conventional sintering methods, the FAST process demonstrated comparable or improved material and mechanical properties with a significantly shorter processing cycle. However, the results demonstrated on the 25 ton laboratory scale unit were significantly different compared to results for the same materials sintered using the 250 ton industrial scale unit. The temperature gradients observed on the 250 ton FAST unit were significantly larger than previous reports on smaller FAST units. This result showed future efforts to scale up the FAST sintering process while maintaining similar results will require careful attention to minimizing temperature gradients. This could potentially be achieved by reducing radiative heat loss during processing and/or optimizing the graphite die design and implementing heat spreaders in specific locations dependent on the host material.s thermal and electrical properties as well as the sample geometry.

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

Nitrogen Ceramics Meeting in France

DTIC Science & Technology

1988-01-21

100 and Mocellin (Ecole Polytechnique de Laus- 300*C. Other semiconductors are sensi- anne, Switzerland); this reaction is ob- tive to a very large...number of gases, but served when sintering powder mixtures at only NH3 affects the electrical resistiv- 1400-1600*C ( Mocellin , 1986). Mocellin ity of...isostatic pressure sintering; pres- Mocellin , A., Revue de Chime Mingrale, sure sintering after a preliminary heat 23 (1986), 80. 3

SYNCHROTRON RADIATION, FREE ELECTRON LASER, APPLICATION OF NUCLEAR TECHNOLOGY, ETC.: A new cell for X-ray absorption spectroscopy study under high pressure

NASA Astrophysics Data System (ADS)

Zheng, Li-Rong; Che, Rong-Zheng; Liu, Jing; Du, Yong-Hua; Zhou, Ying-Li; Hu, Tian-Dou

2009-08-01

X-ray absorption fine structure (XAFS) spectroscopy is a powerful technique for the investigation of the local environment around selected atoms in condensed matter. XAFS under pressure is an important method for the synchrotron source. We design a cell for a high pressure XAFS experiment. Sintered boron carbide is used as the anvils of this high pressure cell in order to obtain a full XAFS spectrum free from diffraction peaks. In addition, a hydraulic pump was adopted to make in-suit pressure modulation. High quality XAFS spectra of ZrH2 under high pressure (up to 13 GPa) were obtained by this cell.

Preparation and characterization of copper-graphite composites by electrical explosion of wire in liquid.

PubMed

Bien, T N; Gul, W H; Bac, L H; Kim, J C

2014-11-01

Copper-graphite nanocomposites containing 5 vol.% graphite were prepared by a powder metallurgy route using an electrical wire explosion (EEW) in liquid method and spark plasma sintering (SPS) process. Graphite rods with a 0.3 mm diameter and copper wire with a 0.2 mm diameter were used as raw materials for EEWin liquid. To compare, a pure copper and copper-graphite mixture was also prepared. The fabricated graphite was in the form of a nanosheet, onto which copper particles were coated. Sintering was performed at 900 degrees C at a heating rate of 30 degrees C/min for 10 min and under a pressure of 70 MPa. The density of the sintered composite samples was measured by the Archimedes method. A wear test was performed by a ball-on-disc tribometer under dry conditions at room temperature in air. The presence of graphite effectively reduced the wear of composites. The copper-graphite nanocomposites prepared by EEW had lower wear rates than pure copper material and simple mixed copper-graphite.

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

Fabrication of Bi2223 bulks with high critical current properties sintered in Ag tubes

NASA Astrophysics Data System (ADS)

Takeda, Yasuaki; Shimoyama, Jun-ichi; Motoki, Takanori; Kishio, Kohji; Nakashima, Takayoshi; Kagiyama, Tomohiro; Kobayashi, Shin-ichi; Hayashi, Kazuhiko

2017-03-01

Randomly grain oriented Bi2223 sintered bulks are one of the representative superconducting materials having weak-link problem due to very short coherence length particularly along the c-axis, resulting in poor intergrain Jc properties. In our previous studies, sintering and/or post-annealing under moderately reducing atmospheres were found to be effective for improving grain coupling in Bi2223 sintered bulks. Further optimizations of the synthesis process for Bi2223 sintered bulks were attempted in the present study to enhance their intergrain Jc. Effects of applied pressure of uniaxial pressing and sintering conditions on microstructure and superconducting properties have been systematically investigated. The best sample showed intergrain Jc of 2.0 kA cm-2 at 77 K and 8.2 kA cm-2 at 20 K, while its relative density was low ∼65%. These values are quite high as for a randomly oriented sintered bulk of cuprate superconductors.

Active material for fiber core made by powder-in-tube method: subsequent homogenization by means of stack-and-draw technique

NASA Astrophysics Data System (ADS)

Velmiskin, Vladimir V.; Egorova, Olga N.; Mishkin, Vladimir; Nishchev, Konstantin; Semjonov, Sergey L.

2012-04-01

A procedure for the preparation of optically homogeneous glass for fiber preforms through sintering of coarse oxide particles and further processing of the resultant glass, including several drawing and stacking steps, is described. Reducing the pressure to 10-2 Torr during sintering considerably reduced the amount of gas bubbles in Yb/Al-doped silica glass and decreased the background loss to 100 dB/km after the third drawing-stacking-consolidation cycle. For comparison, a fiber singly doped with alumina was fabricated by the same procedure as above. The level of wavelength- independent losses in that fiber was 65 dB/km.

Borax as flux on sintering of iron Ancor Steel 1000® under glow discharge

NASA Astrophysics Data System (ADS)

Ariza Suarez, H. G.; Sarmiento Santos, A.; Ortiz Otálora, C. A.

2016-02-01

This work studies the flux effect of borax (di sodium tetraborate decahydrate) on sintering of iron Ancor Steel 1000® in abnormal glow discharge. The incidence of the percentage by weight of borax and the sintering temperature in the process were observed. Samples of powder metallurgical iron were prepared with proportions of 0.50%, 2.0%, 4.0% and 6.0% by weight of borax using the procedures of powder metallurgy. The samples were sintered at 800 and 1100°C for 30min, by glow discharge at low pressure in a reducing atmosphere composed of 20% H2+80% Ar. The samples in compact green-state were analyzed by TGA-DSC to determine the fusion process and mass loss during sintering. The analysis of microhardness and density, shows that at a sintering temperature of 800°C the sample density decreases and the sample microhardness increases with respect to sintered samples without borax. Sintered samples were analysed by DRX showing the absence of precipitates.

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

Recycling of Exhaust Batteries in Lead-Foam Electrodes

NASA Astrophysics Data System (ADS)

Costanza, Girolamo; Tata, Maria Elisa

Lead and lead-alloy foams have been investigated in this research. In particular low-cost techniques for the direct production of lead-based electrodes have been analyzed and discussed in this work. The relevance of the main process parameters (powder compacting pressure, granulometry, base metal composition, sintering temperature and time) have been focused and the effect on foam morphology has been discussed too. In particular "Sintering and Dissolution Process" (SDP) and "Replication Process" (RP) have been employed and suitable modified. Both spherical urea and NaCl have been adopted in the SDP method. In the replication process it has been evidenced that the viscosity of the melt is fundamental. Furthermore the research examines lead recovery and recycling of exhaust batteries into foam-based electrodes. A novel method for the direct conversion of Pb scrap into lead foam is discussed too.

Radial basis function network learns ceramic processing and predicts related strength and density

NASA Technical Reports Server (NTRS)

Cios, Krzysztof J.; Baaklini, George Y.; Vary, Alex; Tjia, Robert E.

1993-01-01

Radial basis function (RBF) neural networks were trained using the data from 273 Si3N4 modulus of rupture (MOR) bars which were tested at room temperature and 135 MOR bars which were tested at 1370 C. Milling time, sintering time, and sintering gas pressure were the processing parameters used as the input features. Flexural strength and density were the outputs by which the RBF networks were assessed. The 'nodes-at-data-points' method was used to set the hidden layer centers and output layer training used the gradient descent method. The RBF network predicted strength with an average error of less than 12 percent and density with an average error of less than 2 percent. Further, the RBF network demonstrated a potential for optimizing and accelerating the development and processing of ceramic materials.

PRODUCCION DE PLACAS DELGADAS DE UO$sub 2$ INFORME NO. 71. (Production of Thin Plates of UO$sub 2$. Report No. 71)

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

Koll, H.; Carrea, A.J.

1962-01-01

The effect of some parameters on the fabrication of thin plates of UO/ sub 2/ by the sintering process is studied. Compacting pressures of 0.25 to 2 ton/cm/sub 2/, temperatures from 1100 to 1400 deg C, and sintering times from 1 to 3 hrs were used to determine the optimum values of these parameters. An analysis of the effect of the lubricant during the compression showed that the results were improved by the substitution of polyethylene glycol types for steric types, as the former were more easily removed from the compact and did not attack the UO/sub 2/ during sintering.more » Fracture during compression and extraction was studied. The compression law for the powder was determined, and the valid ity of the Bal'shin law was proved. The furnace atmospher is of importance to the sintered product. Two types of atmosphere were analyzed ---neutral atmosphere during sintering with final reduction in hydrogen and slightly reducing atmosphere during the entire process. An analysis of the effects on the final density and porosity showed that adding 3% H/sub 2/ to Ar produced good density and a stoichiometric oxide in the final product. It was shown that density is not a sufficient measurement to evaluate the degree of sintering. Only the combined use of density and porosity give a good evaluation. The compression pressure has a great effect on the pore size and distribution in the sintered product. Best results are obtained with high pressures, which gives small uniformly distributed pores. A metallographic study was made to determine the relation between pore size and distribution and the process parameters. Compact zones'' were observed with mean diameter from 1 to 2 mm with very reduced porosity. These zones had better hardness and resistance to corrosion and chemical attack than the rest of the material. (tr-auth)« less

Investigation of Boron addition and compaction pressure on the compactibility, densification and microhardness of 316L Stainless Steel

NASA Astrophysics Data System (ADS)

Ali, S.; Rani, A. M. A.; Altaf, K.; Baig, Z.

2018-04-01

Powder Metallurgy (P/M) is one of the continually evolving technologies used for producing metal materials of various sizes and shapes. However, some P/M materials have limited use in engineering for their performance deficiency including fully dense components. AISI 316L Stainless Steel (SS) is one of the promising materials used in P/M that combines outstanding corrosion resistance, strength and ductility for numerous applications. It is important to analyze the material composition along with the processing conditions that lead to a superior behaviour of the parts manufactured with P/M technique. This research investigates the effect of Boron addition on the compactibility, densification, sintering characteristics and microhardness of 316L SS parts produced with P/M. In this study, 0.25% Boron was added to the 316L Stainless Steel matrix to study the increase in densification of the 316L SS samples. The samples were made at different compaction pressures ranging from 100 MPa to 600 MPa and sintered in Nitrogen atmosphere at a temperature of 1200°C. The effect of compaction pressure and sintering temperature and atmosphere on the density and microhardness was evaluated. The microstructure of the samples was examined by optical microscope and microhardness was found using Vickers hardness machine. Results of the study showed that sintered samples with Boron addition exhibited high densification with increase in microhardness as compared to pure 316L SS sintered samples.

Role of Cu During Sintering of Fe0.96Cu0.04 Nanoparticles

NASA Astrophysics Data System (ADS)

Sivaprahasam, D.; Sriramamurthy, A. M.; Bysakh, S.; Sundararajan, G.; Chattopadhyay, K.

2018-04-01

Nanoparticle agglomerates of passivated Fe ( n-Fe) and Fe0.96Cu0.04 ( n-Fe0.96Cu0.04), synthesized through the levitational gas condensation (LGC) process, were compacted and sintered using the conventional powder metallurgy method. The n-Fe0.96Cu0.04 agglomerates produced lower green density than n-Fe, and when compacted under pressure beyond 200 MPa, they underwent lateral cracking during ejection attributed to the presence of a passive oxide layer. Sintering under dynamic hydrogen atmosphere can produce a higher density of compact in n-Fe0.96Cu0.04 in comparison to n-Fe. Both the results of dilatometry and thermogravimetric (TG) measurements of the samples under flowing hydrogen revealed enhancement of the sintering process as soon as the reduction of oxide layers could be accomplished. The shrinkage rate of n-Fe0.96Cu0.04 reached a value three times higher than n-Fe at a low temperature of 723 K (450 °C) during heating. This enhanced shrinkage rate was the manifestation of accumulation of Cu at the surface of the particles. The formation of a thin-surface melted layer enriched with copper during heating to isothermal holding facilitated as a medium of transport for diffusion of the elements. The compacts produced by sintering at 773 K (500 °C), with relative density 82 pct, were found to be unstable and oxidized instantly when exposed to ambient atmosphere. The stable compacts of density more than 92 pct with 300- to 450-nm grain size could only be produced when sintering was carried out at 973 K (700 °C) and beyond. The 0.22 wt pct residual oxygen obtained in the sintered compact is similar to what is used for conventional ferrous powder metallurgy products.

Fabrication of β-tricalcium phosphate composite ceramic sphere-based scaffolds with hierarchical pore structure for bone regeneration.

PubMed

He, Fupo; Qian, Guowen; Ren, Weiwei; Li, Jiyan; Fan, Peirong; Shi, Haishan; Shi, Xuetao; Deng, Xin; Wu, Shanghua; Ye, Jiandong

2017-04-24

Polymer sphere-based scaffolds, which are prepared by bonding the adjacent spheres via sintering the randomly packed spheres, feature uniform pore structure, full three-dimensional (3D) interconnection, and considerable mechanical strength. However, bioceramic sphere-based scaffolds fabricated by this method have never been reported. Due to high melting temperature of bioceramic, only limited diffusion rate can be achieved when sintering the bioceramic spheres, which is far from enough to form robust bonding between spheres. In the present study, for the first time we fabricated 3D interconnected β-tricalcium phosphate ceramic sphere-based (PG/TCP) scaffolds by introducing phosphate-based glass (PG) as sintering additive and placing uniaxial pressure during the sintering process. The sintering mechanism of PG/TCP scaffolds was unveiled. The PG/TCP scaffolds had hierarchical pore structure, which was composed by interconnected macropores (>200 μm) among spheres, pores (20–120 μm) in the interior of spheres, and micropores (1–3 μm) among the grains. During the sintering process, partial PG reacted with β-TCP, forming β-Ca2P2O7; metal ions from PG substituted to Ca2+ sites of β-TCP. The mechanical properties (compressive strength 2.8–10.6 MPa; compressive modulus 190–620 MPa) and porosity (30%–50%) of scaffolds could be tailored by manipulating the sintering temperatures. The introduction of PG accelerated in vitro degradation of scaffolds, and the PG/TCP scaffolds showed good cytocompatibility. This work may offer a new strategy to prepare bioceramic scaffolds with satisfactory physicochemical properties for application in bone regeneration.

Effect of Sintering Temperature to Physical, Magnetic Properties and Crystal Structure on Permanent Magnet BaFe12O19 Prepared From Mill Scale

NASA Astrophysics Data System (ADS)

Ramlan; Muljadi; Sardjono, Priyo; Gulo, Fakhili; Setiabudidaya, Dedi

2017-07-01

Permanent magnet of Barium hexa Ferrite with formula BaFe12O19 has been made by metallurgy powder method from raw materials : Barium carbonate (BaCO3 E-merck) and Iron Oxide (Fe2O3 from mill scale). Both of raw materials have been mixed with stoichiometry composition by using a ball mill for 24 hours. The fine powder obtained from milling process was formed by using a hydraulic press at pressure 50 MPa and continued with sintering process. The sintering temperature was varied : 1150°C, 1200°C, 1250°C and 1300°C with holding time for 1 hour. The sintered samples were characterized such as : physical properties (bulk density, porosity and shrinkage), magnetic properties (flux density, remanence, coercivity and magnetic saturation) by using VSM and crystal structure by using XRD. According characterization results show that the crystal structure of BaFe12O19 does not change after sintering process, but the grain size tends to increase. The optimum condition is achieved at temperature 1250°C, and at this condition, the sample has characterization such as : bulk density = 4.35 g/cm3, porosity = 1.03% and firing shrinkage = 11.63%, flux density = 681.1 Gauss, remanence (σr) = 20.78 emu/g, coercivity (Hc) = 2058 Oe and magnetic saturation (σs) 45.16 emu/g.

Investigation of the Deposition and Densification Parameters on the Mechanical Properties of Pressurized Spray Deposited (PSD) 3-D Printed Ceramic Components

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

Menchhofer, Paul A.; Becker, Benjamin

Oak Ridge National Laboratory (ORNL) and HotEnd Works teamed to investigate the use of pressurized spray deposition (PSD) technology for the production of ceramic parts via additive manufacturing. Scanning electron microscopy of sintered parts provided by HotEnd Works revealed voids large enough to compromise the mechanical properties of PSD manufactured parts. Scanning electron microscopy and particle size analysis of the alumina oxide powder feedstocks indicated that the powders contained some large particles and some agglomerations in the powder. Further classification of the powder feedstocks and removal of the agglomerates by sonication in the liquid used for the PSD process aremore » recommended. Analysis of sintered parts indicated that the sonic modulus for the alumina part is consistent with other known values for alumina. The density for this part was determined by standard Archimedes immersion density methods and was found to be > 99.7 % of the theoretical density for pure alumina.« less

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

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

Federal Register 2010, 2011, 2012, 2013, 2014

2012-08-23

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

77 FR 58578 - Certain Sintered Rare Earth Magnets, Methods of Making Same and Products Containing Same...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-09-21

... INTERNATIONAL TRADE COMMISSION [Investigation No. 337-TA-855] Certain Sintered Rare Earth Magnets... importation of certain sintered rare earth magnets, methods of making same and products containing same by... importation of certain sintered rare earth magnets, methods of making same and products containing same that...

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Properties and rapid low-temperature consolidation of nanocrystalline Fe-ZrO2 composite by pulsed current activated sintering

NASA Astrophysics Data System (ADS)

Kang, Hyun-Su; Ko, In-Yong; Yoon, Jin-Kook; Doh, Jung-Mann; Hong, Kyung-Tae; Shon, In-Jin

2011-02-01

Nanopowders of Fe and ZrO2 were synthesized from Fe2O3 and Zr by high-energy ball milling. The powder sizes of Fe and ZrO2 were 70 nm and 12 nm, respectively. Highly dense nanostructured 4/3Fe-ZrO2 composite was consolidated by a pulsed current activated sintering method within 1 minute from the mechanically synthesized powders (Fe-ZrO2) and horizontal milled Fe2O3+Zr powders under the 1 GPa pressure. The grain sizes of Fe and ZrO2 in the composite were calculated. The average hardness and fracture toughness values of nanostuctured 4/3Fe-ZrO2 composite were investigated.

Methods of flash sintering

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

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

2016-05-10

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

Anode composite for molten carbonate fuel cell

DOEpatents

Iacovangelo, Charles D.; Zarnoch, Kenneth P.

1983-01-01

An anode composite useful for a molten carbonate fuel cell comprised of a porous sintered metallic anode component having a porous bubble pressure barrier integrally sintered to one face thereof, said barrier being comprised of metal coated ceramic particles sintered together and to said anode by means of said metal coating, said metal coating enveloping said ceramic particle and being selected from the group consisting of nickel, copper and alloys thereof, the median pore size of the barrier being significantly smaller than that of the anode.

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.

Grain growth in uranium nitride prepared by spark plasma sintering

NASA Astrophysics Data System (ADS)

Johnson, Kyle D.; Lopes, Denise Adorno

2018-05-01

Uranium mononitride (UN) has long been considered a potential high density, high performance fuel candidate for light water reactor (LWR) and fast reactor (FR) applications. However, deployability of this fuel has been limited by the notable resistance to sintering and subsequent difficulty in producing a desirable microstructure, the high costs associated with 15N enrichment, as well as the known proclivity to oxidation and interaction with steam. In this study, the stimulation of grain growth in UN pellets sintered using SPS has been investigated. The results reveal that by using SPS and controlling temperature, time, and holding pressure, grain growth can be stimulated and controlled to produce a material featuring both a desired porosity and grain size, at least within the range of interest for nuclear fuel candidates. Grain sizes up to 31 μm were obtained using temperatures of 1650 °C and hold times of 15 min. Evaluation by EBSD reveal grain rotation and coalescence as the dominant mechanism in grain growth, which is suppressed by the application of higher external pressure. Moreover, complete closure of the porosity of the material was observed at relative densities of 96% TD, resulting in a material with sufficient porosity to accommodate LWR burnup. These results indicate that a method exists for the economic fabrication of an 15N-bearing uranium mononitride fuel with favorable microstructural characteristics compatible with use in a light water-cooled nuclear reactor.

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

PubMed

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

2017-09-20

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

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.

The permeability evolution of tuffisites and outgassing from dense rhyolitic magma

NASA Astrophysics Data System (ADS)

Heap, M. J.; Tuffen, H.; Wadsworth, F. B.; Reuschlé, T.; Castro, J. M.; Schipper, C. I.

2017-12-01

Recent observations of rhyolitic lava effusion from eruptions in Chile indicate that simultaneous pyroclastic venting facilitates outgassing. Venting from conduit-plugging lava domes is pulsatory and occurs through shallow fracture networks that deliver pyroclastic debris and exsolved gases to the surface. However, these fractures become blocked as the particulate fracture infill sinters viscously, thus drastically reducing permeability. Tuffisites, fossilized debris-filled fractures of this venting process, are abundant in pyroclastic material ejected during hybrid explosive-effusive activity. Dense tuffisite-hosting obsidian bombs ejected from Volcán Chaitén (Chile) in 2008 afford an opportunity to better understand the permeability evolution of tuffisites within low-permeability conduit plugs, wherein gas mobility is reliant upon fracture pathways. We use laboratory measurements of the permeability and porosity of tuffisites that preserve different degrees of sintering, combined with a grainsize-based sintering model and constraints on pressure-time paths from H2O diffusion, to place first-order constraints on tuffisite permeability evolution. Inferred timescales of sintering-driven tuffisite compaction and permeability loss, spanning minutes to hours, coincide with observed vent pulsations during hybrid rhyolitic activity and, more broadly, timescales of pressurization accompanying silicic lava dome extrusion. We therefore conclude that sintering exerts a first-order control on fracture-assisted outgassing from low-permeability, conduit-plugging silicic magma.

[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.

An application of powder metallurgy to dentistry.

PubMed

Oda, Y; Ueno, S; Kudoh, Y

1995-11-01

Generally, the dental casting method is used to fabricate dental prostheses made with metal. The method of fabricating dental prostheses from sintered titanium alloy has certain advantages: the elimination of casting defects, a sintering temperature that is lower than the melting point, and a shorter processing time. By examining (1) the properties of green, sintered compacts of titanium powder, (2) the effects of adding aluminum powder on the properties of green, sintered compacts of Ti-Al compound, and (3) the effects of adding copper powder on the properties of green, sintered compacts of Ti-Al-Cu compound, the authors developed a sintered titanium alloy on a trial basis. Because the properties satisfied the requirements of dental restorations, a powder metallurgical method of making dental restorations from this sintered titanium alloy was devised. Applications of such sintered titanium alloys for the metal coping of metal-ceramic crowns and denture base plates were discussed.

Thermoelectric Coolers with Sintered Silver Interconnects

NASA Astrophysics Data System (ADS)

Kähler, Julian; Stranz, Andrej; Waag, Andreas; Peiner, Erwin

2014-06-01

The fabrication and performance of a sintered Peltier cooler (SPC) based on bismuth telluride with sintered silver interconnects are described. Miniature SPC modules with a footprint of 20 mm2 were assembled using pick-and-place pressure-assisted silver sintering at low pressure (5.5 N/mm2) and moderate temperature (250°C to 270°C). A modified flip-chip bonder combined with screen/stencil printing for paste transfer was used for the pick-and-place process, enabling high positioning accuracy, easy handling of the tiny bismuth telluride pellets, and immediate visual process control. A specific contact resistance of (1.4 ± 0.1) × 10-5 Ω cm2 was found, which is in the range of values reported for high-temperature solder interconnects of bismuth telluride pellets. The realized SPCs were evaluated from room temperature to 300°C, considerably outperforming the operating temperature range of standard commercial Peltier coolers. Temperature cycling capability was investigated from 100°C to 235°C over more than 200 h, i.e., 850 cycles, during which no degradation of module resistance or cooling performance occurred.

High-intensity pulse light sintering of silver nanowire transparent films on polymer substrates: the effect of the thermal properties of substrates on the performance of silver films.

PubMed

Jiu, Jinting; Sugahara, Tohru; Nogi, Masaya; Araki, Teppei; Suganuma, Katsuaki; Uchida, Hiroshi; Shinozaki, Kenji

2013-12-07

Silver nanowire (AgNW) films with a random mesh structure have attracted considerable attention as high-performance flexible transparent electrodes that can replace the expensive and brittle ITO-sputtered films widely used in displays, touch screens, and solar cells. Methods such as heating, pressure treatment, and light treatment are usually used to obtain an optically transparent and electrically conductive film comparable to those of commercial ITO. However, the adhesion between the AgNW film and the substrate is so weak that other overcoatings or extra treatments are necessary. Here, a high-intensity pulsed light (HIPL) sintering technique was developed to rapidly and simply sinter the AgNW film and thus achieve strong adhesion and even high conductivity on these flexible polymer substrates which will be widely applied to the printing of electronic devices. The conductivity of the AgNW film closely depended on the thermal performance of substrates, and the adhesion was determined by the soft state of the substrate surface originating from the glass transition or melting of substrates with light intensity. The rapid sintering technique can be popularized to fabricate new devices on these polymer substrates by considering the thermal properties of the substrate to improve the performance of devices.

Fundamental study of transpiration cooling. [pressure drop and heat transfer data from porous metals

NASA Technical Reports Server (NTRS)

Koh, J. C. Y.; Dutton, J. L.; Benson, B. A.

1973-01-01

Isothermal and non-isothermal pressure drop data and heat transfer data generated on porous 304L stainless steel wire forms, sintered spherical stainless steel powder, and sintered spherical OFHC copper powder are reported and correlated. Pressure drop data was collected over a temperature range from 500 R to 2000 R and heat transfer data collected over a heat flux range from 5 to 15 BTU/in2/sec. It was found that flow data could be correlated independently of transpirant temperature and type (i.e., H2, N2). It was also found that no simple relation between heat transfer coefficient and specimen porosity was obtainable.

Preparation of bulk superhard B-C-N nanocomposite compact

DOEpatents

Zhao, Yusheng [Los Alamos, NM; He, Duanwei [Sichuan, CN

2011-05-10

Bulk, superhard, B--C--N nanocomposite compacts were prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture at a pressure in a range of from about 15 GPa to about 25 GPa, and sintering the pressurized encapsulated ball-milled mixture at a temperature in a range of from about 1800-2500 K. The product bulk, superhard, nanocomposite compacts were well sintered compacts with nanocrystalline grains of at least one high-pressure phase of B--C--N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compacts had a measured Vicker's hardness in a range of from about 41 GPa to about 68 GPa.

Flash (Ultra-Rapid) Spark-Plasma Sintering of Silicon Carbide

PubMed Central

Olevsky, Eugene A.; Rolfing, Stephen M.; Maximenko, Andrey L.

2016-01-01

A new ultra-rapid process of flash spark plasma sintering is developed. The idea of flash spark plasma sintering (or flash hot pressing - FHP) stems from the conducted theoretical analysis of the role of thermal runaway phenomena for material processing by flash sintering. The major purpose of the present study is to theoretically analyze the thermal runaway nature of flash sintering and to experimentally address the challenge of uncontrollable thermal conditions by the stabilization of the flash sintering process through the application of the external pressure. The effectiveness of the developed FHP technique is demonstrated by the few seconds–long consolidation of SiC powder in an industrial spark plasma sintering device. Specially designed sacrificial dies heat the pre-compacted SiC powder specimens to a critical temperature before applying any voltage to the powder volume and allowing the electrode-punches of the SPS device setup to contact the specimens and pass electric current through them under elevated temperatures. The experimental results demonstrate that flash sintering phenomena can be realized using conventional SPS devices. The usage of hybrid heating SPS devices is pointed out as the mainstream direction for the future studies and utilization of the new flash hot pressing (ultra-rapid spark plasma sintering) technique. PMID:27624641

Flash (Ultra-Rapid) Spark-Plasma Sintering of Silicon Carbide

DOE PAGES

Olevsky, Eugene A.; Rolfing, Stephen M.; Maximenko, Andrey L.

2016-09-14

A new ultra-rapid process of flash spark plasma sintering is developed. The idea of flash spark plasma sintering (or flash hot pressing - FHP) stems from the conducted theoretical analysis of the role of thermal runaway phenomena for material processing by flash sintering. The major purpose of the present study is to theoretically analyze the thermal runaway nature of flash sintering and to experimentally address the challenge of uncontrollable thermal conditions by the stabilization of the flash sintering process through the application of the external pressure. The effectiveness of the developed FHP technique is demonstrated by the few seconds–long consolidationmore » of SiC powder in an industrial spark plasma sintering device. Specially designed sacrificial dies heat the pre-compacted SiC powder specimens to a critical temperature before applying any voltage to the powder volume and allowing the electrode-punches of the SPS device setup to contact the specimens and pass electric current through them under elevated temperatures. The experimental results demonstrate that flash sintering phenomena can be realized using conventional SPS devices. The usage of hybrid heating SPS devices is pointed out as the mainstream direction for the future studies and utilization of the new flash hot pressing (ultra-rapid spark plasma sintering) technique.« less

Dense garnet-like Li5La3Nb2O12 solid electrolyte prepared by self-consolidation method

NASA Astrophysics Data System (ADS)

Zhao, Pengcheng; Xiang, Yu; Xu, Yan; Wen, Yuehua; Zhang, Wenfeng; Zhu, Xiayu; Li, Meng; Zhang, Sontong; Ming, Hai; Jin, Zhaoqing; Cao, Gaoping

2018-06-01

Li5La3Nb2O12 (LLNO) is a typical garnet-like solid electrolyte with solitary cubic structure. However, its ionic conductivity is relatively low due to the low relative density when prepared by cold isostatic pressing method, which usually involves high-pressure machines, poor productivity, tedious pressing operations, and low density. In this paper, self-consolidation method is developed to sinter dense LLNO electrolyte. Although not any pressing operations are employed in the entire process, the relative density of LLNO is promoted up to 95%, which is much higher than the reported values of 45-80%. SEM images reveal that the sample is built by huge particles in size of 80 μm indicating that there are few boundaries in the sample. Moreover, a rich content of Li-Al-O compounds is detected out in the boundary areas, which may act as sintering aids for the sample to consolidate automatically. According to the highest density, the bulk ionic conductivity of LLNO sample reaches up to 1.61 × 10-4 S cm-1 at 30 °C, which is in the same order of magnitude as the value of cubic Li7La3Zr2O12 electrolyte. This work verifies the self-consolidation mechanism for the sintering of ceramic electrolytes and could significantly facilitate the development of LLNO membrane technology.

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

PubMed

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

2018-06-11

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

Effects of compaction pressure and particle shape on the porosity and compression mechanical properties of sintered Ti6Al4V powder compacts for hard tissue implantation.

PubMed

Güden, Mustafa; Celik, Emrah; Hizal, Alpay; Altindiş, Mustafa; Cetiner, Sinan

2008-05-01

Sintered Ti6Al4V powder compacts potentially to be used in implant applications were prepared using commercially available spherical and angular powders (100-200 mum) within the porosity range of 34-54%. Cylindrical green powder compacts were cold compacted at various pressures and then sintered at 1200 degrees C for 2 h. The final percent porosity and mean pore sizes were determined as functions of the applied compaction pressure and powder type. The mechanical properties were investigated through compression testing. Results have shown that yield strength of the powder compacts of 40-42% porosity was comparable with that of human cortical bone. As compared with previously investigated Ti powder compacts, Ti6Al4V powder compacts showed higher strength at similar porosity range. Microscopic observations on the failed compact samples revealed that failure occurred primarily by the separation of interparticle bond regions in the planes 45 degrees to the loading axis. Copyright 2007 Wiley Periodicals, Inc.

Production of ZrC Matrix for Use in Gas Fast Reactor Composite Fuels

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

Vasudevamurthy, Gokul; Knight, Travis W.; Roberts, Elwyn

2007-07-01

Zirconium carbide is being considered as a candidate for inert matrix material in composite nuclear fuel for Gas fast reactors due to its favorable characteristics. ZrC can be produced by the direct reaction of pure zirconium and graphite powders. Such a reaction is exothermic in nature. The reaction is self sustaining once initial ignition has been achieved. The heat released during the reaction is high enough to complete the reaction and achieve partial sintering without any external pressure applied. External heat source is required to achieve ignition of the reactants and maintain the temperature close to the adiabatic temperature tomore » achieve higher levels of sintering. External pressure is also a driving force for sintering. In the experiments described, cylindrical compacts of ZrC were produced by direct combustion reaction. External induction heating combined with varying amounts of external applied pressure was employed to achieve varying degrees of density/porosity. The effect of reactant particle size on the product characteristics was also studied. The samples were characterized for density/porosity, composition and microstructure. (authors)« less

Synthesis and characterization of aluminium–alumina micro- and nano-composites by spark plasma sintering

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

Dash, K., E-mail: khushbudash@gmail.com; Chaira, D.; Ray, B.C.

Graphical abstract: The evolution of microstructure by varying the particle size of reinforcement in the matrix employing spark plasma sintering has been demonstrated here in Al–Al{sub 2}O{sub 3} system. An emphasis has been laid on varying the reinforcement particle size and evaluating the microstructural morphologies and their implications on mechanical performance of the composites. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size < 50 nm) reinforced in aluminium matrix were fabricated by powder metallurgy route using spark plasma sintering technique technique at a temperature of 773 K and pressure of 50 MPa. Another set of specimensmore » having composition 1, 5, 20 vol.% of alumina (average size ∼ 10 μm) had been fabricated to compare the physical as well as mechanical attributes of the microcomposite as well as the nanocomposites. These micro- and nano-composites have been characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy followed by density, microhardness and nanoindentation measurements. The alumina nanoparticles revealed an interface showing appreciable physical intimacy with the aluminium matrix compared to that of the alumina microparticles. The interfacial integrity in case of nanocomposites is better than in the microcomposite which has been studied using microscopic techniques. Spark plasma sintering imparts enhanced densification as well as matrix-reinforcement proximity which has been corroborated with the experimental results. - Highlights: • The Al–Al{sub 2}O{sub 3} micro- and nano-composites fabricated by spark plasma sintering. • Better matrix-reinforcement integrity in nanocomposites than microcomposites. • Spark plasma sintering method results in higher density and hardness values. • High density and hardness values of nanocomposites than microcomposites. • High dislocation density in spark plasma sintered Al–Al{sub 2}O{sub 3} composites. - Abstract: In the present study, an emphasis has been laid on evaluation of the microstructural morphologies and their implications on mechanical performance of the composites by varying the reinforcement particle size. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size < 50 nm) and microcomposites of 1, 5, 20 volume % of alumina (average size ∼ 10 μm) reinforced in aluminium matrix were fabricated by spark plasma sintering technique at a temperature of 773 K and pressure of 50 MPa. These micro- and nano-composites have been characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy followed by density, microhardness and nanoindentation hardness measurements. The alumina nanoparticles revealed appreciable physical intimacy with the aluminium matrix than that of alumina microparticles. The highest nanohardness recorded 0.85 GPa and 99% densification for 7 and 1 vol.% Al–Al{sub 2}O{sub 3} nancomposites respectively. Spark plasma sintering imparts enhanced densification and matrix-reinforcement proximity which have been corroborated with the experimental results.« less

Electrically-conductive proppant and methods for making and using same

DOEpatents

Cannan, Chad; Roper, Todd; Savoy, Steve; Mitchell, Daniel R.

2016-09-06

Electrically-conductive sintered, substantially round and spherical particles and methods for producing such electrically-conductive sintered, substantially round and spherical particles from an alumina-containing raw material. Methods for using such electrically-conductive sintered, substantially round and spherical particles in hydraulic fracturing operations.

Determining optimal operation parameters for reducing PCDD/F emissions (I-TEQ values) from the iron ore sintering process by using the Taguchi experimental design.

PubMed

Chen, Yu-Cheng; Tsai, Perng-Jy; Mou, Jin-Luh

2008-07-15

This study is the first one using the Taguchi experimental design to identify the optimal operating condition for reducing polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/ Fs) formations during the iron ore sintering process. Four operating parameters, including the water content (Wc; range = 6.0-7.0 wt %), suction pressure (Ps; range = 1000-1400 mmH2O), bed height (Hb; range = 500-600 mm), and type of hearth layer (including sinter, hematite, and limonite), were selected for conducting experiments in a pilot scale sinter pot to simulate various sintering operating conditions of a real-scale sinter plant We found that the resultant optimal combination (Wc = 6.5 wt%, Hb = 500 mm, Ps = 1000 mmH2O, and hearth layer = hematite) could decrease the emission factor of total PCDD/Fs (total EF(PCDD/Fs)) up to 62.8% by reference to the current operating condition of the real-scale sinter plant (Wc = 6.5 wt %, Hb = 550 mm, Ps = 1200 mmH2O, and hearth layer = sinter). Through the ANOVA analysis, we found that Wc was the most significant parameter in determining total EF(PCDD/Fs (accounting for 74.7% of the total contribution of the four selected parameters). The resultant optimal combination could also enhance slightly in both sinter productivity and sinter strength (30.3 t/m2/day and 72.4%, respectively) by reference to those obtained from the reference operating condition (29.9 t/m (2)/day and 72.2%, respectively). The above results further ensure the applicability of the obtained optimal combination for the real-scale sinter production without interfering its sinter productivity and sinter strength.

Density, Microstructure, Strength and Fractography of Spark Plasma and Conventionally Sintered Mn Steels

NASA Astrophysics Data System (ADS)

Tenerowicz-Zaba, M.; Kupkova, M.; Kabatova, M.; Dudrova, E.; Dzupon, M.; Sulowski, M.

2017-12-01

The aim of the study was to investigate Spark Plasma Sintering (SPS) of 1-3%Mn steels and compare the resultant microstructures, strengths and failure mechanisms with those of conventionally sintered materials. SPS was performed in a vacuum of 5 Pa at 1000°C for 15min under a uniaxial pressure of 20 MPa. The heating rate of 100°C/min was applied. For conventional processing, mixtures of powders were prepared in a Turbula mixer for 30 minutes. Samples were single pressed at 660 MPa, according to PN-EN ISO 2740 standard. Sintering of compacts was carried out in a laboratory tube furnace at 1120°C and 1250°C for 60 minutes in a mixture of 95%N2-5%H2. Heating and cooling rates were 75C°/min and 60°C/min, respectively. The density of SPS samples was higher (up to 7.37 g/cm3) than those after conventional sintering (up to 6.7 g/cm3). Yield strengths of SPS samples were in the range 920-1220 MPa, compared to the maximum of 602 MPa for conventionally sintered Fe-3%Mn-0.8%C. Transverse rupture strengths were the same for this alloy, 1234 MPa, but reached 1473 MPa for SPS 2Mn variant. Interfaces in SPS samples were significantly less contaminated with oxides, which is the result of a more favorable microclimate and pressure acting during SPS. These preliminary results indicate that further research on the SPS of Mn steels is warranted.

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

NASA Astrophysics Data System (ADS)

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

2016-08-01

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

[Study on friction and wear properties of dental zirconia ceramics processed by microwave and conventional sintering methods].

PubMed

Guoxin, Hu; Ying, Yang; Yuemei, Jiang; Wenjing, Xia

2017-04-01

This study evaluated the wear of an antagonist and friction and wear properties of dental zirconia ceramic that was subjected to microwave and conventional sintering methods. Ten specimens were fabricated from Lava brand zirconia and randomly assigned to microwave and conventional sintering groups. A profile tester for surface roughness was used to measure roughness of the specimens. Wear test was performed, and steatite ceramic was used as antagonist. Friction coefficient curves were recorded, and wear volume were calculated. Finally, optical microscope was used to observe the surface morphology of zirconia and steatite ceramics. Field emission scanning electron microscopy was used to observe the microstructure of zirconia. Wear volumes of microwave and conventionally sintered zirconia were (6.940±1.382)×10⁻², (7.952±1.815) ×10⁻² mm³, respectively. Moreover, wear volumes of antagonist after sintering by the considered methods were (14.189±4.745)×10⁻², (15.813±3.481)×10⁻² mm³, correspondingly. Statistically significant difference was not observed in the wear resistance of zirconia and wear volume of steatite ceramic upon exposure to two kinds of sintering methods. Optical microscopy showed that ploughed surfaces were apparent in zirconia. The wear surface of steatite ceramic against had craze, accompanied by plough. Scanning electron microscopy showed that zirconia was sintered compactly when subjected to both conventional sintering and microwave methods, whereas grains of zirconia sintered by microwave alone were smaller and more uniform. Two kinds of sintering methods are successfully used to produce dental zirconia ceramics with similar friction and wear properties.
.

Recycling positive-electrode material of a lithium-ion battery

DOEpatents

Sloop, Steven E.

2017-11-21

Examples are disclosed of methods to recycle positive-electrode material of a lithium-ion battery. In one example, the positive-electrode material is heated under pressure in a concentrated lithium hydroxide solution. After heating, the positive-electrode material is separated from the concentrated lithium hydroxide solution. After separating, the positive electrode material is rinsed in a basic liquid. After rinsing, the positive-electrode material is dried and sintered.

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.

Effect of Sintering Atmosphere and Solution Treatment on Density, Microstructure and Tensile Properties of Duplex Stainless Steels Developed from Pre-alloyed Powders

NASA Astrophysics Data System (ADS)

Murali, Arun Prasad; Mahendran, Sudhahar; Ramajayam, Mariappan; Ganesan, Dharmalingam; Chinnaraj, Raj Kumar

2017-10-01

In this research, Powder Metallurgy (P/M) of Duplex Stainless Steels (DSS) of different compositions were prepared through pre-alloyed powders and elemental powders with and without addition of copper. The powder mix was developed by pot mill for 12 h to obtain the homogeneous mixture of pre-alloyed powder with elemental compositions. Cylindrical green compacts with the dimensions of 30 mm diameter and 12 mm height were compacted through universal testing machine at a pressure level of 560 ± 10 MPa. These green compacts were sintered at 1350 °C for 2 h in hydrogen and argon atmospheres. Some of the sintered stainless steel preforms were solution treated at 1050 °C followed by water quenching. The sintered as well as solution treated samples were analysed by metallography examination, Scanning Electron Microscopy and evaluation of mechanical properties. Ferrite content of sintered and solution treated DSS were measured by Fischer Ferritoscope. It is inferred that the hydrogen sintered DSS depicted better density (94% theoretical density) and tensile strength (695 MPa) than the argon sintered steels. Similarly the microstructure of solution treated DSS revealed existence of more volume of ferrite grains than its sintered condition. Solution treated hydrogen sintered DSS A (50 wt% 316L + 50 wt% 430L) exhibited higher tensile strength of 716 MPa and elongation of 17%, which are 10-13% increment than the sintered stainless steels.

Solvent/Non-Solvent Sintering To Make Microsphere Scaffolds

NASA Technical Reports Server (NTRS)

Laurencin, Cato T.; Brown, Justin L.; Nair, Lakshmi

2011-01-01

A solvent/non-solvent sintering technique has been devised for joining polymeric microspheres to make porous matrices for use as drug-delivery devices or scaffolds that could be seeded with cells for growing tissues. Unlike traditional sintering at elevated temperature and pressure, this technique is practiced at room temperature and pressure and, therefore, does not cause thermal degradation of any drug, protein, or other biochemical with which the microspheres might be loaded to impart properties desired in a specific application. Also, properties of scaffolds made by this technique are more reproducible than are properties of comparable scaffolds made by traditional sintering. The technique involves the use of two miscible organic liquids: one that is and one that is not a solvent for the affected polymer. The polymeric microspheres are placed in a mold having the size and shape of the desired scaffold, then the solvent/non-solvent mixture is poured into the mold to fill the void volume between the microspheres, then the liquid mixture is allowed to evaporate. Some of the properties of the resulting scaffold can be tailored through choice of the proportions of the liquids and the diameter of the microspheres.

The development and characterization of a novel aluminum-copper-magnesium P/M alloy

NASA Astrophysics Data System (ADS)

Boland, Christopher Daniel

Powder metallurgy (P/M) is a metal fabrication process that is characterized by high yield and ability to be automated, as well as the resultant part complexity and reproducibility. This press and sinter process is favoured by the automotive industry. Aluminum alloy P/M parts are particularly attractive because they have a high strength to weight ratio and they can be made to have high corrosion and wear resistance. There are few commercial Al P/M alloys currently in use and they occupy a small portion of the market. To expand the use of aluminum in the industry a new alloy was created, modeled after the wrought AC2024 family of alloys. P/M 2324, with a nominal composition of Al-4.4Cu-1.5Mg, was assessed using physical, chemical and mechanical methods to help maximize alloy properties through processing. The objective of this work was to develop a viable industrial alloy. The investigation of 2324 included the evaluation of starting powders, starting composition, processing methods, secondary treatments, and industrial response. All blending and compacting was completed at Dalhousie University, while sintering was undertaken at Dalhousie and GKN Sinter Metals. The green alloy was assessed for best compaction pressure using green density and strength. The sintered alloy was assessed to determine the best press and sinter variables, using dimensional change, sintered density, apparent hardness, tensile properties and microscopy. These same sintered properties were tested to determine if sintering done on a laboratory scale could be replicated industrially. The viability of heat treatment was tested using differential scanning calorimetry, hardness and tensile properties. The alloy was also subject to modifications of Cu and Mg amounts, as well as to the addition of tin to the base composition. It was determined that compaction at 400MPa and sintering at 600°C for 20min produced the best properties for the sintered bodies. The resultant mechanical properties were attributed to a high sintered density (2.68g/cm 3 or 97% of theoretical) and strengthening mechanisms present in the Al-Cu-Mg system. These mechanisms included possible secondary phases formed in the alloy seen using microscopy and differential scanning calorimetry analyses. A T6 heat treatment of solutionizing at 495°C for 1.5h, water quench and aging for 10h was found to improve the properties of 2324. Modifications to Cu and Mg alloying additions produced few gains. However, the presence of 0.2Sn (w/o) was found to enhance the alloy. Resultant properties of the optimal alloy included an apparent hardness of 76.6HRE and an ultimate tensile strength of 367MPa. Also studied was the discrepancy observed in sintering at GKN and Dalhousie and the mechanisms at work with the addition of Sn. 2324 was adapted successfully to P/M applications. It was capable of performing against an established Al P/M industry standard, and with further testing its uses can undoubtedly be expanded.

Ammonia formation caused by the presence of water in the wet grinding of silicon nitride powder

NASA Technical Reports Server (NTRS)

Kanno, Y.; Suzuki, K.; Kuwahara, Y.

1984-01-01

Si3 N4 powder (amorphous, alpha-, and beta-Si3 N4) was mixed with MeOH containing 8.87 mol. % H2O and ground. The NH3 generation rapidly increased after a grinding time of 100 hours. Silicon nitride sintered material was chosen as one of the high temperature, high strength structural materials and studies of the control of the raw material powder, preparation of the sintered body (finding the right assistant, hot press, high pressure sintering, fracture toughness and oxidation at high temperature were performed.

Uranium migration in spark plasma sintered W/UO2 CERMETS

NASA Astrophysics Data System (ADS)

Tucker, Dennis S.; Wu, Yaqiao; Burns, Jatuporn

2018-03-01

W/UO2 CERMET samples were sintered in a Spark Plasma Sintering (SPS) furnace at various temperature under vacuum and pressure. High Resolution Transmission Electron Microscopy (HRTEM) with Energy Dispersive Spectroscopy (EDS) was performed on the samples to determine interface structures and uranium diffusion from the UO2 particles into the tungsten matrix. Local Electrode Atom Probe (LEAP) was also performed to determine stoichiometry of the UO2 particles. It was seen that uranium diffused approximately 10-15 nm into the tungsten matrix. This is explained in terms of production of oxygen vacancies and Fick's law of diffusion.

[Evaluation of alumina effects on the mechanical property and translucency of nano-zirconia all-ceramics].

PubMed

Jiang, Li; Zhao, Yong-qi; Zhang, Jing-chao; Liao, Yun-mao; Li, Wei

2010-06-01

To study the effects of alumina content on sintered density, mechanical property and translucency of zirconia nanocomposite all-ceramics. Specimens of zirconia nanocomposite all-ceramics were divided into five groups based on their alumina content which are 0% (control group), 2.5%, 5.0%, 7.5% and 10.0% respectively. The sintered densities were measured using Archimedes' method. Specimens' bending strengths were measured with three-point bending test (ISO 6872). The visible light transmittances were measured with spectrophotometric arrangements and the fractured surfaces were observed using scanning electron microscope (SEM). The control group of pure zirconia could be sintered to the theoretical density under pressure-less sintering condition. The bending strength was (1100.27 ± 54.82) MPa, the fracture toughness was (4.96 ± 0.35) MPa×m(1/2) and the transmittance could reach 17.03%. The sintered density and transmittance decreased as alumina content increased from 2.5% to 10%. However, the fracture toughness only increased slightly. In all four alumina groups, the additions of alumina had no significant effect on samples' bending strengths (P > 0.05). When the content of alumina was 10%, fracture toughness of specimens reached (6.13 ± 0.44) MPa×m(1/2) while samples' transmittance declined to 6.21%. SEM results showed that alumina particles had no significant effect on the grain size and distribution of tetragonal zirconia polycrystals. Additions of alumina to yttria-tetragonal zirconia polycrystals could influence its mechanical property and translucency. Additions of the other phase to zirconia ceramics should meet the clinical demands of strength and esthetics.

Consolidation of metallic hollow spheres by electric sintering

NASA Astrophysics Data System (ADS)

Mironov, V.; Tatarinov, A.; Lapkovsky, V.

2017-07-01

This paper considers peculiarities of the technology of production of structures from metallic hollow spheres (MHS) using magnetic fields and electric sintering. In these studies, the raw material was MHS obtained by burning of polystyrene balls coated by carbon steel. MHS had an outer diameter of 3-5 mm and a steel wall thickness of 70-120 microns. Pulsed current generators were used for electric sintering of MHS to obtain different spatial structures. Since MHS have small strength, the compressive pressure during sintering should be minimal. To improve the adhesion strength and reduce the required energy for sintering, hollow spheres were coated with copper by ion-plasma sputtering in vacuum. The coating thickness was 10-15 microns. The ferromagnetic properties of MHS allowed using of magnet fields for orientation of the spheres in the structures, as well as using of perforated tapes acting as orienting magnetic cores. Ultrasonic testing of MHS structures has been tried using through propagation of ultrasound in low kilohertz frequency range. Sensitivity of the propagation parameters to water filling of inter-spheres space and sintering temperature was demonstrated.

Aspects regarding the correlation between the physical-mechanical and tribological characteristics of composites materials reinforced with carbon fibers

NASA Astrophysics Data System (ADS)

Caliman, R.

2017-08-01

The purpose of this paper is to highlight a number of factors that influence the physical-mechanical and tribological characteristics of sintered composite materials. Such factors are grouped generally in two categories: technological parameters (pressure compacting, sintering temperature, sintering duration, heat treatment) and the receipt of sintered composite materials. In this paper is presented a program of experiments developed both in composite materials sintered polymer matrix (non-metallic) and in the metal matrix (eg., Al) which was prepared in advance a methodology original production and research for this particular type of materials. The experiments have focused development and testing of a number of 14 polymer composite and 5 composite sintered Al base, in both situations armed with carbon fiber in various forms. Tribological tests followed the establishment of the coefficient of friction and wear rate of the sliding speed at the constant values (v = 7.2 mm/s) and the normal load (N = 8 daN) and for different orientations of the fibers to the direction of sliding: normal (N type), parallel (P) and antiparallel-perpendicular (AP type).

Rub tolerance evaluation of two sintered NiCrAl gas path seal materials. [wear tests of gas turbine engine seals

NASA Technical Reports Server (NTRS)

Bill, R. C.

1978-01-01

Two strength level variations of sintered NiCrAl (about 40 percent dense), candidate high pressure turbine seal materials, were subject to rub tolerance testing against AM 355 steel blade tips. The high strength material (17 N/sq mm tensile strength) showed frictional and radial loads that were 20 to 50 percent higher than those measured for the low strength material (15.5 N/ sq mm tensile strength). Measured wear to the AM 355 blade tips was not significantly different for the two sintered NiCrAl seal materials. Wear of the sintered NiCrAl was characterized by material removal to a depth greater than the depth to which blade tips were driven into the seal, indicating self-erosion effects.

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.

Submicron cubic boron nitride as hard as diamond

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

Liu, Guoduan; Kou, Zili, E-mail: kouzili@scu.edu.cn, E-mail: yanxz@hpstar.ac.cn; Lei, Li

Here, we report the sintering of aggregated submicron cubic boron nitride (sm-cBN) at a pressure of 8 GPa. The sintered cBN compacts exhibit hardness values comparable to that of single crystal diamond, fracture toughness about 5-fold that of cBN single crystal, in combination with a high oxidization temperature. Thus, another way has been demonstrated to improve the mechanical properties of cBN besides reducing the grain size to nano scale. In contrast to other ultrahard compacts with similar hardness, the sm-cBN aggregates are better placed for potential industrial application, as their relative low pressure manufacturing perhaps be easier and cheaper.

Fracture Toughness of Advanced Ceramics at Room Temperature

PubMed Central

Quinn, George D.; Salem, Jonathan; Bar-on, Isa; Cho, Kyu; Foley, Michael; Fang, Ho

1992-01-01

This report presents the results obtained by the five U.S. participating laboratories in the Versailles Advanced Materials and Standards (VAMAS) round-robin for fracture toughness of advanced ceramics. Three test methods were used: indentation fracture, indentation strength, and single-edge pre-cracked beam. Two materials were tested: a gas-pressure sintered silicon nitride and a zirconia toughened alumina. Consistent results were obtained with the latter two test methods. Interpretation of fracture toughness in the zirconia alumina composite was complicated by R-curve and environmentally-assisted crack growth phenomena. PMID:28053447

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

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)

Performance and Reliability of Bonded Interfaces for High-Temperature Packaging. Annual Report

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

DeVoto, Douglas

2016-04-01

Current generation automotive power electronics packages utilize silicon devices and lead-free solder alloys. To meet stringent technical targets for 2020 and beyond (for cost, power density, specific power, efficiency and reliability), wide-bandgap devices are being considered since they offer advantages such as operation at higher frequencies, voltages, and temperatures. Traditional power electronics packages must be redesigned to utilize the full potential of wide-bandgap devices, and the die- and substrate-attach layers are key areas where new material development and validation is required. Present solder alloys do not meet the performance requirements for these new package designs while also meeting cost andmore » hazardous substance restrictions. Sintered silver (Ag) promises to meet the needs for die- and substrate-attach interfaces but synthesis optimization and reliability evaluation must be completed. Sintered Ag material was proposed as an alternative solution in power electronics packages almost 20 years back. However, synthesis pressure requirements up 40 MPa caused a higher complexity in the production process and more stringent flatness specifications for the substrates. Recently, several manufacturers have developed sintered Ag materials that require lower (3-5 MPa) or even no bonding pressures. Degradation mechanisms for these sintered Ag materials are not well known and need to be addressed. We are addressing these aspects to some extent in this project. We are developing generalized (i.e., independent of geometry) stress intensity factor versus cycles-to-failure relations for sintered Ag. Because sintered Ag is a relatively new material for automotive power electronics, the industry currently does not have a good understanding of recommended synthesis parameters or expected reliability under prescribed conditions. It is an important deliverable of this project to transfer findings to industry to eliminate barriers to using sintered Ag as a viable and commercialized die- and substrate-attach material. Only a few manufacturers produce sintered Ag pastes and may consider some processing conditions as proprietary. It is the goal of this project to openly explore and define best practices in order to impact the maximum number of power electronics module manufacturers and suppliers.« less

Functionally gradient material of the system Ni-MgO, Ni-NiO, Ni-Si3N4 or Al-AlN, by pressureless sintering

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

Atarashiya, Koji; Kurokawa, Kazuya; Nagai, Tadao

1992-08-01

Generally speaking, the preparation of FGM-blocks, especially in the metal-nitride systems, by the method of powder metallurgy needs an extremely high temperature and high pressure. But, in this work using a ductile nickel metal powder or an ultrafine particle, the FGM-blocks were easily prepared using a powder metallurgy at a lower temperature. A mixture of a metallic powder and a non-metallic powder whose contents were gradually changed was pressed in a steel die under pressure of 20-32 MPa. These green compacts were heated at 900-1573 K in controlled atmosphere under null pressure. The FGM-blocks prepared by this method were characterizedmore » by their properties and were used in joinings. The joinings of metal/FGM/ceramics, metal/FGM and ceramics/FGM were completely accomplished at 900-1573 K. 6 refs.« 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.

A constitutive model and numerical simulation of sintering processes at macroscopic level

NASA Astrophysics Data System (ADS)

Wawrzyk, Krzysztof; Kowalczyk, Piotr; Nosewicz, Szymon; Rojek, Jerzy

2018-01-01

This paper presents modelling of both single and double-phase powder sintering processes at the macroscopic level. In particular, its constitutive formulation, numerical implementation and numerical tests are described. The macroscopic constitutive model is based on the assumption that the sintered material is a continuous medium. The parameters of the constitutive model for material under sintering are determined by simulation of sintering at the microscopic level using a micro-scale model. Numerical tests were carried out for a cylindrical specimen under hydrostatic and uniaxial pressure. Results of macroscopic analysis are compared against the microscopic model results. Moreover, numerical simulations are validated by comparison with experimental results. The simulations and preparation of the model are carried out by Abaqus FEA - a software for finite element analysis and computer-aided engineering. A mechanical model is defined by the user procedure "Vumat" which is developed by the first author in Fortran programming language. Modelling presented in the paper can be used to optimize and to better understand the process.

Lower sintering temperature of nanostructured dense ceramics compacted from dry nanopowders using powerful ultrasonic action

NASA Astrophysics Data System (ADS)

Khasanov, O.; Reichel, U.; Dvilis, E.; Khasanov, A.

2011-10-01

Nanostructured high dense zirconia ceramics have been sintered from dry nanopowders compacted by uniaxial pressing with simultaneous powerful ultrasonic action (PUA). Powerful ultrasound with frequency of 21 kHz was supplied from ultrasonic generator to the mold, which was the ultrasonic wave-guide. Previously the mold was filled by non-agglomerated zirconia nanopowder having average particle size of 40 nm. Any binders or plasticizers were excluded at nanopowder processing. Compaction pressure was 240 MPa, power of ultrasonic generator at PUA was 1 kW and 3 kW. The fully dense zirconia ceramics has been sintered at 1345°C and high-dense ceramics with a density of 99.1%, the most grains of which had the sizes Dgr <= 200 nm, has been sintered at low sintering temperature (1325°C). Applied approach prevents essential grain growth owing to uniform packing of nanoparticles under vibrating PU-action at pressing, which provides the friction forces control during dry nanopowder compaction without contaminating binders or plasticizers.

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

NASA Astrophysics Data System (ADS)

Peng, Qin; Yang, Bin; Friedrich, Bernd

2018-01-01

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

Application of Box-Behnken Design and Response Surface Methodology for Surface Roughness Prediction Model of CP-Ti Powder Metallurgy Components Through WEDM

NASA Astrophysics Data System (ADS)

Das, Arunangsu; Sarkar, Susenjit; Karanjai, Malobika; Sutradhar, Goutam

2018-04-01

The present work was undertaken to investigate and characterize the machining parameters (such as surface roughness, etc.) of uni-axially pressed commercially pure titanium sintered powder metallurgy components. Powder was uni-axially pressed at designated pressure of 840 MPa to form cylindrical samples and the green compacts were sintered at 0.001 mbar for about 4 h with sintering temperature varying from 1350 to 1450 °C. The influence of the sintering temperature, pulse-on and pulse-off time at wire-EDM on the surface roughness of the preforms has been investigated thoroughly. Experiments were conducted under different machining parameters in a CNC operated wire-cut EDM. The surface roughness of the machined surface was measured and critically analysed. The optimum surface roughness was achieved under the conditions of 6 μs pulse-on time, 9 μs pulse-off time and at sintering temperature of 1450 °C.

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

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

Nunn, S.D.

1991-01-01

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

Method of sintering materials with microwave radiation

DOEpatents

Kimrey, Jr., Harold D.; Holcombe, Jr., Cressie E.; Dykes, Norman L.

1994-01-01

A method of sintering ceramic materials following: A compacted article comprising inorganic particles coated with carbon is provided, the carbon providing improved microwave coupling. The compacted article is then heated by microwave radiation to a temperature and for a period of time sufficient to sinter the compacted article.

[Application of sintered Ti powder to dental prostheses].

PubMed

Hikosaka, Tatsuya; Tanaka, Yoshinobu; Hoshiai, Kazumoto; Kanazawa, Takeshi; Nakamura, Yoshinori; Tsuda, Kenji; Ohasi, Hideya

2005-04-01

Powder metallurgy is a metal processing technology. Porous titanium produced from powder is widely used. The method is applied to titanium, which is not easy to cast as it sinters under melting point. In prosthetic dentistry, powder metallurgy can be applied to high fusing metal that is biocompatible. In this study, we examined the mechanical characteristics of the Ti sheet produced by sintering and discussed its application to dental prosthesis manufacturing. Ti sheets of 1-mm thickness, in which a binder was added to spherical Ti powder, were produced with the Doctor Blade Method. The sintering was carried out between 900-1150 degrees C at 6 temperatures. The sintered compact was evaluated by dimensional change rate, hardness test, bending strength, tensile strength and SEM observation. Another compact was sintered on the refractory cast. Mechanical strength significantly increased with sintering temperature. In addition, excellent mechanical strength was acquired by adding crushed powder and performing the de-binder process. In the sintering on the refractory cast, pre-baking for more than 100 minutes and sintering at over 1050 degrees C was needed for practical application. It thus seems possible to apply sintered titanium to dental prostheses. However, it will be necessary to examine the control of the shrinkage of the sintered compact in the future too.

Method of forming aluminum oxynitride material and bodies formed by such methods

DOEpatents

Bakas, Michael P [Ammon, ID; Lillo, Thomas M [Idaho Falls, ID; Chu, Henry S [Idaho Falls, ID

2010-11-16

Methods of forming aluminum oxynitride (AlON) materials include sintering green bodies comprising aluminum orthophosphate or another sacrificial material therein. Such green bodies may comprise aluminum, oxygen, and nitrogen in addition to the aluminum orthophosphate. For example, the green bodies may include a mixture of aluminum oxide, aluminum nitride, and aluminum orthophosphate or another sacrificial material. Additional methods of forming aluminum oxynitride (AlON) materials include sintering a green body including a sacrificial material therein, using the sacrificial material to form pores in the green body during sintering, and infiltrating the pores formed in the green body with a liquid infiltrant during sintering. Bodies are formed using such methods.

Dispensing of high concentration Ag nano-particles ink for ultra-low resistivity paper-based writing electronics.

PubMed

Wang, Fuliang; Mao, Peng; He, Hu

2016-02-17

Paper-based writing electronics has received a lot of interest recently due to its potential applications in flexible electronics. To obtain ultra-low resistivity paper-based writing electronics, we developed a kind of ink with high concentration of Ag Nano-particles (up to 80 wt%), as well as a related dispensing writing system consisting an air compressor machine and a dispenser. Additionally, we also demonstrated the writability and practical application of our proposed ink and writing system. Based on the study on the effect of sintering time and pressure, we found the optimal sintering time and pressure to obtain high quality Ag NPs wires. The electrical conductivity of nano-silver paper-based electronics has been tested using the calculated resistivity. After hot-pressure sintering at 120 °C, 25 MPa pressure for 20 minutes, the resistivity of silver NPs conductive tracks was 3.92 × 10(-8) (Ωm), only 2.45 times of bulk silver. The mechanical flexibility of nano-silver paper-based electronics also has been tested. After 1000 bending cycles, the resistivity slightly increased from the initial 4.01 × 10(-8) to 5.08 × 10(-8) (Ωm). With this proposed ink preparation and writing system, a kind of paper-based writing electronics with ultra-low resistivity and good mechanical flexibility was achieved.

Method of sintering materials with microwave radiation

DOEpatents

Kimrey, H.D. Jr.; Holcombe, C.E. Jr.; Dykes, N.L.

1994-06-14

Disclosed is a method of sintering ceramic materials. A compacted article comprising inorganic particles coated with carbon is provided, the carbon providing improved microwave coupling. The compacted article is then heated by microwave radiation to a temperature and for a period of time sufficient to sinter the compacted article. No Drawings

Underwater explosive compaction-sintering of tungsten-copper coating on a copper surface

NASA Astrophysics Data System (ADS)

Chen, Xiang; Li, Xiaojie; Yan, Honghao; Wang, Xiaohong; Chen, Saiwei

2018-01-01

This study investigated underwater explosive compaction-sintering for coating a high-density tungsten-copper composite on a copper surface. First, 50% W-50% Cu tungsten-copper composite powder was prepared by mechanical alloying. The composite powder was pre-compacted and sintered by hydrogen. Underwater explosive compaction was carried out. Finally, a high-density tungsten-copper coating was obtained by diffusion sintering of the specimen after explosive compaction. A simulation of the underwater explosive compaction process showed that the peak value of the pressure in the coating was between 3.0 and 4.8 GPa. The hardness values of the tungsten-copper layer and the copper substrate were in the range of 87-133 and 49 HV, respectively. The bonding strength between the coating and the substrate was approximately 100-105 MPa.

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

NASA Astrophysics Data System (ADS)

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

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

High pressure infiltration sintering behavior of WC-Co alloys

NASA Astrophysics Data System (ADS)

Fan, Xiaoqin; He, Duanwei; Wang, Pei; Li, Dong; Liu, Yinjuan; Ma, Dejiang; Du, Yanchun; Gao, Shangpan; Kou, Zili

2016-10-01

In this paper, two average tungsten carbide particle sizes of 2, 0.5 μm are placed respectively, in contact with a WC-16Co substrate, pressed at the pressure of 4.5-5.5 GPa, and heated to temperatures ranging from 1350°C to 1500°C in a large-volume cubic press. During the process Co was forced out of the WC-16Co substrate into the compressed powder. The resulting infiltrated samples were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), Vickers hardness and cutting performance tests. The results of XRD confirmed that the sintered bulks have WC and Co phases. The scanning electron microscopy (SEM) analysis reveals that the WC grains in well-sintered alloys are round in shape and cobalt with lower content is uniformly dispersed in the WC grain boundaries. The sintered sub-micron WC-Co alloy with a cobalt content of 3.8 wt% exhibits a prominent combination of high hardness value of 23.1 GPa and a large fracture toughness value of 8.6 MPa m½. The high-speed cutting tests indicating its cutting performance is significantly superior to the commercial YG6X (WC-6 wt%Co with WC grain size of 0.5 μm).

On the factors affecting porosity dissolution in selective laser sintering process

NASA Astrophysics Data System (ADS)

Ly, H.-B.; Monteiro, E.; Dal, M.; Regnier, G.

2018-05-01

Selective Laser Sintering process is one of the additive manufacturing techniques in which parts are manufactured layer by layer. During such process, gas bubbles are formed in the melted polymer due to faster polymer grains coalescence at surface than deeper in the powder bed. Although gas diffusion is possible through the polymer melt, it's usual that some porosities remain in the final part if their initial sizes are too big and solidification time too short. In this contribution, a bubble dissolution model involving fluid dynamics and mass transport has been developed to study factors affecting porosity resorption kinetic. In this model, gas diffusion follows Fick's laws and the melted polymer is supposed Newtonian. At the polymer/gas interface, surface tension is considered and Henry's law is used to relate the partial pressure of gas with its concentration in the fluid. This problem is solved numerically by means of the finite element method in 1D. After validation of the numerical tool, the influence on dissolution time of several parameters (e.g. the initial size and form of gas porosities, the viscosity, the diffusion coefficient, the surface tension constant or the ambient pressure) has been examined.

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

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

DOE PAGES

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

2016-07-19

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

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.

Numerical study of the process parameters in spark plasma sintering (sps)

NASA Astrophysics Data System (ADS)

Chowdhury, Redwan Jahid

Spark plasma sintering (SPS) is one of the most widely used sintering techniques that utilizes pulsed direct current together with uniaxial pressure to consolidate a wide variety of materials. The unique mechanisms of SPS enable it to sinter powder compacts at a lower temperature and in a shorter time than the conventional hot pressing, hot isostatic pressing and vacuum sintering process. One of the limitations of SPS is the presence of temperature gradients inside the sample, which could result in non-uniform physical and microstructural properties. Detailed study of the temperature and current distributions inside the sintered sample is necessary to minimize the temperature gradients and achieve desired properties. In the present study, a coupled thermal-electric model was developed using finite element codes in ABAQUS software to investigate the temperature and current distributions inside the conductive and non-conductive samples. An integrated experimental-numerical methodology was implemented to determine the system contact resistances accurately. The developed sintering model was validated by a series of experiments, which showed good agreements with simulation results. The temperature distribution inside the sample depends on some process parameters such as sample and tool geometry, punch and die position, applied current and thermal insulation around the die. The role of these parameters on sample temperature distribution was systematically analyzed. The findings of this research could prove very useful for the reliable production of large size sintered samples with controlled and tailored properties.

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.

Method of producing amorphous thin films

DOEpatents

Brusasco, Raymond M.

1992-01-01

Disclosed is a method of producing thin films by sintering which comprises: a. coating a substrate with a thin film of an inorganic glass forming parulate material possessing the capability of being sintered, and b. irridiating said thin film of said particulate material with a laser beam of sufficient power to cause sintering of said material below the temperature of liquidus thereof. Also disclosed is the article produced by the method claimed.

Method of producing amorphous thin films

DOEpatents

Brusasco, R.M.

1992-09-01

Disclosed is a method of producing thin films by sintering which comprises: (a) coating a substrate with a thin film of an inorganic glass forming material possessing the capability of being sintered; and (b) irradiating said thin film of said particulate material with a laser beam of sufficient power to cause sintering of said material below the temperature of liquidus thereof. Also disclosed is the article produced by the method claimed. 4 figs.

Microwave sintering of single plate-shaped articles

DOEpatents

Katz, Joel D.; Blake, Rodger D.

1995-01-01

Apparatus and method for high temperature sintering of plate-shaped articles of alumina, magnesia, silica, yttria, zirconia, and mixtures thereof using microwave radiation. An article is placed within a sintering structure located within a sintering container which is placed in a microwave cavity for heating. The rates at which heating and cooling take place is controlled.

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

NASA Astrophysics Data System (ADS)

Antonov, E. N.; Krotova, L. I.; Minaev, N. V.; Minaeva, S. A.; Mironov, A. V.; Popov, V. K.; Bagratashvili, V. N.

2015-11-01

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

Sintering Theory and Practice

NASA Astrophysics Data System (ADS)

German, Randall M.

1996-01-01

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

The Influence of Sintering Method on Kaolin-Based Geopolymer Ceramics with Addition of Ultra High Molecular Weight Polyethylene as Binder

NASA Astrophysics Data System (ADS)

Romisuhani, A.; AlBakri, M. M.; Kamarudin, H.; Andrei, S. V.

2017-11-01

The influence of sintering method on kaolin-based geopolymer ceramics with addition of Ultra High Molecular Weight Polyethylene as binder were studied. Geopolymer were formed at room temperature from kaolin and sodium silicate in a highly alkaline medium, followed by curing and drying at 80 °C. 12 M of sodium hydroxide solution were mixed with sodium silicate at a ratio of 0.24 to form alkaline activator. Powder metallurgy technique were used in order to produce kaolin geopolymer ceramics with addition of Ultra High Molecular Weight Polyethylene. The samples were heated at temperature of 1200 °C with two different sintering method which are conventional method and two-step sintering method. The strength and density were tested.

Method for directly recovering fluorine from gas streams

DOEpatents

Orlett, Michael J.; Saraceno, Anthony J.

1981-01-01

This invention is a process for the direct recovery of gaseous fluorine from waste-gas streams or the like. The process comprises passing the gas stream through a bed of anhydrous K.sub.3 NiF.sub.6 pellets to fluorinate the same to K.sub.3 NiF.sub.7 and subsequently desorbing the fluorine by heating the K.sub.3 NiF.sub.7 pellets to a temperature re-converting them to K.sub.3 NiF.sub.6. The efficiency of the fluorine-absorption step is maximized by operating in a selected and conveniently low temperature. The desorbed fluorine is highly pure and is at a pressure of several atmospheres. Preferably, the K.sub.3 NiF.sub.6 pellets are prepared by a method including the steps of forming agglomerates of hydrated K.sub.3 NiF.sub.5, sintering the agglomerates to form K.sub.3 NiF.sub.5 pellets of enhanced reactivity with respect to fluorine, and fluorinating the sintered pellets to K.sub.3 NiF.sub.6.

Sintering Uranium Dioxide of Domestic Production. Report No. 78; SINTERIZACION DE DIOXIDO DE URANIO DE PRODUCCION NACIONAL. Informe No. 78

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

Carrea, A.J.

1963-01-01

After a brief indication of the uranium- oxygen equilibrium and the methods for the preparation of UO/sub 2/, the sintering of UO/sub 2/ is considered. The effects of various sintering atmospheres on the properties of the product are discussed and tabulated. The method used for the processing of domestic ores for the preparation of UO/sub 2/ and the fabricition of the sintered UO/sub 2/are described. The properties of the product obtained are illustrated graphically. (J.S.R.)

Preparation of Cu and Fly Ash Composite by Powder Metallurgy Technique

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

Chew, P. Y.; Lim, P. S.; Ng, M. C.

2011-03-30

Cu and Fly Ash (FA) mixtures with different weight percentages were prepared. Pellets of the mixture powder were produced with the dimension of 17.7 mm in diameter and 10-15 mm in height. These different composites were compacted at a constant pressure of 280 MPa. One of the selected weight percentages was then compacted to form into pellet and sintered at different temperatures which were at 900, 950 and 1000 deg. C respectively for 2 hours. Density of green pellet was measured before sintered in furnace. After sintering, all the pellets with different temperatures were re-weighed and sintered density were calculated.more » The densification of the green and sintered pellets was required to be measured as one of the parameter in selection of the best material properties. Porosity of the pellet shall not be ignored in order to analyze the close-packed particles stacking in the pellet. SEM micrograph had been captured to observe the presence of pores and agglomeration of particles in the sample produced.« less

The fracture strength of cryomilled 99.7 Al nanopowders consolidated by high frequency induction sintering

NASA Astrophysics Data System (ADS)

El-Danaf, Ehab A.; Baig, Muneer; Almajid, Abdulhakim A.; Soliman, Mahmoud S.

2014-08-01

Mechanical Attrition of metallic powders induces severe plastic deformation and consequently reduces the average grain size. Powders of 99.7 Al (45μm particle size), cryomilled for 7 hrs having a crystal size of ~ 20 nm, were consolidated by high frequency induction sintering under a constant pressure of 50 MPa and at two temperatures of 500 and 550 °C for two sintering dwell times of 1 and 3 minutes at a constant heating rate of 400 °C/min. The bright field TEM image and X-ray line broadening technique, for the cryomilled powders, were used to measure-the crystallite size. Simple compression at an initial strain rate of 10-4 s-1 was conducted at room temperature, 373 and 473 K, and the yield strength was documented and correlated with the sintering parameters. The as-received 99.7 Al powders-consolidated using one of the sintering parameters was used as a reference material to compare the mechanical properties. Hardness, density and crystal size of the consolidated sample, that gave the highest yield and fracture strength, were measured.

Experimental and textural investigation of welding: effects of compaction, sintering, and vapor-phase crystallization in the rhyolitic Rattlesnake Tuff

NASA Astrophysics Data System (ADS)

Grunder, Anita L.; Laporte, Didier; Druitt, Tim H.

2005-04-01

The abrupt changes in character of variably welded pyroclastic deposits have invited decades of investigation and classification. We conducted two series of experiments using ash from the nonwelded base of the rhyolitic Rattlesnake Tuff of Oregon, USA, to examine conditions of welding. One series of experiments was conducted at atmospheric pressure (1 At) in a muffle furnace with variable run times and temperature and another series was conducted at 5 MPa and 600 °C in a cold seal apparatus with variable run times and water contents. We compared the results to a suite of incipiently to densely welded, natural samples of the Rattlesnake Tuff. Experiments at 1 At required a temperature above 900 °C to produce welding, which is in excess of the estimated pre-eruptive magmatic temperature of the tuff. The experiments also yielded globular clast textures unlike the natural tuff. During the cold-seal experiments, the gold sample capsules collapsed in response to sample densification. Textures and densities that closely mimic the natural suite were produced at 5 MPa, 600 °C and 0.4 wt.% H 2O, over run durations of hours to 2 days. Clast deformation and development of foliation in 2-week runs were greater than in natural samples. Both more and less water reduced the degree of welding at otherwise constant run conditions. For 5 MPa experiments, changes in the degree of foliation of shards and of axial ratios of bubble shards and non-bubble (mainly platy) shards, are consistent with early densification related to compaction and partial rotation of shards into a foliation. Subsequent densification was associated with viscous deformation as indicated by more sintered contacts and deformation of shards. Sintering (local fusion of shard-shard contacts) was increasingly important with longer run times, higher temperatures, and greater pressures. During runs with high water concentrations, sintering was rare and adhesion between clasts was dominated by precipitation of sublimates in pore spaces. A few tenths wt.% H 2O in the rhyolite glass promote the development of welding by sharp reduction of glass viscosity. Large amounts of water inhibit welding by creating surface sublimates that interfere with sintering and may exert fluid pressure counter to lithostatic load if sintering and vapor-phase sublimates seal permeability in the tuff.

Dispensing of high concentration Ag nano-particles ink for ultra-low resistivity paper-based writing electronics

PubMed Central

Wang, Fuliang; Mao, Peng; He, Hu

2016-01-01

Paper-based writing electronics has received a lot of interest recently due to its potential applications in flexible electronics. To obtain ultra-low resistivity paper-based writing electronics, we developed a kind of ink with high concentration of Ag Nano-particles (up to 80 wt%), as well as a related dispensing writing system consisting an air compressor machine and a dispenser. Additionally, we also demonstrated the writability and practical application of our proposed ink and writing system. Based on the study on the effect of sintering time and pressure, we found the optimal sintering time and pressure to obtain high quality Ag NPs wires. The electrical conductivity of nano-silver paper-based electronics has been tested using the calculated resistivity. After hot-pressure sintering at 120 °C, 25 MPa pressure for 20 minutes, the resistivity of silver NPs conductive tracks was 3.92 × 10−8 (Ωm), only 2.45 times of bulk silver. The mechanical flexibility of nano-silver paper-based electronics also has been tested. After 1000 bending cycles, the resistivity slightly increased from the initial 4.01 × 10−8 to 5.08 × 10−8 (Ωm). With this proposed ink preparation and writing system, a kind of paper-based writing electronics with ultra-low resistivity and good mechanical flexibility was achieved. PMID:26883558

Modeling Ultra-fast assembly and sintering of gold nanostructures

NASA Astrophysics Data System (ADS)

Lane, J. Matthew D.; Salerno, K. Michael; Grest, Gary S.; Fan, Hongyou

We use fully atomistic simulations to understand the role of extreme pressure in the assembly and sintering of fcc superlattices of alkanethiol-coated gold nanocrystals into larger nanostructures. Recent quasi-isentropic experiments have shown that 1D, 2D and 3D nanostructures can be formed and recovered from dynamic compression experiments on Sandia's Veloce pulsed power accelerator. Here, we describe the role of coating properties, such as ligand length and grafting density, on ligand migration and deformation processes during pressure-driven coalescence of metal nano cores into permanent nanowires, nanosheets and 3D structures. The role of uniaxial vs isotropic pressure and the effects of compression along various superlattice orientations will be discussed. Sandia National Laboratories is a multi-mission laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

Simultaneous Luminescence Pressure and Temperature Measurement System for Hypersonic Wind Tunnels

NASA Technical Reports Server (NTRS)

Buck, Gregory M.

1995-01-01

Surface pressures and temperatures are determined from visible emission brightness and green-to-red color ratioing of induced luminescence from a ceramic surface with an organic dye coating. A ceramic-dye matrix of porous silica ceramic with an adsorbed dye is developed for high-temperature pressure sensitivity and stability (up to 150 C). Induced luminescence may be excited using a broad range of incident radiation from visible blue light (488-nm wavelength) to the near ultraviolet (365 nm). Ceramic research models and test samples are fabricated using net-form slip-casting and sintering techniques. Methods of preparation and effects of adsorption film thickness on measurement sensitivity are discussed. With the present 8-bit imaging system a 10% pressure measurement uncertainty from 50 to 760 torr is estimated, with an improvement to 5% from 3 to 1500 torr with a 12-bit imaging system.

Alumina ceramic based high-temperature performance of wireless passive pressure sensor

NASA Astrophysics Data System (ADS)

Wang, Bo; Wu, Guozhu; Guo, Tao; Tan, Qiulin

2016-12-01

A wireless passive pressure sensor equivalent to inductive-capacitive (LC) resonance circuit and based on alumina ceramic is fabricated by using high temperature sintering ceramic and post-fire metallization processes. Cylindrical copper spiral reader antenna and insulation layer are designed to realize the wireless measurement for the sensor in high temperature environment. The high temperature performance of the sensor is analyzed and discussed by studying the phase-frequency and amplitude-frequency characteristics of reader antenna. The average frequency change of sensor is 0.68 kHz/°C when the temperature changes from 27°C to 700°C and the relative change of twice measurements is 2.12%, with high characteristic of repeatability. The study of temperature-drift characteristic of pressure sensor in high temperature environment lays a good basis for the temperature compensation methods and insures the pressure signal readout accurately.

Microwave sintering of single plate-shaped articles

DOEpatents

Katz, J.D.; Blake, R.D.

1995-07-11

Apparatus and method are disclosed for high temperature sintering of plate-shaped articles of alumina, magnesia, silica, yttria, zirconia, and mixtures thereof using microwave radiation. An article is placed within a sintering structure located within a sintering container which is placed in a microwave cavity for heating. The rates at which heating and cooling take place is controlled. 2 figs.

Effect of consolidation techniques on the properties of Al matrix composite reinforced with nano Ni-coated SiC

NASA Astrophysics Data System (ADS)

Abolkassem, Shimaa A.; Elkady, Omayma A.; Elsayed, Ayman H.; Hussein, Walaa A.; Yehya, Hosam M.

2018-06-01

Al /Ni-SiC composite was prepared via powder metallurgy technique. SiC particles were coated with 10 wt% nano nickel by electroless deposition, then mixed by three percents (5, 10 and 15 wt%) with Al powder in a ball mill using 10:1 ball to powder ratio for 5 h. Three types of sintering techniques were used to prepare the composite. Uniaxial cold compacted samples were sintered in a vacuum furnace at 600 °C for 1 h. The second group was the vacuum sintered samples which were post-processed by hot isostatic press (HIP) at 600 °C for 1hr under the pressure of 190 MPa. The third group was the hot pressed samples that were consolidated at 550 °C under the uniaxial pressure of 840 MPa. The results showed that the hot pressed samples have the highest densification values (97-100%), followed by the HIP samples (94-98%), then come the vacuum sintered ones (92-96%). X-ray diffraction analysis (XRD) indicated the presence of Al and Al3Ni, which means that all SiC particles were encapsulated with nickel as short peaks for SiC were observed. Hardness results revealed that HIP samples have the highest hardness values. The magnetization properties were improved by increasing SiC/Ni percent, and HIP samples showed the highest magnetization parameter values.

Titanium dental copings prepared by a powder metallurgy method: a preliminary report.

PubMed

Eriksson, Mikael; Andersson, Matts; Carlström, Elis

2004-01-01

The purpose of this study was to determine if the Procera pressed-powder method can be used to fabricate titanium copings. Commercially pure titanium powder was used to prepare the copings. The powder was pressed onto an enlarged tooth preparation die of aluminum using cold isostatic pressing. The outer shape of the coping was formed using a Procera milling machine, and the copings were vacuum sintered. Titanium copings could be prepared using this method. The density of the sintered copings reached 97% to 99%+ of theoretic density, and the copings showed ductile behavior after sintering. Enlarging the tooth preparation die to compensate for the sintering shrinkage could optimize the final size of the copings. Ductile and dense titanium dental copings can be produced with powder-metal processing using cold isostatic pressing, followed by milling and sintering to final shape. The forming technique has, if properly optimized, a potential of becoming a more cost-efficient production method than spark erosion.

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

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.

Method of forming a joint

DOEpatents

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

2006-08-22

A method of joining at least two sintered bodies to form a composite structure, including providing a first multicomponent metallic oxide having a perovskitic or fluorite crystal structure; providing a second sintered body including a second multicomponent metallic oxide having a crystal structure of the same type as the first; and providing at an interface a joint material containing at least one metal oxide containing at least one metal identically contained in at least one of the first and second multicomponent metallic oxides. The joint material is free of cations of Si, Ge, Sn, Pb, P and Te and has a melting point below the sintering temperatures of both sintered bodies. The joint material is heated to a temperature above the melting point of the metal oxide(s) and below the sintering temperatures of the sintered bodies to form the joint. Structures containing such joints are also disclosed.

In-situ resource utilization in the design of advanced lunar facilities

NASA Technical Reports Server (NTRS)

1990-01-01

Resource utilization will play an important role in the establishment and support of a permanently manned lunar base. At the University of Houston - College of Architecture and the Sasakawa International Center for Space Architecture, a study team recently investigated the potential use of lunar in-situ materials in the design of lunar facilities. The team identified seven potential lunar construction materials; concrete, sulfur concrete, cast basalt, sintered basalt, glass, fiberglass, and metals. Analysis and evaluation of these materials with respect to their physical properties, processes, energy requirements, resource efficiency, and overall advantages and disadvantages lead to the selection of basalt materials as the more likely construction material for initial use on a lunar base. Basalt materials can be formed out of in-situ lunar regolith, with minor material beneficiation, by a simple process of heating and controlled cooling. The team then conceptualized a construction system that combines lunar regolith sintering and casting to make pressurized structures out of lunar resources. The design uses a machine that simultaneously excavates and sinters the lunar regolith to create a cylindrical hole, which is then enclosed with cast basalt slabs, allowing the volume to be pressurized for use as a living or work environment. Cylinder depths of up to 4 to 6 m in the lunar mare or 10 to 12 m in the lunar highlands are possible. Advantages of this construction system include maximum resource utilization, relatively large habitable volumes, interior flexibility, and minimal construction equipment needs. Conclusions of this study indicate that there is significant potential for the use of basalt, a lunar resource derived construction material, as a low cost alternative to Earth-based materials. It remains to be determined when in lunar base phasing this construction method should be implemented.

Effects of sintering time and temperature to the characteristics of FeCrAl powder compacts formed at elevated temperature

NASA Astrophysics Data System (ADS)

Rahman, M. M.; Rahman, H. Y.; Awang, M. A. A.; Sopyan, I.

2018-01-01

This paper presents the outcomes of an experimental investigation on the effect of sintering schedule, i.e., holding time and temperature to the final properties of FeCrAl powder compacts prepared through uniaxial die compaction process at above room temperature. The feedstock was prepared by mechanically mixing iron powder ASC 100.29 with chromium (22 wt%) and aluminium (11 wt%) for 30 min at room temperature. A cylindrical shape die was filled with the powder mass and heated for one hour for uniform heating of the die assembly together with the powder mass. Once the temperature reached to the setup temperature, i.e., 150°C, the powder mass was formed by applying an axial pressure of 425 MPa simultaneously from upward and downward directions. The as-pressed green compacts were then cooled to room temperature and subsequently sintered in argon gas fired furnace at a rate of 5°C/min for three different holding times, i.e., 30, 60, and 90 min at three different sintering temperatures, i.e., 800, 900, and 1000°C. The sintered samples were characterized for their density, electrical resistivity, bending strength, and microstructure. The results revealed that the sample sintered at 1000°C for 90 min achieved the better characteristics.

Effect of Alloying Type and Lean Sintering Atmosphere on the Performance of PM Components

NASA Astrophysics Data System (ADS)

Sundaram, M. Vattur; Shvab, R.; Millot, S.; Hryha, E.; Nyborg, L.

2017-12-01

In order to be cost effective and to meet increasing performance demands, powder metallurgy steel components require continuous improvement in terms of materials and process development. This study demonstrates the feasibility of manufacturing structural components using two different alloys systems, i.e. lean Cr-prealloyed and diffusion bonded water atomised powders with different processing conditions. The components were sintered at two different temperatures, i.e. 1120 and 1250 °C for 30 minutes in three different atmospheres: vacuum, N2- 10%H2 atmosphere as well as lean N2-5%H2-0.5%CO-(0.1-0.4)%CH4 sintering atmosphere. Components after sintering were further processed by either low pressure carburizing, sinterhardening or case hardening. All trials were performed in the industrial furnaces to simulate the actual production of the components. Microstructure, fractography, apparent and micro hardness analyses were performed close to the surface and in the middle of the sample to characterize the degree of sintering (temperature and atmosphere) and the effect of heat treatment. In all cases, components possess mostly martensitic microstructure with a few bainitic regions. The fracture surface shows well developed sinter necks. Inter- and trans-granular ductile and cleavage fracture modes are dominant and their fraction is determined by the alloy and processing route.

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

Method of densifying an article formed of reaction bonded silicon nitride

NASA Technical Reports Server (NTRS)

Mangels, John A. (Inventor)

1982-01-01

A method of densifying an article formed of reaction bonded silicon nitride is disclosed. The reaction bonded silicon nitride article is packed in a packing mixture consisting of silicon nitride powder and a densification aid. The reaction bonded silicon nitride article and packing powder are sujected to a positive, low pressure nitrogen gas treatment while being heated to a treatment temperature and for a treatment time to cause any open porosity originally found in the reaction bonded silicon nitride article to be substantially closed. Thereafter, the reaction bonded silicon nitride article and packing powder are subjected to a positive high pressure nitrogen gas treatment while being heated to a treatment temperature and for a treatment time to cause a sintering of the reaction bonded silicon nitride article whereby the strength of the reaction bonded silicon nitride article is increased.

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.

Reduction of Orifice-Induced Pressure Errors

NASA Technical Reports Server (NTRS)

Plentovich, Elizabeth B.; Gloss, Blair B.; Eves, John W.; Stack, John P.

1987-01-01

Use of porous-plug orifice reduces or eliminates errors, induced by orifice itself, in measuring static pressure on airfoil surface in wind-tunnel experiments. Piece of sintered metal press-fitted into static-pressure orifice so it matches surface contour of model. Porous material reduces orifice-induced pressure error associated with conventional orifice of same or smaller diameter. Also reduces or eliminates additional errors in pressure measurement caused by orifice imperfections. Provides more accurate measurements in regions with very thin boundary layers.

High-Pressure-Induced Comminution and Recrystallization of CH3 NH3 PbBr3 Nanocrystals as Large Thin Nanoplates.

PubMed

Yin, Tingting; Fang, Yanan; Chong, Wee Kiang; Ming, Koh Teck; Jiang, Shaojie; Li, Xianglin; Kuo, Jer-Lai; Fang, Jiye; Sum, Tze Chien; White, Timothy J; Yan, Jiaxu; Shen, Ze Xiang

2018-01-01

High pressure (HP) can drive the direct sintering of nanoparticle assemblies for Ag/Au, CdSe/PbS nanocrystals (NCs). Instead of direct sintering for the conventional nanocrystals, this study experimentally observes for the first time high-pressure-induced comminution and recrystallization of organic-inorganic hybrid perovskite nanocrystals into highly luminescent nanoplates with a shorter carrier lifetime. Such novel pressure response is attributed to the unique structural nature of hybrid perovskites under high pressure: during the drastic cubic-orthorhombic structural transformation at ≈2 GPa, (301) the crystal plane fully occupied by organic molecules possesses a higher surface energy, triggering the comminution of nanocrystals into nanoslices along such crystal plane. Beyond bulk perovskites, in which pressure-induced modifications on crystal structures and functional properties will disappear after pressure release, the pressure-formed variants, i.e., large (≈100 nm) and thin (<10 nm) perovskite nanoplates, are retained and these exhibit simultaneous photoluminescence emission enhancing (a 15-fold enhancement in the photoluminescence) and carrier lifetime shortening (from ≈18.3 ± 0.8 to ≈7.6 ± 0.5 ns) after releasing of pressure from 11 GPa. This pressure-induced comminution of hybrid perovskite NCs and a subsequent amorphization-recrystallization treatment offer the possibilities of engineering the advanced hybrid perovskites with specific properties. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Heat Transfer Measurements for a Film Cooled Turbine Vane Cascade

DTIC Science & Technology

2008-05-01

were made of 0.75 in (1.91 cm) thick clear acrylic. The test vanes were made by rapid prototyping technique of a Duraform polyamide sintering material...conditions using the following definition: pVc hSt ρ = (4) We acquired pressure survey measurements under steady state conditions. Total pressure

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.

Aerosol filtration with steel fiber filters

NASA Astrophysics Data System (ADS)

Bergman, W.; Wilson, K.; Larsen, G.; Lopez, R.

1993-04-01

An experimental study has been conducted of aerosol penetration through a new high efficiency steel fiber filter and filter media that was developed in cooperation with Pall Corporation. Previous studies have shown that sintered steel fiber media have significant improvements in higher filter efficiency and lower pressure drop than the previous steel filter technology based on sintered powder metal media. In the present study, measurements were made of the penetration of dioctyl sebacate (DOS) aerosols through flat sheet samples, pleated cartridge filters, and a 1000 cfm filter having 64 cartridges housed in a 2 x 2 x 1 ft. frame. The steel fiber media used in our study consists of 2 micron diameter stainless steel (316 L) fibers sintered together into sheets.

Sintered wire cathode

DOEpatents

Falce, Louis R [San Jose, CA; Ives, R Lawrence [Saratoga, CA

2009-06-09

A porous cathode structure is fabricated from a plurality of wires which are placed in proximity to each other in elevated temperature and pressure for a sintering time. The sintering process produces the porous cathode structure which may be divided into a plurality of individual porous cathodes, one of which may be placed into a dispenser cathode support which includes a cavity for containing a work function reduction material such as BaO, CaO, and Al.sub.2O.sub.3. The work function reduction material migrates through the pores of the porous cathode from a work replenishment surface adjacent to the cavity of the dispenser cathode support to an emitting cathode surface, thereby providing a dispenser cathode which has a uniform work function and therefore a uniform electron emission.

Effect of sintering temperature on flexural properties of alumina fiber-reinforced, alumina-based ceramics prepared by tape casting technique.

PubMed

Tanimoto, Yasuhiro; Nemoto, Kimiya

2006-01-01

The purpose of this study was to investigate the effect of sintering temperature on flexural properties of an alumina fiber-reinforced, alumina-based ceramic (alumina-fiber/alumina composite) prepared by a tape casting technique. The alumina-based ceramic used a matrix consisting of 60 wt% Al(2)O(3) powder and 40 wt% SiO(2)-B(2)O(3) glass powder with the following composition in terms of wt%: 33 SiO(2), 32 B(2)O(3), 20 CaO, and 15 MgO. Prepreg sheets of alumina-fiber/alumina composite in which uniaxial aligned alumina fibers were infiltrated with the alumina-based matrix were fabricated continuously using a tape casting technique employing a doctor blade system. Four sintering temperatures were investigated: 900 degrees C, 1000 degrees C, 1100 degrees C, and 1200 degrees C, all for 4 hours under atmospheric pressure in a furnace. The surface of the alumina-fiber/alumina composite after sintering was observed with a field-emission scanning electron microscope (FE-SEM). A three-point bending test was carried out to measure the flexural strength and modulus of alumina-fiber/alumina composite specimens. In addition, sintered alumina fiber was characterized by X-ray diffraction (XRD). FE-SEM observation showed that alumina-fiber/alumina composite was confirmed to be densely sintered for all sintering temperatures. Three-point bending measurement revealed that alumina-fiber/alumina composite produced at sintering temperatures of 1100 degrees C and 1200 degrees C exhibit flexural strengths lower than those of alumina-fiber/alumina composite produced at sintering temperatures of 900 degrees C and 1000 degrees C; alumina-fiber/alumina composite produced at sintering temperatures of 1100 degrees C and 1200 degrees C exhibit flexural moduli lower than that of alumina-fiber/alumina composite produced at a sintering temperature of 1000 degrees C. Additional XRD pattern of alumina fiber indicated that with increasing sintering temperature, the crystallographic structure of gamma-alumina transformed to mullite. There were significant differences in the flexural properties between the alumina-fiber/alumina composite sintered at the four temperatures. This indicates that the choice of optimum sintering temperature is an important factor for successful dental applications of alumina-fiber/alumina composite developed by the tape casting system.

Sub-second carbon-nanotube-mediated microwave sintering for high-conductivity silver patterns on plastic substrates

NASA Astrophysics Data System (ADS)

Jung, Sunshin; Chun, Su Jin; Han, Joong Tark; Woo, Jong Seok; Shon, Cha-Hwa; Lee, Geon-Woong

2016-02-01

A method of microwave sintering that is mediated by carbon nanotubes (CNTs) has been developed to obtain high-conductivity Ag patterns on the top of heat-sensitive plastic substrates within a short time. The Ag patterns are printed on CNTs formed on plastic substrates and rapidly heated to a great extent by the heat transferred from the microwave-heated CNTs. The conductivity of the microwave-sintered Ag patterns reaches ~39% that of bulk Ag within 1 s without substrate deformation. Furthermore, microwave sintering enhances the adhesion of Ag patterns to the thermoplastic substrates because the sintering causes interfacial fusion between the Ag patterns and the substrates, and CNTs physically connect the patterns with the substrates.A method of microwave sintering that is mediated by carbon nanotubes (CNTs) has been developed to obtain high-conductivity Ag patterns on the top of heat-sensitive plastic substrates within a short time. The Ag patterns are printed on CNTs formed on plastic substrates and rapidly heated to a great extent by the heat transferred from the microwave-heated CNTs. The conductivity of the microwave-sintered Ag patterns reaches ~39% that of bulk Ag within 1 s without substrate deformation. Furthermore, microwave sintering enhances the adhesion of Ag patterns to the thermoplastic substrates because the sintering causes interfacial fusion between the Ag patterns and the substrates, and CNTs physically connect the patterns with the substrates. Electronic supplementary information (ESI) available: Temperature difference in Ag/CNT/PC samples; the carbon content and electrical performance after microwave sintering; microwave sintering of Ag/CNT patterns; physical connection between the substrate and sintered Ag lines; touch-piano (figure and movie). See DOI: 10.1039/c5nr08082g

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.

Silicon nitride sintered body

NASA Technical Reports Server (NTRS)

Suzuki, K.; Shinohara, N.

1984-01-01

The sintering of silicon carbide and it production are described. The method of production is by calcination in which molding is followed by sintering without compression. The invention improves the composition of the silicon carbide ceramic. Six examples of the invention are illustrated and discussed.

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.

Effect of deposition temperature & oxygen pressure on mechanical properties of (0.5) BZT-(0.5)BCT ceramic thin films

NASA Astrophysics Data System (ADS)

Sailaja, P.; Kumar, N. Pavan; Rajalakshmi, R.; Kumar, R. Arockia; Ponpandian, N.; Prabahar, K.; Srinivas, A.

2018-05-01

Lead free ferroelectric thin films of {(0.5) BZT-(0.5) BCT} (termed as BCZT) were deposited on Pt/TiO2/SiO2/Si substrates by pulsed laser deposition at four deposition temperatures 600, 650, 700, 750°C and at two oxygen pressures viz. 75mtorr and 100 mtorr using BCZT ceramic target (prepared by solid state sintering method). The effect of deposition temperature and oxygen pressure on the structure, microstructure and mechanical properties of BCZT films were studied. X-ray diffraction patterns of deposited films confirm tetragonal crystal symmetry and the crystallinity of the films increases with increasing deposition temperature. Variation in BCZT grain growth was observed when the films are deposited at different temperatures andoxygen pressures respectively. The mechanical properties viz. hardness and elastic modulus were also found to be high with increase in the deposition temperature and oxygen pressure. The results will be discussed.

Removable partial denture alloys processed by laser-sintering technique.

PubMed

Alageel, Omar; Abdallah, Mohamed-Nur; Alsheghri, Ammar; Song, Jun; Caron, Eric; Tamimi, Faleh

2018-04-01

Removable partial dentures (RPDs) are traditionally made using a casting technique. New additive manufacturing processes based on laser sintering has been developed for quick fabrication of RPDs metal frameworks at low cost. The objective of this study was to characterize the mechanical, physical, and biocompatibility properties of RPD cobalt-chromium (Co-Cr) alloys produced by two laser-sintering systems and compare them to those prepared using traditional casting methods. The laser-sintered Co-Cr alloys were processed by the selective laser-sintering method (SLS) and the direct metal laser-sintering (DMLS) method using the Phenix system (L-1) and EOS system (L-2), respectively. L-1 and L-2 techniques were 8 and 3.5 times more precise than the casting (CC) technique (p < 0.05). Co-Cr alloys processed by L-1 and L-2 showed higher (p < 0.05) hardness (14-19%), yield strength (10-13%), and fatigue resistance (71-72%) compared to CC alloys. This was probably due to their smaller grain size and higher microstructural homogeneity. All Co-Cr alloys exhibited low porosity (2.1-3.3%); however, pore distribution was more homogenous in L-1 and L-2 alloys when compared to CC alloys. Both laser-sintered and cast alloys were biocompatible. In conclusion, laser-sintered alloys are more precise and present better mechanical and fatigue properties than cast alloys for RPDs. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 1174-1185, 2018. © 2017 Wiley Periodicals, Inc.

Panoscopic approach for high-performance Te-doped skutterudite

DOE PAGES

Liang, Tao; Su, Xianli; Yan, Yonggao; ...

2017-02-24

One-step plasma-activated sintering (OS-PAS) fabrication of single-phase high-performance CoSb 3-based skutterudite thermoelectric material with a hierarchical structure on a time scale of a few minutes is first reported here. The formation mechanism of the CoSb 3 phase and the effects of the current and pressure fields on the phase transformation and microstructure evolution are studied in the one-step PAS process. The application of the panoscopic approach to this system and its effect on the transport properties are investigated. The results show that the hierarchical structure forms during the formation of the skutterudite phase under the effects of both current andmore » sintering pressure. The samples fabricated by the OS-PAS technique have defined hierarchical structures, which scatter phonons more intensely over a broader range of frequencies and significantly reduce the lattice thermal conductivity. High-performance bulk Te-doped skutterudite with the maximum ZT of 1.1 at 820 K for the composition CoSb 2.875Te 0.125 was obtained. Such high ZT values rival those obtained from single filled skutterudites. As a result, this newly developed OS-PAS technique enhances the thermoelectric performance, dramatically shortens the synthesis period and provides a facile method for obtaining hierarchical thermoelectric materials on a large scale.« less

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

[Translucency of dental zirconia ceramics sintered in conventional and microwave ovens].

PubMed

Yuemei, Jiang; Ying, Yang; Wenhui, Zhan; Guoxin, Hu; Qiuxia, Yang

2015-12-01

To evaluate the effect of microwave sintering on the translucency of zirconia and to compare these effect with those of conventional sintering. The relationship between the microstructure of specimens and translucency was investigated. A total of 10 disc-shaped specimens were fabricated from 2 commercial brands of zirconia, namely, Zenostar and Lava. Each group included 5 discs. Conventional sintering was performed according to the manufacturers' specifications. The maximum temperature for Zenostar was 1,490 °C, whereas that for Lava was 1,500 °C. The dwelling time was 2 h. The sintering temperature for microwave sintering was 1,420 °C, heating rate was 15 °C · min⁻¹, and dwelling time was 30 min. After sintering, the translucency parameter (TP) of the specimens were measured with ShadeEye NCC. The sintered density of the specimens was determined by Archimedes' method. The grain size and microstructure of the specimens were investigated by scanning electron microscopy. Density and translucency slightly increased by microwave sintering, but no significant difference was found between microwave and conventional sintering (P > 0.05). Small and uniform microstructure were obtained from microwave sintering. The mean TP of Lava was significantly higher than that of Zenostar (P < 0.001). The translucency of zirconia sintered by microwave sintering is similar to that of the zirconia sintered by conventional sintering.

Microwave sintering of sol-gel derived abrasive grain

DOEpatents

Plovnick, Ross; Celikkaya, Ahmet; Blake, Rodger D.

1997-01-01

A method is provided for making microwave-sintered, free flowing alpha alumina-based ceramic abrasive grain, under conditions effective to couple microwaves with calcined alpha alumina-based abrasive gain precursor and sinter it at a temperature of at least about 1150.degree. C.

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

Comparison of laser and intense pulsed light sintering (IPL) for inkjet-printed copper nanoparticle layers

PubMed Central

Niittynen, Juha; Sowade, Enrico; Kang, Hyunkyoo; Baumann, Reinhard R.; Mäntysalo, Matti

2015-01-01

In this contribution we discuss the sintering of an inkjet-printed copper nanoparticle ink based on electrical performance and microstructure analysis. Laser and intense pulsed light (IPL) sintering are employed in order to compare the different techniques and their feasibility for electronics manufacturing. A conductivity of more than 20% of that of bulk copper material has been obtained with both sintering methods. Laser and IPL sintering techniques are considered to be complementary techniques and are highly suitable in different application fields. PMID:25743631

Numerical Simulation of Sintering Process in Ceramic Powder Injection Moulded Components

NASA Astrophysics Data System (ADS)

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

2007-05-01

A phenomenological model based on viscoplastic constitutive law is presented to describe the sintering process of ceramic components obtained by powder injection moulding. The parameters entering in the model are identified through sintering experiments in dilatometer with the proposed optimization method. The finite element simulations are carried out to predict the density variations and dimensional changes of the components during sintering. A simulation example on the sintering process of hip implant in alumina has been conducted. The simulation results have been compared with the experimental ones. A good agreement is obtained.

Densification behavior, nanocrystallization, and mechanical properties of spark plasma sintered Fe-based bulk amorphous alloys

NASA Astrophysics Data System (ADS)

Singh, Ashish Kumar

Fe-based amorphous alloys are gaining increasing attention due to their exceptional wear and corrosion resistance for potential structural applications. Two major challenges that are hindering the commercialization of these amorphous alloys are difficulty in processing of bulk shapes (diameter > 10 mm) and lack of ductility. Spark plasma sintering (SPS) is evolving as a promising technique for processing bulk shapes of amorphous and nanocrystalline materials. The objective of this work is to investigate densification behavior, nanocrystallization, and mechanical properties of SPS sintered Fe-based amorphous alloys of composition Fe48Cr15Mo14Y2C15B6. SPS processing was performed in three distinct temperature ranges of amorphous alloys: (a) below glass transition temperature (Tg), (b) between Tg and crystallization temperature (Tx), and (c) above Tx. Punch displacement data obtained during SPS sintering was correlated with the SPS processing parameters such as temperature, pressure, and sintering time. Powder rearrangement, plastic deformation below T g, and viscous flow of the material between Tg and Tx were observed as the main densification stages during SPS sintering. Micro-scale temperature distributions at the point of contact and macro-scale temperature distribution throughout the sample during SPS of amorphous alloys were modeled. The bulk amorphous alloys are expected to undergo structural relaxation and nanocrystallization during SPS sintering. X-ray diffraction (XRD), small angle neutron scattering (SANS), and transmission electron microscopy (TEM) was performed to investigate the evolution of nanocrystallites in SPS sintered Fe-based bulk amorphous alloys. The SANS analysis showed significant scattering for the samples sintered in the supercooled region indicating local structural and compositional changes with the profuse nucleation of nano-clusters (~4 nm). Compression tests and microhardness were performed on the samples sintered at different temperatures ranging from 570 °C to 800 °C. Maximum compression strength (1.1+/-0.2 MPa) was obtained for the samples sintered in the supercooled region. Effects of crystallization on tribological behavior of sintered samples were also investigated where crystallization resulted in increase in wear resistance. Laser surface hardening of SPS sintered amorphous samples were performed. Depending on the processing parameters, the laser surface irradiation causes structural relaxation and nanocrystallization, resulting in surface hardening.

Microwave sintering of nanophase ceramics without concomitant grain growth

DOEpatents

Eastman, Jeffrey A.; Sickafus, Kurt E.; Katz, Joel D.

1993-01-01

A method of sintering nanocrystalline material is disclosed wherein the nanocrystalline material is microwaved to heat the material to a temperature less than about 70% of the melting point of the nanocrystalline material expressed in degrees K. This method produces sintered nanocrystalline material having a density greater than about 95% of theoretical and an average grain size not more than about 3 times the average grain size of the nanocrystalline material before sintering. Rutile TiO.sub.2 as well as various other ceramics have been prepared. Grain growth of as little as 1.67 times has resulted with densities of about 90% of theoretical.

Microstructure and Mechanical Properties of Highly Alloyed FeCrMoVC Steel Fabricated by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Oh, Seung-Jin; Jun, Joong-Hwan; Lee, Min-Ha; Shon, In-Jin; Lee, Seok-Jae

2018-05-01

In this study, we successfully fabricated highly alloyed FeCrMoVC specimens within 2 min by using the spark plasma sintering (SPS) method. The densities of the sintered specimens were almost identical to their theoretical values. Fine (Mo, V)-rich carbides with lamellar structure were precipitated along the grain boundaries of the as-sintered specimen, whereas relatively large carbides were formed additionally in the transgranular region during the tempering treatment. Compared with the specimen produced by a conventional casting method, the FeCrMoVC specimens from SPS showed smaller grain size with finer carbides and higher hardness values.

Cathode preparation method for molten carbonate fuel cell

DOEpatents

Smith, James L.; Sim, James W.; Kucera, Eugenia H.

1988-01-01

A method of preparing a porous cathode structure for use in a molten carbonate fuel cell begins by providing a porous integral plaque of sintered nickel oxide particles. The nickel oxide plaque can be obtained by oxidizing a sintered plaque of nickel metal or by compacting and sintering finely divided nickel oxide particles to the desired pore structure. The porous sintered nickel oxide plaque is contacted with a lithium salt for a sufficient time to lithiate the nickel oxide structure and thus enhance its electronic conductivity. The lithiation can be carried out either within an operating fuel cell or prior to assembling the plaque as a cathode within the fuel cell.

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.

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

Work Function and Conductivity of Inkjet-Printed Silver Layers: Effect of Inks and Post-treatments

NASA Astrophysics Data System (ADS)

Mitra, Dana; Mitra, Kalyan Yoti; Dzhagan, Volodymyr; Pillai, Nikhil; Zahn, Dietrich R. T.; Baumann, Reinhard R.

2018-03-01

The electronic properties of a printed layer are influenced by a number of factors, including the nature of the ink (nanoparticle- or solution-based), ink composition (solvents, additives, concentration), and post-treatment technologies, especially sintering. One of the major challenges in the field of printed electronics is achieving the desired performance, for example, in terms of conductivity, resistivity, or work function (WF). This work investigates the dependence of sheet resistance and WF on various sintering methodologies. Four different silver nanoparticle inks were inkjet-printed on a flexible polymeric foil and post-treated by thermal sintering (in an oven) or novel sintering processes using infrared or intense pulsed light. The surfaces of the printed and sintered layers were investigated optically, and various inhomogeneities in the layer surface were observed, varying from a smooth to a highly rough appearance with ring-shaped drying structures. An analysis of the sheet resistance revealed notable variation among the various inks and sintering methodologies used. Here, for the very first time, WF is measured and evaluated as a function of sintering methodology and silver ink, and the respective layer formation characteristics realized with the inkjet printing technology. The WF values obtained by ultraviolet photoemission show a similar spread and allow unambiguous trends to be tracked with respect to the type of ink and sintering method used. The values of the WF obtained range from 3.7 eV to 4.3 eV, approaching the reported bulk values of 4.3-4.7 eV. The various silver inks resulted in different WFs when the same sintering method was used, while the same silver ink resulted in different WFs when various sintering methods were applied. Therefore, it is believed that the WF can be tuned over a broad range in a controlled manner to satisfy electronic device requirements.

Structural, magnetic, elastic, dielectric and electrical properties of hot-press sintered Co1-xZnxFe2O4 (x = 0.0, 0.5) spinel ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Singh Yadav, Raghvendra; Kuřitka, Ivo; Havlica, Jaromir; Hnatko, Miroslav; Alexander, Cigáň; Masilko, Jiri; Kalina, Lukas; Hajdúchová, Miroslava; Rusnak, Jaroslav; Enev, Vojtěch

2018-02-01

In this article, Co1-xZnxFe2O4 (x = 0.0 and 0.5) disc-shaped pellets were formed by hot-press sintering of nanoparticles at temperature 925 °C for 10 min in vacuum atmosphere under 30 MPa mechanical pressure. X-ray diffraction study confirmed the formation of spinel cubic ferrite structure of hot-press sintered spinel ferrite Co1-xZnxFe2O4 (x = 0.0 and 0.5) samples. The scanning electron microscopy image indicated that the growth and densification of smaller ferrite nanoparticles were higher than larger ferrite nanoparticles. Magnetic properties of sintered samples were investigated by the superconducting quantum interface device (SQUID) magnetometer at room temperature. The hot press sintered Co1-xZnxFe2O4 (x = 0.0 and 0.5) pellet samples exhibited magnetic properties dependent on the grain size of spinel ferrite particles. The maximum saturation magnetization 82.47 emu/g was obtained for Co0.5Zn0.5Fe2O4 hot press sintered sample of ball-milled ferrite particles. Further, the impact of grain size and density of sample on hardness, dielectric property and ac conductivity of hot-press sintered samples was investigated. In addition, the longitudinal wave velocity (Vl), transverse wave velocity (Vt), mean elastic wave velocity (Vm), bulk modulus (B), rigidity modulus (G), Young's modulus (E), Poisson ratio (σ) and Debye temperature (θD) were calculated. The elastic moduli of hot press sintered ferrite samples were corrected to zero porosity using Hosselman and Fulrath model.

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.

Processing Techniques Developed to Fabricate Lanthanum Titanate Piezoceramic Material for High-Temperature Smart Structures

NASA Technical Reports Server (NTRS)

Goldsby, Jon C.; Farmer, Serene C.; Sayir, Ali

2004-01-01

Piezoelectric ceramic materials are potential candidates for use as actuators and sensors in intelligent gas turbine engines. For piezoceramics to be applied in gas turbine engines, they will have to be able to function in temperatures ranging from 1000 to 2500 F. However, the maximum use temperature for state-of-the-art piezoceramic materials is on the order of 300 to 400 F. Research activities have been initiated to develop high-temperature piezoceramic materials for gas turbine engine applications. Lanthanum titanate has been shown to have high-temperature piezoelectric properties with Curie temperatures of T(sub c) = 1500 C and use temperatures greater than 1000 C. However, the fabrication of lanthanum titanate poses serious challenges because of the very high sintering temperatures required for densification. Two different techniques have been developed at the NASA Glenn Research Center to fabricate dense lanthanum titanate piezoceramic material. In one approach, lower sintering temperatures were achieved by adding yttrium oxide to commercially available lanthanum titanate powder. Addition of only 0.1 mol% yttrium oxide lowered the sintering temperature by as much as 300 C, to just 1100 C, and dense lanthanum titanate was produced by pressure-assisted sintering. The second approach utilized the same commercially available powders but used an innovative sintering approach called differential sintering, which did not require any additive.

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.

Hydrothermal corrosion of silicon carbide joints without radiation

DOE PAGES

Koyanagi, Takaaki; Katoh, Yutai; Terrani, Kurt A.; ...

2016-09-28

In this paper, hydrothermal corrosion of four types of the silicon carbide (SiC) to SiC plate joints were investigated under pressurized water reactor and boiling water reactor relevant chemical conditions without irradiation. The joints were formed by metal diffusion bonding using molybdenum or titanium interlayer, reaction sintering using Ti—Si—C system, and SiC nanopowder sintering. Most of the joints withstood the corrosion tests for five weeks. The recession of the SiC substrates was limited. Based on the recession of the bonding layers, it was concluded that all the joints except for the molybdenum diffusion bond are promising under the reducing environmentsmore » without radiation. Finally, the SiC nanopowder sintered joint was the most corrosion tolerant under the oxidizing environment among the four joints.« less

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.

High magnetic-refrigeration performance of plate-shaped La{sub 0.5}Pr{sub 0.5}Fe{sub 11.4}Si{sub 1.6} hydrides sintered in high-pressure H{sub 2} atmosphere

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

Sun, N. K., E-mail: naikunsun@163.com; Guo, J.; Zhao, X. G., E-mail: xgzhao@imr.ac.cn

2015-03-02

La(Fe, Si){sub 13} hydride is regarded as one of the most promising room-temperature refrigerants. However, to use the alloys in an active magnetic regenerator machine, it is vital to prepare thin refrigerants. In this work, a high H{sub 2} gas pressure of 50 MPa was employed to suppress the desorption of hydrogen atoms during the sintering process of plate-shaped La{sub 0.5}Pr{sub 0.5}Fe{sub 11.4}Si{sub 1.6} hydrides. At 330 K, a high-density sintered thin plate shows a large magnetic-entropy change ΔS{sub m} of 15.5 J/kg K (106 mJ/cm{sup 3 }K) for a field change of 2 T. The volumetric ΔS{sub m} is almost twice as large as that ofmore » bonded La(Fe,Si){sub 13} hydrides. Favorably, hysteresis is almost absent due to the existence of micropores with a porosity of 0.69% which has been analyzed with high-resolution X-ray microtomography.« less

Effect of grain growth of [beta]-silicon nitride on strength, Weibull modulus, and fracture toughness

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

Hirosaki, Naota; Akimune, Yoshio; Mitomo, Mamoru

1993-07-01

[beta]-Si[sub 3]N[sub 4] powder containing 1 mol% of equimolar Y[sub 2]O[sub 3]-Nd[sub 2]O[sub 3] was gas-pressure sintered at 2,000C for 2 h (SN2), 4 h (SN4), and 8 h (SN8) in 30-MPa nitrogen gas. These materials had a microstructure of in-situ composites'' as a result of exaggerated grain growth of some [beta]-Si[sub 3]N[sub 4] grains during firing. Growth of elongated grains was controlled by the sintering time, so that the desired microstructures were obtained. SN2 had a Weibull modulus as high as 53 because of the uniform size and spatial distribution of its large grains. SN4 had a fracture toughnessmore » of 10.3 MPa[center dot]m[sup 1/2] because of toughening provided by the bridging of elongated grains, whereas SN8 showed a lower fracture toughness, possibly caused by extensive microcracking resulting from excessively large grains. Gas-pressure sintering of [beta]-Si[sub 3]N[sub 4] powder was shown to be effective in fostering selective grain growth for obtaining the desired composite microstructure.« less

Microwave sintering of multiple articles

DOEpatents

Blake, Rodger D.; Katz, Joel D.

1993-01-01

Apparatus and method for producing articles of alumina and of alumina and silicon carbide in which the articles are sintered at high temperatures using microwave radiation. The articles are placed in a sintering container which is placed in a microwave cavity for heating. The rates at which heating and cooling take place is controlled.

Method of sintering ceramic materials

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.

1992-01-01

A method for sintering ceramic materials is described. A ceramic article is coated with layers of protective coatings such as boron nitride, graphite foil, and niobium. The coated ceramic article is embedded in a container containing refractory metal oxide granules and placed within a microwave oven. The ceramic article is heated by microwave energy to a temperature sufficient to sinter the ceramic article to form a densified ceramic article having a density equal to or greater than 90% of theoretical density.

Reflow-oven-processing of pressureless sintered-silver interconnects

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

Wereszczak, Andrew A.; Chen, Branndon R.; Oistad, Brian A.

Here, a method was developed to pressurelessly fabricate strong and consistent sinterable-silver joints or interconnects using reflow oven heating. Circular sinterable-silver interconnects, having nominal diameter of 5 mm and 0.1 mm thickness were stencil printed, contact-dried, and then pressurelessly sinter-bonded to Au-plated direct copper bonded ceramic substrates at 250 °C in ambient air. That sintering was done in either a reflow oven or a convective oven (latter being a conventional heating source for processing sinterable-silver). Consistently strong (>40 MPa) interconnects were produced with reflow oven heating and were as strong as those produced with convective oven heating. This is significantmore » because reflow oven technology affords better potential for continuous mass production and it was shown that strong sintered-silver bonds can indeed be achieved with its use.« less

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.

Lanthanide (Nd, Gd) compounds with garnet and monazite structures. Powders synthesis by "wet" chemistry to sintering ceramics by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Potanina, Ekaterina; Golovkina, Ludmila; Orlova, Albina; Nokhrin, Aleksey; Boldin, Maksim; Sakharov, Nikita

2016-05-01

Complex oxide Y2.5Nd0.5Al5O12 with garnet structure and phosphates NdPO4 and GdPO4 with monazite structure were obtained by using precipitation methods. Ceramics Y2.5Nd0.5Al5O12 and NdPO4 were processed by Spark Plasma Sintering (SPS). Relative density more 98%, sintering time did not exceed 8 min, sintering temperature 1330-1390 °C. Leaching rates of elements from ceramics were 10-6-10-7 g/(cm2 d). The process of ceramics sintering has two-stage character: the first step of sintering-compaction process is related to the plastic flow of the material, the second step-to the process of grain boundary diffusion and grain growth.

Reflow-oven-processing of pressureless sintered-silver interconnects

DOE PAGES

Wereszczak, Andrew A.; Chen, Branndon R.; Oistad, Brian A.

2018-01-04

Here, a method was developed to pressurelessly fabricate strong and consistent sinterable-silver joints or interconnects using reflow oven heating. Circular sinterable-silver interconnects, having nominal diameter of 5 mm and 0.1 mm thickness were stencil printed, contact-dried, and then pressurelessly sinter-bonded to Au-plated direct copper bonded ceramic substrates at 250 °C in ambient air. That sintering was done in either a reflow oven or a convective oven (latter being a conventional heating source for processing sinterable-silver). Consistently strong (>40 MPa) interconnects were produced with reflow oven heating and were as strong as those produced with convective oven heating. This is significantmore » because reflow oven technology affords better potential for continuous mass production and it was shown that strong sintered-silver bonds can indeed be achieved with its use.« less

Method of manufacturing ceramic shaped articles

NASA Technical Reports Server (NTRS)

Inoue, K.

1983-01-01

A method of manufacturing ceramic shaped articles, wherein tapes of ceramic powder material in mixture with a binder material and special additives are shaped and then articles are stamped out from said tapes and sintered in a sintering furnace is described.

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.

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.

A new integrated evaluation method of heavy metals pollution control during melting and sintering of MSWI fly ash.

PubMed

Li, Rundong; Li, Yanlong; Yang, Tianhua; Wang, Lei; Wang, Weiyun

2015-05-30

Evaluations of technologies for heavy metal control mainly examine the residual and leaching rates of a single heavy metal, such that developed evaluation method have no coordination or uniqueness and are therefore unsuitable for hazard control effect evaluation. An overall pollution toxicity index (OPTI) was established in this paper, based on the developed index, an integrated evaluation method of heavy metal pollution control was established. Application of this method in the melting and sintering of fly ash revealed the following results: The integrated control efficiency of the melting process was higher in all instances than that of the sintering process. The lowest integrated control efficiency of melting was 56.2%, and the highest integrated control efficiency of sintering was 46.6%. Using the same technology, higher integrated control efficiency conditions were all achieved with lower temperatures and shorter times. This study demonstrated the unification and consistency of this method. Copyright © 2015 Elsevier B.V. All rights reserved.

Method of sintering ceramic materials

DOEpatents

Holcombe, C.E.; Dykes, N.L.

1992-11-17

A method for sintering ceramic materials is described. A ceramic article is coated with layers of protective coatings such as boron nitride, graphite foil, and niobium. The coated ceramic article is embedded in a container containing refractory metal oxide granules and placed within a microwave oven. The ceramic article is heated by microwave energy to a temperature sufficient to sinter the ceramic article to form a densified ceramic article having a density equal to or greater than 90% of theoretical density. 2 figs.

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.

Densification of oxide superconductors by hot isostatic pressing

NASA Astrophysics Data System (ADS)

Tien, J. K.; Borofka, J. C.; Hendrix, B. C.; Caulfield, T.; Reichman, S. H.

1988-07-01

Currently, consolidation of high Tc superconductor powders is done by sintering, which is not effective in the reduction of porosity. This work assesses the feasibility of hot isostatic pressing (HIP) to obtain fully dense bulk superconductor using HIP modeling and experimental verification. It is concluded that fully dense YBa2Cu3O7 can be obtained in reasonable times at temperatures down to around 650 °C. The trade-offs between temperature, time, and pressure are examined as well as the effects of powder particle size, powder grain size, and trapped gas pressure. The model has. been verified by experiment under three conditions: 100 MPa HIP at 900 °C for 2 hours, 100 MPa HIP at 750 °C for 2 hours, and sintering at 950 °C for 16 hours. The additional advantages of HIPing oxide superconductors are also discussed.

[Study on preparation and physicochemical properties of surface modified sintered bone].

PubMed

Li, Jingfeng; Zheng, Qixin; Guo, Xiaodong

2012-06-01

The aim of this study is to investigate a new method for preparing a biomimetic bone material-surface modified sintered bovine cancellous bone, and to improve its bioactivity as a tissue engineering bone. The prepared sintered bovine cancellous bones with the same size were randomly divided into two groups, immersing in 1 and 1. 5 times simulated body fluid (SBF), respectively. The three time periods of soak time were 7, 14, and 21 days. After sintered bone was dried, the surface morphology of sintered bone and surface mineralization composition were observed under scanning electron microscopy (SEM). By comparing the effect of surface modification of sintered bone materials, we chose the most ideal material and studied its pore size, the rate of the porosity, the compress and bend intensity. And then the material and the sintered bone material without surface modification were compared. The study indicated that sintered bone material immersed in SBF (1.5 times) for 14 days showed the best effect of surface modification, retaining the original physico-chemical properties of sintered bone.

Chemical Sintering Generates Uniform Porous Hyaluronic Acid Hydrogels

PubMed Central

Cam, Cynthia; Segura, Tatiana

2014-01-01

Implantation of scaffolds for tissue repair has been met with limited success primarily due to the inability to achieve vascularization within the construct. Many strategies have shifted to incorporate pores into these scaffolds to encourage rapid cellular infiltration and subsequent vascular ingrowth. We utilized an efficient chemical sintering technique to create a uniform network of polymethyl methacrylate (PMMA) microspheres for porous hyaluronic acid hydrogel formation. The porous hydrogels generated from chemical sintering possessed comparable pore uniformity and interconnectivity as the commonly used non- and heat sintering techniques. Moreover, similar cell response to the porous hydrogels generated from each sintering approach was observed in cell viability, spreading, proliferation in vitro, as well as, cellular invasion in vivo. We propose chemical sintering of PMMA microspheres using a dilute acetone solution as an alternative method to generating porous hyaluronic acid hydrogels since it requires equal or ten-fold less processing time as the currently used non-sintering or heat sintering technique, respectively. PMID:24120847

The Effects of Atmosphere on the Sintering of Ultrafine-Grained Tungsten with Ti

NASA Astrophysics Data System (ADS)

Ren, Chai; Koopman, Mark; Fang, Z. Zak; Zhang, Huan

2016-11-01

Tungsten (W) is a brittle material at room temperature making it very difficult to fabricate. Although the lack of ductility remains a difficult challenge, nano-sized and ultrafine-grained (UFG) structures offer the potential to overcome tungsten's room-temperature brittleness. One way to manufacture UFG W is to compact and sinter nano-sized W powder. It is challenging, however, to control grain growth during sintering. As one method to inhibit grain growth, the effect of Ti-based additives on the densification and grain growth of nano-W powders was investigated in this study. Addition of 1% Ti into tungsten led to more than a 63% decrease in average grain size of sintered samples at comparable density levels. It was found that sintering in Ar yielded a finer grain size than sintering in H2 at similar densities. The active diffusion mechanisms during sintering were different for W-1% Ti nano powders sintered in Ar and H2.

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

Dry-spray deposition of TiO2 for a flexible dye-sensitized solar cell (DSSC) using a nanoparticle deposition system (NPDS).

PubMed

Kim, Min-Saeng; Chun, Doo-Man; Choi, Jung-Oh; Lee, Jong-Cheon; Kim, Yang Hee; Kim, Kwang-Su; Lee, Caroline Sunyong; Ahn, Sung-Hoon

2012-04-01

TiO2 powders were deposited on indium tin oxide (ITO) coated polyethylene terephthalate (PET) substrates for application to the photoelectrode of a dye-sensitized solar cell (DSSC). In the conventional DSSC manufacturing process, a semiconductor oxide such as TiO2 powder requires a sintering process at higher temperature than the glass transition temperature (T(g)) of polymers, and thus utilization of flexible polymer substrates in DSSC research has been constrained. To overcome this restriction related to sintering, we used a nanoparticle deposition system (NPDS) that could produce a thin coating layer through a dry-spray method under atmospheric pressure at room temperature. The powder was sprayed through a slit-type nozzle having a 0.4 x 10 mm2 rectangular outlet. In order to determine the deposited TiO2 thickness, five kinds of TiO2 layered specimens were prepared, where the specimens have single and double layer structures. Deposited powders on the ITO coated PET substrates were observed using FE-SEM and a scan profiler The thicker TiO2 photoelectrode with a DSSC having a double layer structure showed higher energy efficiency than the single layer case. The highest fabricated flexible DSSC displayed a short circuit current density J(sc) = 1.99 mA cm(-2), open circuit voltage V(oc) = 0.71 V, and energy efficiency eta = 0.94%. These results demonstrate the possibility of utilizing the dry-spray method to fabricate a TiO2 layer on flexible polymer substrates at room temperature under atmospheric pressure.

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

NASA Astrophysics Data System (ADS)

Molaro, Jamie; Phillips, Cynthia B.; Meirion-Griffith, Gareth

2017-10-01

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

Effects of sintering temperature on electrical properties of sheep enamel hydroxyapatite

NASA Astrophysics Data System (ADS)

Dumludag, F.; Gunduz, O.; Kılıc, O.; Kılıc, B.; Ekren, N.; Kalkandelen, C.; Oktar, F. N.

2017-12-01

Bioceramics, especially calcium phosphate based bioceramics, whose examples are hydroxyapatite, and calcium phosphate powders have been widely used in the biomedical engineering applications. Hydroxyapatite (HA) is one of the most promising biomaterials, which are derived from natural sources, chemical method, animal like dental enamel and corals. The influence of sintering temperature on the electrical properties (i.e. DC conductivity, AC conductivity) of samples of sintered sheep enamel (SSSE) was studied in air and in vacuum ambient at room temperature. The sheep enamel were sintered at varying temperatures between 1000°C and 1300°C. DC conductivity results revealed that while dc conductivity of the SSSE decreases with increasing the sintering temperature in air ambient the values increased with increasing the sintering temperature in vacuum ambient. AC conductivity measurements were performed in the frequency range of 40 Hz - 105 Hz. The results showed that ac conductivity values decrease with increasing the sintering temperature.

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

Sintering behavior and mechanical properties of zirconia compacts fabricated by uniaxial press forming

PubMed Central

Oh, Gye-Jeong; Yun, Kwi-Dug; Lee, Kwang-Min; Lim, Hyun-Pil

2010-01-01

PURPOSE The purpose of this study was to compare the linear sintering behavior of presintered zirconia blocks of various densities. The mechanical properties of the resulting sintered zirconia blocks were then analyzed. MATERIALS AND METHODS Three experimental groups of dental zirconia blocks, with a different presintering density each, were designed in the present study. Kavo Everest® ZS blanks (Kavo, Biberach, Germany) were used as a control group. The experimental group blocks were fabricated from commercial yttria-stabilized tetragonal zirconia powder (KZ-3YF (SD) Type A, KCM. Corporation, Nagoya, Japan). The biaxial flexural strengths, microhardnesses, and microstructures of the sintered blocks were then investigated. The linear sintering shrinkages of blocks were calculated and compared. RESULTS Despite their different presintered densities, the sintered blocks of the control and experimental groups showed similar mechanical properties. However, the sintered block had different linear sintering shrinkage rate depending on the density of the presintered block. As the density of the presintered block increased, the linear sintering shrinkage decreased. In the experimental blocks, the three sectioned pieces of each block showed the different linear shrinkage depending on the area. The tops of the experimental blocks showed the lowest linear sintering shrinkage, whereas the bottoms of the experimental blocks showed the highest linear sintering shrinkage. CONCLUSION Within the limitations of this study, the density difference of the presintered zirconia block did not affect the mechanical properties of the sintered zirconia block, but affected the linear sintering shrinkage of the zirconia block. PMID:21165274

Effect of Gold on the Microstructural Evolution and Integrity of a Sintered Silver Joint

NASA Astrophysics Data System (ADS)

Muralidharan, Govindarajan; Leonard, Donovan N.; Meyer, Harry M.

2017-07-01

There is a need for next-generation, high-performance power electronic packages and systems employing wide-bandgap devices to operate at high temperatures in automotive and electric grid applications. Sintered silver joints are currently being evaluated as an alternative to Pb-free solder joints. Of particular interest is the development of joints based on silver paste consisting of nano- or micron-scale particles that can be processed without application of external pressure. The microstructural evolution at the interface of a pressureless-sintered silver joint formed between a SiC die with Ti/Ni/Au metallization and an active metal brazed (AMB) substrate with Ag metallization at 250°C has been evaluated using scanning electron microscopy (SEM), x-ray microanalysis, and x-ray photoelectron spectroscopy (XPS). Results from focused ion beam (FIB) cross-sections show that, during sintering, pores in the sintered region near to the Au layer tend to be narrow and elongated with long axis oriented parallel to the interface. Further densification results in formation of many small, relatively equiaxed pores aligned parallel to the interface, creating a path for easy crack propagation. X-ray microanalysis results confirm interdiffusion between Au and Ag and that a region with poor mechanical strength is formed at the edge of this region of interdiffusion.

[Effect of five kinds of pigments on the chromaticity of dental zirconia ceramic].

PubMed

Huang, Hui; Zheng, Yuan-li; Zhang, Fu-qiang; Sun, Jing; Gao, Lian

2007-08-01

All-ceramic dental restorations should match the colour of the natural teeth in order to fulfill aesthetic demands. The goal of this study was to evaluate the colouration of zirconia ceramic by adding five kinds of pigments. The influence of the pigments concentrations on the chromaticity were also analysed. Different concentrations of five kinds of pigments were added on zirconia powder, then compacted at 200MPa using cold isostatic pressure, sintered to 1400 degrees centigrade and hold for two hours. The chromaticity of sintered bodies were measured with chroma meter. The colours achieved by the different pigments were presented in the CIELab system. The a* value increased with the added amount of Er(2)O(3), while b* value raised with the increasing amount of CeO(2) and Pr(6)O(11). However, three pigments failed to decrease L* value and the sintered body looked too bright. The sintered bodies were brown when adding Fe(2)O(3) to zirconia. Adding MnO2 could decrease the L* value of sintered bodies significantly, but had little influence on the a* and b* value. Five kinds of colorized zirconia ceramic could cover with the chromaticity range of dental ceramic which necessitate further investigation.

Coupling of in-situ X-ray Microtomography Observations with Discrete Element Simulations-Application to Powder Sintering

NASA Astrophysics Data System (ADS)

Olmos, L.; Bouvard, D.; Martin, C. L.; Bellet, D.; Di Michiel, M.

2009-06-01

The sintering of both a powder with a wide particle size distribution (0-63 μm) and of a powder with artificially created pores is investigated by coupling in situ X-ray microtomography observations with Discrete Element simulations. The micro structure evolution of the copper particles is observed by microtomography all along a typical sintering cycle at 1050° C at the European Synchrotron Research Facilities (ESRF, Grenoble, France). A quantitative analysis of the 3D images provides original data on interparticle indentation, coordination and particle displacements throughout sintering. In parallel, the sintering of similar powder systems has been simulated with a discrete element code which incorporates appropriate sintering contact laws from the literature. The initial numerical packing is generated directly from the 3D microtomography images or alternatively from a random set of particles with the same size distribution. The comparison between the information drawn from the simulations and the one obtained by tomography leads to the conclusion that the first method is not satisfactory because real particles are not perfectly spherical as the numerical ones. On the opposite the packings built with the second method show sintering behaviors close to the behaviors of real materials, although particle rearrangement is underestimated by DEM simulations.

Advanced Ceramic Technology for Space Applications at NASA MSFC

NASA Technical Reports Server (NTRS)

Alim, Mohammad A.

2003-01-01

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

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

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.

Consolidation Process in Near Net Shape Manufacturing of Armstrong CP-Ti/Ti-6Al-4V Powders

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

Yamamoto, Yukinori; Kiggans, Jim; Clark, Michael B

2010-01-01

This paper summarizes our recent efforts to develop the manufacturing technologies of consolidated net-shape components by using new low-cost commercially pure titanium (CP-Ti) and Ti-6Al-4V alloy powders made by the Armstrong process. Fabrication processes of net shape/ near net shape components, such as uniaxial die-pressing, cold isostatic pressing (CIP), sintering, roll compaction and stamping, have been evaluated. The press-and-sinter processing of the powders were systematically investigated in terms of theoretical density and microstructure as a function of time, pressure, and temperature. Up to 96.4% theoretical density has been achieved with the press-and-sinter technology. Tensile properties of the consolidated samples exhibitmore » good ductility as well as equivalent yield/ultimate tensile strengths to those of fully consolidate materials, even with the presence of a certain amount of porosity. A consolidation model is also under development to interpret the powder deformation during processing. Net shape components made of the Armstrong powder can successfully be fabricated with clearer surface details by using press-and-sinter processing.« less

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.

Effect of ZrO2 on the sintering behavior, strength and high-frequency dielectric properties of electrical ceramic porcelain insulator

NASA Astrophysics Data System (ADS)

Singh Mehta, Niraj; Sahu, Praveen Kumar; Ershad, Md; Saxena, Vipul; Pyare, Ram; Ranjan Majhi, Manas

2018-01-01

In the present study, the effect of ZrO2 on the sintering, strength and dielectric behavior of electrical ceramic porcelain insulator with substituting alumina content by zirconia (in weight percentage from 0% to 30%) is investigated. The different composition of samples containing different zirconia (ZrO2) contents of 0, 10, 20, and 30 wt% are prepared using the uniaxial pressure technique applying 160 MPa pressure. Further, the prepared samples are also analyzed for sintering temperatures (1350 °C), and effects are observed on mechanical and electric properties of porcelain insulator. Different characterizations such as Dilatometer, x-ray diffraction, scanning electron microscopy and differential thermal analysis/thermo gravimetric analysis were used to evaluate the thermal, phase detection, micro structural and weight loss changes by increasing concentration of ZrO2 on base porcelain composition. At 1350 °C, for the composition having 20 wt% ZrO2 with 10 wt% alumina, the maximum density was observed 2.81 g cm-3 with a porosity of 2.23%. The highest tensile strength of 41 ± 3 MPa is observed for the same sample composition. The minimum value of thermal expansion coefficient is found to be in the range of 10-6 for the sample with 30 wt% ZrO2 content sintered at 1350 °C compared to other prepared samples. Similarly, the highest dielectric value (5.1-4.4) having dielectric loss (0.08-0.12) is achieved for the sample with 30 wt% ZrO2 content sintered at 1350 °C in the frequency range of 4-20 GHz at room temperature. According to the mechanical properties, the composition having 20 wt% ZrO2 on base ceramic porcelain composition has enormous potential to serve as a high strength refractory material. For dielectric properties, the composition having 30 wt% ZrO2 is more suitable for the electrical application.

Microstructure and mechanical properties of NiCoCrAlYTa alloy processed by press and sintering route

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

Pereira, J.C., E-mail: jpereira@uc.edu.ve; Centro de Investigaciones en Mecánica, Facultad de Ingeniería, Universidad de Carabobo; Zambrano, J.C.

2015-03-15

Nickel-based superalloys such as NiCoCrAlY are widely used in high-temperature applications, such as gas turbine components in the energy and aerospace industries, due to their strength, high elastic modulus, and high-temperature oxidation resistance. However, the processing of these alloys is complex and costly, and the alloys are currently used as a bond coat in thermal barrier coatings. In this work, the effect of cold press and sintering processing parameters on the microstructure and mechanical properties of NiCoCrAlY alloy were studied using the powder metallurgy route as a new way to obtain NiCoCrAlYTa samples from a gas atomized prealloyed powder feedstock.more » High mechanical strength and adequate densification up to 98% were achieved. The most suitable compaction pressure and sintering temperature were determined for NiCoCrAlYTa alloy through microstructure characterization. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and energy dispersive spectroscopy microanalysis (EDS) were performed to confirm the expected γ-Ni matrix and β-NiAl phase distribution. Additionally, the results demonstrated the unexpected presence of carbides and Ni–Y-rich zones in the microstructure due to the powder metallurgy processing parameters used. Thus, microhardness, nanoindentation and uniaxial compression tests were conducted to correlate the microstructure of the alloy samples with their mechanical properties under the different studied conditions. The results show that the compaction pressure did not significantly affect the mechanical properties of the alloy samples. In this work, the compaction pressures of 400, 700 and 1000 MPa were used. The sintering temperature of 1200 °C for NiCoCrAlYTa alloy was preferred; above this temperature, the improvement in mechanical properties is not significant due to grain coarsening, whereas a lower temperature produces a decrease in mechanical properties due to high porosity and poor solid-state diffusion. - Graphical abstract: Display Omitted - Highlights: • We made NiCoCrAlYTa alloy by a conventional powder metallurgy route. • High densification and adequate strength were observed. • The presence of unexpected carbides found along γ/γ and γ/β grain boundaries was detected. • The effect of cold press and sintering processing parameters on the microstructure and mechanical properties were studied.« less

Effect of grain size on structural and dielectric properties of barium titanate piezoceramics synthesized by high energy ball milling

NASA Astrophysics Data System (ADS)

Verma, Narendra Kumar; Patel, Sandeep Kumar Singh; Kumar, Dinesh; Singh, Chandra Bhal; Singh, Akhilesh Kumar

2018-05-01

We have investigated the effect of sintering temperature on the densification behaviour, grain size, structural and dielectric properties of BaTiO3 ceramics, prepared by high energy ball milling method. The Powder x-ray diffraction reveals the tetragonal structure with space group P4mm for all the samples. The samples were sintered at four different temperatures, (T = 900°C, 1000°C, 1100°C, 1200°C and 1300°C). Density increased with increasing sintering temperature, reaching up to 97% at 1300°C. A grain growth was observed with increasing sintering temperature. Impedance analyses of the sintered samples at various temperatures were performed. Increase in dielectric constant and Curie temperature is observed with increasing sintering temperature.

Method for sintering fuel cell electrodes using a carrier

DOEpatents

Donelson, R.; Bryson, E.S.

1995-03-28

A carrier is described for conveying components of a fuel cell to be sintered through a sintering furnace. The carrier comprises a metal sheet coated with a carbon-based paint, the carbon-based paint comprising an organic binder. The carbon-based paint may be an alcohol or a solvent-based paint or a water-based paint.

Orifice-induced pressure error studies in Langley 7- by 10-foot high-speed tunnel

NASA Technical Reports Server (NTRS)

Plentovich, E. B.; Gloss, B. B.

1986-01-01

For some time it has been known that the presence of a static pressure measuring hole will disturb the local flow field in such a way that the sensed static pressure will be in error. The results of previous studies aimed at studying the error induced by the pressure orifice were for relatively low Reynolds number flows. Because of the advent of high Reynolds number transonic wind tunnels, a study was undertaken to assess the magnitude of this error at high Reynolds numbers than previously published and to study a possible method of eliminating this pressure error. This study was conducted in the Langley 7- by 10-Foot High-Speed Tunnel on a flat plate. The model was tested at Mach numbers from 0.40 to 0.72 and at Reynolds numbers from 7.7 x 1,000,000 to 11 x 1,000,000 per meter (2.3 x 1,000,000 to 3.4 x 1,000,000 per foot), respectively. The results indicated that as orifice size increased, the pressure error also increased but that a porous metal (sintered metal) plug inserted in an orifice could greatly reduce the pressure error induced by the orifice.

Spark plasma sintering of highly dense fine-grained mineral aggregates

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Process Simulation of Cold Pressing and Sintering of Armstrong CP-Ti Powders

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

Gorti, Sarma B; Sabau, Adrian S; Peter, William H

A computational methodology is presented for the process simulation of cold pressing and sintering of Armstrong CP-Ti powders. Since the powder consolidation is governed by specific pressure-dependent constitutive equations, solution algorithms were developed for the ABAQUS user material subroutine, UMAT, for computing the plastic strain increments based on an implicit integration of the nonlinear yield function, flow rule, and hardening equations. Sintering was simulated using a model based on diffusional creep using the user subroutine CREEP. The initial mesh, stress, and density for the simulation of sintering were obtained from the results of the cold pressing simulation, minimizing the errorsmore » from decoupling the cold pressing and sintering simulations. Numerical simulation results are presented for the cold compaction followed by a sintering step of the Ti powders. The numerical simulation results for the relative density were compared to those measured from experiments before and after sintering, showing that the relative density can be accurately predicted. Notice: This manuscript has been authored by UT-Battelle, LLC, under Contract No. DE-AC05-00OR22725 with the U.S. Department of Energy. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce the published form of this manuscript, or allow others to do so, for United States Government purposes. ACKNOWLEDGEMENTS This research was sponsored by the U.S. DOE, and carried out at ORNL, under Contract DE-AC05-00OR22725 with UT-Battelle, LLC. This research was sponsored by the U.S. DOE, EERE Industrial Technology Program Office under CPS Agreement # 17881.« less

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

PubMed

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

2018-04-11

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

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

Surface hardening of Al alloys through controlled ball-milling and sintering.

PubMed

Kim, Seek Hyeoun; Kim, Yong Jin; Ahn, Jung-Ho

2012-07-01

One of the drawbacks of aluminum and its alloys is the lack of proper heat-treatment for surface-hardening. In the present work, a new and simple method of hardening the surface of aluminum and its alloys was developed. Low-energy ball-milling using specific process control agents (PCAs) was employed, using subsequent sintering in a controlled atmosphere. The PCAs in the present work were very effective both for milling and the formation of hard nanocrystalline dispersoids during sintering. The residual oxygen in a sintering atmosphere also played an important role in the formation of AIN or Al-O-N dispersoids. Through the proper control of the processing atmosphere and PCAs, the hardness and thickness of the hardened layers could be adjusted. The results of the wear test showed that the present aluminum alloys can be effectively utilized as light-weight components with a good wear resistance. Furthermore, the present method involves a simple forming process of die-compaction and sintering.

Production technology of an electrolyte for Na/S batteries

NASA Astrophysics Data System (ADS)

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

1982-05-01

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

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.

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.

Ultra high purity, dimensionally stable INVAR 36

NASA Technical Reports Server (NTRS)

Sokolowski, Witold M. (Inventor); Lane, Marc S. (Inventor); Odonnell, Timothy P. (Inventor); Hsieh, Cheng H. (Inventor)

1994-01-01

An INVAR 36 material having long-term dimensional stability is produced by sintering a blend of powders of nickel and iron under pressure in an inert atmosphere to form an alloy containing less than 0.01 parts of carbon and less than 0.1 part aggregate and preferably 0.01 part individually of Mn, Si, P, S and Al impurities. The sintered alloy is heat treated and slowly and uniformly cooled to form a material having a coefficient of thermal expansion of less than 1 ppm/C and a temporal stability of less than 1 ppm/year.

Ultra high purity, dimensionally stable INVAR 36

NASA Technical Reports Server (NTRS)

Sokolowski, Witold M. (Inventor); Lane, Marc S. (Inventor); Hsieh, Cheng H. (Inventor); Odonnell, Timothy P. (Inventor)

1995-01-01

An INVAR 36 material having long-term dimensional stability is produced by sintering a blend of powders of nickel and iron under pressure in an inert atmosphere to form an alloy containing less than 0.01 parts of carbon and less than 0.1 part aggregate and preferably 0.01 part individually of Mn, Si, P, S and Al impurities. The sintered alloy is heat treated and slowly and uniformly cooled to form a material having a coefficient of thermal expansion of less than 1 ppm/C and a temporal stability of less than 1 ppm/year.

HSPES membrane electrode assembly

NASA Technical Reports Server (NTRS)

Kindler, Andrew (Inventor); Yen, Shiao-Ping (Inventor)

2000-01-01

An improved fuel cell electrode, as well as fuel cells and membrane electrode assemblies that include such an electrode, in which the electrode includes a backing layer having a sintered layer thereon, and a non-sintered free-catalyst layer. The invention also features a method of forming the electrode by sintering a backing material with a catalyst material and then applying a free-catalyst layer.

Microstructure and Mechanical Behavior of Amorphous Al-Cu-Ti Metal Foams Synthesized by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Li, Maoyuan; Lu, Lin; Dai, Zhen; Hong, Yiqiang; Chen, Weiwei; Zhang, Yuping; Qiao, Yingjie

Amorphous Al-Cu-Ti metal foams were prepared by spark plasma sintering (SPS) process with the diameter of 10mm. The SPS process was conducted at the pressure of 200 and 300MPa with the temperature of 653-723K, respectively. NaCl was used as the space-holder, forming almost separated pores with the porosity of 65 vol%. The microstructure and mechanical behavior of the amorphous Al-Cu-Ti metal foams were systematically investigated. The results show that the crystallinity increased at elevated temperatures. The effect of pressure and holding time on the crystallization was almost negligible. The intermetallic compounds, i.e. Al-Ti, Al-Cu and Al-Cu-Ti were identified from X-ray diffraction (XRD) patterns. It was found that weak adhesion and brittle intermetallic compounds reduced the mechanical properties, while lower volume fraction and smaller size of NaCl powders improved the mechanical properties.

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.

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.

Method for fabricating prescribed flaws in the interior of metals

DOEpatents

Hsu, David K.; Thompson, Donald O.

1989-03-07

The method for fabricating a metal body having a flaw of predetermined size and shape located therein comprises placing half of the metal powder required to make the metal body in the die of a press and pressing it to create a flat upper surface thereon. A piece of copper foil is cut to the size and shape of the desired interior crack and placed on the upper surface of the powder and centered in position. The remaining powder is then placed in the die to cover the copper foil. The powder is first cold pressed and removed from the press. The powder metal piece is then sintered in a furnace at a temperature above the melting point of the copper and below the melting point of the metal. It is then removed from the furnace, cooled to room temperature, and placed back in the die and pressed further. This procedure results in an interior flaw or crack. Modified forms of the method involve using a press-sinter-press-sinter cycle with the first sinter being below the melting point of the copper and the second sinter being above the melting point of the copper and below the melting point of the metal.

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

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

The Effect of Sintering Temperature on Linear and Nonlinear Optical Properties of YAG Nanoceramics

NASA Astrophysics Data System (ADS)

Gayvoronsky, V. Ya.; Popov, A. S.; Brodyn, M. S.; Uklein, A. V.; Multian, V. V.; Shul'zhenko, O. O.

Recent improvements in powder synthesis and ceramics sintering made it possible to fabricate high-quality optical materials. The work is devoted to the structural and optical characterization of the ({Y_3}{Al_5}{O_{12}}, YAG) ceramics prepared by high-pressure low-temperature technique. The structural properties of the studied ceramic samples was obtained by X-ray diffraction. The studies of the total and in-line transmittance as well as optical scattering indicatrices were performed in visible and NIR ranges. The scatterer size ˜200 nm was estimated by Rayleigh-Gans-Debye model. It was shown that the studied samples demonstrate high transparency at 1064 nm. The nonlinear optical characterization of the samples was done by the self-action of the picosecond laser pulses at 1064 nm. The measured nonlinear optical response (χ^(3)) ˜ 10^{-11} esu) showed significant dependence on the sintering temperature variation.

Rhenium material properties

NASA Technical Reports Server (NTRS)

Biaglow, James A.

1995-01-01

Tensile data were obtained from four different types of rhenium at ambient and elevated temperatures. The four types of rhenium included chemical vapor deposition (CVD) and three powder metallurgy (PM) types, i.e., rolled sheet and pressed and sintered bars, with and without hot isostatic pressure (HIP) treatment. Results revealed a wide range of values with ultimate strengths at ambient temperatures varying from 663 MPa for CVD rhenium to 943 MPa for rolled sheet. A similar spread was also obtained for material tested at 1088 K and 1644 K. The wide variance observed with the different materials indicated that the rhenium manufacturing process, material composition and prior handling strongly dictated its properties. In addition to tensile properties, CVD, pressed and sintered material and HIP rhenium successfully completed 100 cycles of low cycle fatigue. Creep data were also obtained showing that CVD and pressed and sintered rhenium could sustain five hours of testing under a tension of 27.5 MPa at 1922 K.

The impact of the proportion of nanoparticles to the spherical microparticles of silver on the connection parameters LTJT

NASA Astrophysics Data System (ADS)

Szałapak, J.; Kiełbasiński, K.; Krzemiński, J.; Jakubowska, M.

2017-08-01

There are few EU directives restricting use of lead and other hazardous substances in electronics. That leads to ban Pb- Sn alloy from use, the consequence of which is a search for new ways of preparing joints. One of the discussed solutions is using silver particles in Low Temperature Joining Technique (LTJT). This technique allows to use different conducting pastes and lower their sintering temperatures with the use of pressure. The most popular material for the joining tests was silver. Due to its high melting temperature and high pressures needed for lowering the temperature, silver nanoparticles were considered and tested. The temperatures of sintering decreased to 300ºC and the pressures went down from about 40 to less than 10 MPa. Due to unsatisfactory parameters of such joints, the authors prepared mixtures of spherical, submicron-sized silver particles with nanoparticles. Joints were tested for their electrical and shears strength parameters. In this article, the authors show the comparison of different variations of the mixtures with joints prepared only with nanoparticles.

Transport properties of undoped and Br-doped PbTe sintered at high temperature and pressure> 4.0 GPa

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

Yongkwan, Dong; McGuire, Michael A; Malik, Abds-Sami

2009-01-01

The thermoelectric properties of nominally undoped PbTe and Br doped PbTe materials sintered at high-pressure and high-temperature (HPHT) have been studied. All samples show n-type semiconducting behavior with negative thermopower. For undoped PbTe, four different HPHT treatments were performed at pressures between 4.0 and 6.5 GPa. PbTe doped with Br at 0.5, 1.0, 2.0, 3.0 x 10{sup 19} cm{sup -3} was HPHT treated at 4.0 GPa and 1045 C. As the dopant concentration increases, the absolute thermopower decreases, thermal conductivity increases, and electrical resistivity decreases. At a nominal dopant concentration of 1.0 x 10{sup 19} cm{sup -3}, carrier mobility ofmore » 1165 cm{sup 2}/V s and dimensionless thermoelectric figure-of-merit, ZT, of around 0.27 at 300 K were obtained. These results demonstrate that HPHT post-processing is a viable and controllable way of tuning the thermoelectric properties of PbTe-based materials.« less

Effect on the grain size of single-mode microwave sintered NiCuZn ferrite and zinc titanate dielectric resonator ceramics.

PubMed

Sirugudu, Roopas Kiran; Vemuri, Rama Krishna Murthy; Venkatachalam, Subramanian; Gopalakrishnan, Anisha; Budaraju, Srinivasa Murty

2011-01-01

Microwave sintering of materials significantly depends on dielectric, magnetic and conductive Losses. Samples with high dielectric and magnetic loss such as ferrites could be sintered easily. But low dielectric loss material such as dielectric resonators (paraelectrics) finds difficulty in generation of heat during microwave interaction. Microwave sintering of materials of these two classes helps in understanding the variation in dielectric and magnetic characteristics with respect to the change in grain size. High-energy ball milled Ni0.6Cu0.2Zn0.2Fe1.98O4-delta and ZnTiO3 are sintered in conventional and microwave methods and characterized for respective dielectric and magnetic characteristics. The grain size variation with higher copper content is also observed with conventional and microwave sintering. The grain size in microwave sintered Ni0.6Cu0.2Zn0.2Fe1.98O4-delta is found to be much small and uniform in comparison with conventional sintered sample. However, the grain size of microwave sintered sample is almost equal to that of conventional sintered sample of Ni0.3Cu0.5Zn0.2Fe1.98O4-delta. In contrast to these high dielectric and magnetic loss ferrites, the paraelectric materials are observed to sinter in presence of microwaves. Although microwave sintered zinc titanate sample showed finer and uniform grains with respect to conventional samples, the dielectric characteristics of microwave sintered sample are found to be less than that of conventional sample. Low dielectric constant is attributed to the low density. Smaller grain size is found to be responsible for low quality factor and the presence of small percentage of TiO2 is observed to achieve the temperature stable resonant frequency.

Structural and mechanical characterization of boron doped biphasic calcium phosphate produced by wet chemical method and subsequent thermal treatment

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

Albayrak, Onder, E-mail: albayrakonder@mersin.edu.tr

In the current study, boron doped biphasic calcium phosphate bioceramics consisting of a mixture of boron doped hydroxyapatite (BHA) and beta tricalcium phosphate (β-TCP) of varying BHA/β-TCP ratios were obtained after sintering stage. The effects of varying boron contents and different sintering temperatures on the BHA/β-TCP ratios and on the sinterability of the final products were investigated. Particle sizes and morphologies of the obtained precipitates were determined using SEM. XRD and FTIR investigation were conducted to detect the boron formation in the structure of HA and quantitative analysis was performed to determine the BHA/β-TCP ratio before and after sintering stage.more » In order to determine the sinterability of the obtained powders, pellets were prepared and sintered; the rates of densification were calculated and obtained results were correlated by SEM images. Also Vickers microhardness values of the sintered samples were determined. The experimental results verified that boron doped hydroxyapatite powders were obtained after sintering stage and the structure consists of a mixture of BHA and β-TCP. As the boron content used in the precipitation stage increases, β-TCP content of the BHA/β-TCP ratio increases but sinterability, density and microhardness deteriorate. As the sintering temperature increases, β-TCP content, density and microhardness of the samples increase and sinterability improves. - Highlights: • This is the first paper about boron doped biphasic calcium phosphate bioceramics. • Boron doping affects the structural and mechanical properties. • BHA/β-TCP ratio can be adjustable with boron content and sintering temperature.« less

Applying Massively Parallel Kinetic Monte Carlo Methods to Simulate Grain Growth and Sintering in Powdered Metals

DTIC Science & Technology

2011-09-01

Structure Evolution During Sintering From [19]. ...................................20 Figure 10. Ising Model Configuration With Eight Nearest Neighbors...INTRODUCTION A. MOTIVATION The ability to fabricate structural components from metals with a fine (micron- sized), controlled grain size is one of the...hallmarks of modern, structural metallurgy. Powder metallurgy, in particular, consists of powder manufacture, powder blending, compacting, and sintering

THE EFFECT OF TEMPERATURE AND UNIAXIAL PRESSURE ON THE DENSIFICATION BEHAVIOR OF SILICA AEROGEL GRANULES

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

Matyas, Josef; Robinson, Matthew J.; Fryxell, Glen E.

Materials are being developed in U.S. for the removal and immobilization of iodine from gaseous products of nuclear fuel reprocessing in support of the Fuel Cycle Technology Separations and Waste Forms Campaign. The silver-functionalized silica aerogel proved to be an excellent candidate for this treatment because of its high selectivity and sorption capacity for radioiodine and its possible conversion to a durable silica-based waste form. The present study investigated with nitrogen sorption and helium pycnometry the effect of pressureless isothermal sintering at temperatures of 900-1400°C for 2.5-90 min or isothermal hot-pressing at 1200°C for 2.5 min on densification of rawmore » and silver-functionalized silica aerogel granules. Rapid sintering was observed at 1050 and 1200°C. Only 15 min of pressureless sintering at 1200°C resulted in almost complete densification. The macropores disappeared, surface area decreased from 1114 m2/g to 25 m2/g, pore volume from 7.41 cm3/g to 0.09 cm3/g, and adsorption pore size from 18.7 to 7 nm. The skeletal density of sintered granules was similar to the bulk density of amorphous silica (2.2 g/cm3). The hot-pressing accelerated the sintering process, decreasing significantly the pore size and volume.« less

Self Sealing Magmas

NASA Astrophysics Data System (ADS)

von Aulock, Felix W.; Wadsworth, Fabian B.; Kennedy, Ben M.; Lavallee, Yan

2015-04-01

During ascent of magma, pressure decreases and bubbles form. If the volume increases more rapidly than the relaxation timescale, the magma fragments catastrophically. If a permeable network forms, the magma degasses non-violently. This process is generally assumed to be unidirectional, however, recent studies have shown how shear and compaction can drive self sealing. Here, we additionally constrain skin formation during degassing and sintering. We heated natural samples of obsidian in a dry atmosphere and monitored foaming and impermeable skin formation. We suggest a model for skin formation that is controlled by diffusional loss of water and bubble collapse at free surfaces. We heated synthetic glass beads in a hydrous atmosphere to measure the timescale of viscous sintering. The beads sinter at drastically shorter timescales as water vapour rehydrates an otherwise degassed melt, reducing viscosity and glass transition temperatures. Both processes can produce dense inhomogeneities within the timescales of magma ascent and effectively disturb permeabilities and form barriers, particularly at the margins of the conduit, where strain localisation takes place. Localised ash in failure zones (i.e. Tuffisite) then becomes associated with water vapour fluxes and alow rapid rehydration and sintering. When measuring permeabilities in laboratory and field, and when discussing shallow degassing in volcanoes, local barriers for degassing should be taken into account. Highlighting the processes that lead to the formation of such dense skins and sintered infills of cavities can help understanding the bulk permeabilities of volcanic systems.

Characteristics of B2O3 and Fe added into BaFe12O19 permanent magnets prepared at different milling time and sintering temperature

NASA Astrophysics Data System (ADS)

Sebayang, Perdamean; Sari, Ayu Yuswita; Ginting, Delovita; Allan, Yola; Nasruddin M., N.; Sebayang, Kerista

2016-02-01

The objective of present work is to investigate the characteristic of BaFe12O19, B2O3-BaFe12O19 and Fe-BaFe12O19 magnets fabricated at different milling time and sintering temperature. The characteristic of perrmanen magnet BaFe12O19 with different content of B2O3 and Fe which was fabricated at different milling time and sintering temperature were investigated. The powder mixtures were prepared by dry and wet milling at various milling time. The powder were mixtured and prepared by dry and wet milling at various milling time. The mixture powder was then compacted by anisotropic with compressive pressure of 50 N/cm2. The green bodies were sinter at 1050, 1100, 1150 and 1200°C and hold for 1 h, separately. The density, magnetic flux density and B-H curve were measured by Archimedes principle, Gauss meter and Permagraph, respectively. The microstructure and phase composition characterization were performed by SEM and XRD. The results of this study are presented in this paper. It shows that addition of Fe (in wet milling) and B2O3 (in dry milling) respectively give a potential benefit to reduce the sintering temperature and improve the magnetic flux density of barium hexaferrite.

Effect of Gold on the Microstructural Evolution and Integrity of a Sintered Silver Joint

DOE PAGES

Muralidharan, Govindarajan; Leonard, Donovan N.; Meyer, Harry M.

2017-01-05

There is a need for next-generation, high-performance power electronic packages and systems employing wide band gap devices to operate at high temperatures in automotive and electric grid applications. Sintered silver joints are currently being evaluated as an alternative to Pb-free solder joints. Of particular interest is the development of joints based on silver paste consisting of nanoscale or micron scale particles that can be processed without the application of an external pressure. Microstructural evolution at the interface of a pressureless sintered silver joint formed between a SiC die with a Ti/Ni/Au metallization and an Active Metal Brazed substrate with Agmore » metallization at 250 °C was evaluated using Scanning Electron Microscopy, X-ray microanalysis, and X-ray Photo Electron Spectroscopy. Results from Focused Ion Beam cross-sections show that during sintering, the pores in the sintered region close to the Au layer tend to be smaller and are oriented predominantly with their longer dimension oriented parallel to the interface. With further densification, this results in the alignment of small pores parallel to the interface, creating a path for easy crack propagation. Lastly, X-ray microchemical analyses results confirm interdiffusion between Au and Ag and that a region with poor mechanical strength is formed at the edge of this region of interdiffusion.« less

DEVELOPMENT OF AG-1 SECTION FI ON METAL MEDIA FILTERS - 9061

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

Adamson, D; Charles A. Waggoner, C

Development of a metal media standard (FI) for ASME AG-1 (Code on Nuclear Air and Gas Treatment) has been under way for almost ten years. This paper will provide a brief history of the development process of this section and a detailed overview of its current content/status. There have been at least two points when dramatic changes have been made in the scope of the document due to feedback from the full Committee on Nuclear Air and Gas Treatment (CONAGT). Development of the proposed section has required resolving several difficult issues associated with scope; namely, filtering efficiency, operating conditions (mediamore » velocity, pressure drop, etc.), qualification testing, and quality control/acceptance testing. A proposed version of Section FI is currently undergoing final revisions prior to being submitted for balloting. The section covers metal media filters of filtering efficiencies ranging from medium (less than 99.97%) to high (99.97% and greater). Two different types of high efficiency filters are addressed; those units intended to be a direct replacement of Section FC fibrous glass HEPA filters and those that will be placed into newly designed systems capable of supporting greater static pressures and differential pressures across the filter elements. Direct replacements of FC HEPA filters in existing systems will be required to meet equivalent qualification and testing requirements to those contained in Section FC. A series of qualification and quality assurance test methods have been identified for the range of filtering efficiencies covered by this proposed standard. Performance characteristics of sintered metal powder vs. sintered metal fiber media are dramatically different with respect to parameters like differential pressures and rigidity of the media. Wide latitude will be allowed for owner specification of performance criteria for filtration units that will be placed into newly designed systems. Such allowances will permit use of the most appropriate metal media for a system as specified by the owner with respect to material of manufacture, media velocity, system maximum static pressure, maximum differential pressure across the filter, and similar parameters.« less

Triphasic Composite And Method Of Making Same

DOEpatents

Kear, Bernard H.; Sadangi, Rajendra K.; McCandlish, Larry E.; Voronov, Oleg

2000-07-18

A method for fabricating a triphasic composite such as a WC/Co/diamond composite with a high volume fraction of diamond in a WC/Co matrix. The method involves sintering of a WC/Co powder compact to develop a porous preform, which displays some rigidity and strength, infiltrating the porous preform with a controlled distribution of carbon, and high pressure/high temperature treatment of the carbon-containing WC/Co preform to transform the carbon to diamond. The distribution of diamond in the composite can be functionally graded to provide a WC/Co core and a diamond-enriched surface, wherein all three phases form an interconnected structure in three dimensions. Such a tricontinuous structure combines high strength and toughness with superior wear resistance, making it attractive for applications in machine tools and drill bits.

Methods of forming aluminum oxynitride-comprising bodies, including methods of forming a sheet of transparent armor

DOEpatents

Chu, Henry Shiu-Hung [Idaho Falls, ID; Lillo, Thomas Martin [Idaho Falls, ID

2008-12-02

The invention includes methods of forming an aluminum oxynitride-comprising body. For example, a mixture is formed which comprises A:B:C in a respective molar ratio in the range of 9:3.6-6.2:0.1-1.1, where "A" is Al.sub.2O.sub.3, "B" is AlN, and "C" is a total of one or more of B.sub.2O.sub.3, SiO.sub.2, Si--Al--O--N, and TiO.sub.2. The mixture is sintered at a temperature of at least 1,600.degree. C. at a pressure of no greater than 500 psia effective to form an aluminum oxynitride-comprising body which is at least internally transparent and has at least 99% maximum theoretical density.

Low Cost Synthesis Method of Two-Dimensional Titanium Carbide MXene

NASA Astrophysics Data System (ADS)

Rasid, Z. A. M.; Omar, M. F.; Nazeri, M. F. M.; A'ziz, M. A. A.; Szota, M.

2017-06-01

A layered MAX phase of Ti3AlC2 was synthesized through pressureless sintering (PLS) the initial powder of TiH2/Al/C without preliminary dehydrogenation under argon atmosphere at 1350°C. An elegant exfoliations approach was used to prepare a two-dimensional (2D) metal carbide Ti3C2 from layered MAX phase by removing A layer by chemical etching. The use of PLS method instead of any pressure assistance method such as hot isostatic press (HIP) and hot press (HP) lowered the cost of synthesis. Recently, some unique potential of Ti3C2 has been discovered leads to the proposal of potential application, mostly on electronic devices. Morphology and structural analysis was used to confirm the successful of this research.

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

Low temperature sintered giant dielectric permittivity CaCu3Ti4O12 sol-gel synthesized nanoparticle capacitors

NASA Astrophysics Data System (ADS)

Puli, Venkata Sreenivas; Adireddy, Shiva; Kothakonda, Manish; Elupula, Ravinder; Chrisey, Douglas B.

This paper reports on synthesis of polycrystalline complex perovskite CaCu3Ti4O12 (as CCTO) ceramic powders prepared by a sol-gel auto combustion method at different sintering temperatures and sintering times, respectively. The effect of sintering time on the structure, morphology, dielectric and electrical properties of CCTO ceramics is investigated. Tuning the electrical properties via different sintering times is demonstrated for ceramic samples. X-ray diffraction (XRD) studies confirm perovskite-like structure at room temperature. Abnormal grain growth is observed for ceramic samples. Giant dielectric permittivity was realized for CCTO ceramics. High dielectric permittivity was attributed to the internal barrier layer capacitance (IBLC) model associated with the Maxwell-Wagner (MW) polarization mechanism.

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.

Study on selective laser sintering of glass fiber reinforced polystyrene

NASA Astrophysics Data System (ADS)

Yang, Laixia; Wang, Bo; Zhou, Wenming

2017-12-01

In order to improve the bending strength of Polystyrene (PS) sintered parts by selective laser sintering, Polystyrene/glass fiber (PS/GF) composite powders were prepared by mechanical mixing method. The size distribution of PS/GF composite powders was characterized by laser particle size analyzer. The optimum ratio of GF was determined by proportioning sintering experiments. The influence of process parameters on the bending strength of PS and PS/GF sintered parts was studied by orthogonal test. The result indicates that the particle size of PS/GF composite powder is mainly distributed in 24.88 μm~139.8 μm. When the content of GF is 10%, it has better strengthen effect. Finally, the article used the optimum parameter of the two materials to sinter prototype, it is found that the PS/GF prototype has the advantages of good accuracy and high strength.

Mechanical and microstructural characterization of W–Cu FGM fabricated by one-step sintering method through PM route

NASA Astrophysics Data System (ADS)

Gupta, Rajat; Kumar, Rohit; Chaubey, A. K.; Kanpara, Shailesh; Khirwadkar, S. S.

2018-03-01

Five layer W-Cu functionally graded material (FGM) for components in nuclear fusion application was fabricated by a one-step resistance sintering process, known as spark plasma sintering (SPS). In this study effect of sintering temperature (Ts) on physical, mechanical and surface property was investigated. Detailed microstructural study revealed that the graded structure of the composite layers with varying composition from 0 to 100 wt% W and Cu in opposite directions could be well densified after the SPS process. It also indicates that the fine microstructure within functionally graded layers can be maintained because of short sintering time. The sample sintered at 1050°C shows more than 90% theoretical density, hardness greater than 239±5 Hv and excellent surface scratch resistance. The result demonstrates that SPS is promising and more suitable process for fabrication of W-Cu FGM.

Sintered silver joints via controlled topography of electronic packaging subcomponents

DOEpatents

Wereszczak, Andrew A.

2014-09-02

Disclosed are sintered silver bonded electronic package subcomponents and methods for making the same. Embodiments of the sintered silver bonded EPSs include topography modification of one or more metal surfaces of semiconductor devices bonded together by the sintered silver joint. The sintered silver bonded EPSs include a first semiconductor device having a first metal surface, the first metal surface having a modified topography that has been chemically etched, grit blasted, uniaxial ground and/or grid sliced connected to a second semiconductor device which may also include a first metal surface with a modified topography, a silver plating layer on the first metal surface of the first semiconductor device and a silver plating layer on the first metal surface of the second semiconductor device and a sintered silver joint between the silver plating layers of the first and second semiconductor devices which bonds the first semiconductor device to the second semiconductor device.

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.

Evaluation of Microstructure and Mechanical Properties of Al-TiC Metal Matrix Composite Prepared by Conventional, Microwave and Spark Plasma Sintering Methods

PubMed Central

Ghasali, Ehsan; Fazili, Ali; Alizadeh, Masoud; Shirvanimoghaddam, Kamyar; Ebadzadeh, Touradj

2017-01-01

In this research, the mechanical properties and microstructure of Al-15 wt % TiC composite samples prepared by spark plasma, microwave, and conventional sintering were investigated. The sintering process was performed by the speak plasma sintering (SPS) technique, microwave and conventional furnaces at 400 °C, 600 °C, and 700 °C, respectively. The results showed that sintered samples by SPS have the highest relative density (99% of theoretical density), bending strength (291 ± 12 MPa), and hardness (253 ± 23 HV). The X-ray diffraction (XRD) investigations showed the formation of TiO2 from the surface layer decomposition of TiC particles. Scanning electron microscopy (SEM) micrographs demonstrated uniform distribution of reinforcement particles in all sintered samples. The SEM/EDS analysis revealed the formation of TiO2 around the porous TiC particles. PMID:29088114

Cryomilled and spark plasma sintered titanium: the evolution of microstructure

NASA Astrophysics Data System (ADS)

Kozlík, Jiří; Becker, Hanka; Harcuba, Petr; Stráský, Josef; Janeček, Milos

2017-05-01

Bulk ultra-fine grained (UFG) commercially pure Ti was prepared by cryogenic milling in liquid argon and subsequent spark plasma sintering (SPS). During cryogenic milling, individual powder particles are repetitively severely deformed by attrition forces. Powder particles were not significantly refined, but due to severe repetitive plastic deformation, ultra-fine grained microstructure emerges within each powder particle. Cryogenic milling can be therefore considered as a specific severe plastic deformation (SPD) method. Compactization of cryomilled powder by SPS technique (also referred to as field assisted sintering technique - FAST) requires significantly lower sintering temperatures and shorter sintering times for successful compaction when compared to any other sintering technique. This is crucial for maintaining the UFG microstructure due to its limited thermal stability. Several specimens were prepared by varying processing parameters, in particular the sintering temperature. The microstructure of powders and compacted samples was observed by scanning electron microscopy (SEM). Increased sintering temperature results in recrystallization and grain growth. A trade-off relationship between the density of compacted material and grain size was identified. Microhardness of the material was found to depend on residual porosity rather than grain size. This contribution presents cryogenic milling and spark plasma sintering as a viable alternative for achieving UFG microstructure in commercially pure Ti.

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

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

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

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.

Sintering and properties of Si3N4 with and without additives by HIP treatment

NASA Technical Reports Server (NTRS)

Kuratani, S.; Shimada, M.; Koizumi, M.

1986-01-01

Hot Isostatic Pressing (HIP) of Si3N4 powders with and without additives was performed using a glass container, and various kinds of pressureless-sintered Si3N4 were HIP'ed without a container. The effects of HIP treatment on density, microstructure, flexural strength, microhardness, and fracture toughness on Si3N4 ceramics were studied. Using a glass container it was difficult to reach theoretical density. The microhardness of HIP'ed Si3N4 without additives was low, and the fracture toughness of HIP'ed Si3N4 with and without additives was 22 to 25 W/m-K, and it decreased with increasing the amount of additives. The density and flexural strength, and hardness of pressureless-sintered Si3N4 which contained Al2O and Y2O3 as oxide additives were remarkably improved by HIP treatment using nitrogen as a pressure transmitting gas. It is very important to select the sintering conditions for fabricating the presintered body of Si3N4 in order to improve the mechanical properties of Si3N4 by HIP treatment.

Development of hydroxyapatite/polyvinyl alcohol bionanocomposite for prosthesis implants

NASA Astrophysics Data System (ADS)

Karthik, V.; Pabi, S. K.; Chowdhury, S. K. Roy

2018-02-01

Hydroxyapatite (Ca10(PO4)6(OH)2) has similar structural and chemical properties of natural bone mineral and hence widely used as a bone replacement substitute. Natural bone consists of hydroxyapatite and collagen. For mimicking the natural, in the present work, a sintered porous hydroxyapatite component has been vacuum impregnated with Polyvinyl alcohol (PVA), which has better properties like biocompatibility, biodegradability and water- solubility. Hydroxyapatite powders have been made into nanosize to reduce the melting point and hence the sintering temperature. In the present investigation high energy ball mill is used to produce nano-hydroxyapatite powders in bulk quantity by optimizing the milling parameters using stainless steel grinding media. Pellets of 10 mm diameter have been produced from nano- hydroxyapatite powders under different uniaxial compaction pressures. The pellets have been sintered to form porous compacts. The vacuum impregnation of sintered pallets with PVA solution of different strength has been done to find the optimum impregnation condition. Microhardness, compressive strength, wear loss and haemocompatibility of hydroxyapatite ceramics have been studied before and after impregnation of PVA. The nano- hydroxyapatite/PVA composites have superior mechanical properties and reduced wear loss than the non-impregnated porous nano-hydroxyapatite ceramics.

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.

A Metal Bump Bonding Method Using Ag Nanoparticles as Intermediate Layer

NASA Astrophysics Data System (ADS)

Fu, Weixin; Nimura, Masatsugu; Kasahara, Takashi; Mimatsu, Hayata; Okada, Akiko; Shoji, Shuichi; Ishizuka, Shugo; Mizuno, Jun

2015-11-01

The future development of low-temperature and low-pressure bonding technology is necessary for fine-pitch bump application. We propose a bump structure using Ag nanoparticles as an intermediate layer coated on a fine-pitch Cu pillar bump. The intermediate layer is prepared using an efficient and cost-saving squeegee-coating method followed by a 100°C baking process. This bump structure can be easily flattened before the bonding process, and the low-temperature sinterability of the nanoparticles is retained. The bonding experiment was successfully performed at 250°C and 39.8 MPa and the bonding strength was comparable to that achieved via other bonding technology utilizing metal particles or porous material as bump materials.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

The effect of the YBCO-PST composite composition on the superconducting carrier concentration determined by microwave studies under high pressure

NASA Astrophysics Data System (ADS)

Krupski, M.; Stankowski, J.; Przybył, S.; Andrzejewski, B.; Kaczmarek, A.; Hilczer, B.; Marfaing, J.; Caranoni, C.

1999-07-01

The effect of hydrostatic pressure ( p<0.6 GPa) on the superconducting critical temperature Tc in YBa 2Cu 3O 7- δ-Pb(Sc 0.5Ta 0.5)O 3 (YBCO-PST) composite is measured by the method of magnetically modulated microwave absorption (MMMA). The Tc dependence on the PST fraction in weight x (0, 0.25, 0.5 and 0.75) is approximated by an inverted parabola function whereas the influence of pressure on Tc is represented by the equation: d Tc/d p=0.61(2)-1.72(6) x. The result may be explained assuming that PST phase in YBCO-PST composite influences the superconducting carrier concentration similar to the chemical substitution in YBa 2Cu 3O 7 [J.J. Neumeier, H.A. Zimmermann, Phys. Rev. B 47 (1993) 8385]. It is suggested that ions from PST diffuse to YBCO cell during the sintering of the composite.

Method of making a layered composite electrode/electrolyte

DOEpatents

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

2005-01-25

An electrode/electrolyte structure is prepared by a plurality of methods. An unsintered (possibly bisque fired) moderately catalytic electronically-conductive or homogeneous mixed ionic electronic conductive electrode material is deposited on a layer composed of a sintered or unsintered ionically-conductive electrolyte material prior to being sintered. A layer of particulate electrode material is deposited on an unsintered ("green") layer of electrolyte material and the electrode and electrolyte layers are sintered simultaneously, sometimes referred to as "co-firing," under conditions suitable to fully densify the electrolyte while the electrode retains porosity. Or, the layer of particulate electrode material is deposited on a previously sintered layer of electrolyte, and then sintered. Subsequently, a catalytic material is added to the electrode structure by infiltration of an electrolcatalyst precursor (e.g., a metal salt such as a transition metal nitrate). This may be followed by low temperature firing to convert the precursor to catalyst. The invention allows for an electrode with high electronic conductivity and sufficient catalytic activity to achieve high power density in an ionic (electrochemical) device such as fuel cells and electrolytic gas separation systems.

Finite element method analysis of cold forging for deformation and densification of Mo alloyed sintered steel

NASA Astrophysics Data System (ADS)

Kamakoshi, Y.; Nishida, S.; Kanbe, K.; Shohji, I.

2017-10-01

In recent years, powder metallurgy (P/M) materials have been expected to be applied to automobile products. Then, not only high cost performance but also more strength, wear resistance, long-life and so on are required for P/M materials. As an improvement method of mechanical properties of P/M materials, a densification is expected to be one of effective processes. In this study, to examine behaviours of the densification of Mo-alloyed sintered steel in a cold-forging process, finite element method (FEM) analysis was performed. Firstly, a columnar specimen was cut out from the inner part of a sintered specimen and a load-stroke diagram was obtained by the compression test. 2D FEM analysis was performed using the obtained load-stroke diagram. To correct the errors of stress between the porous mode and the rigid-elastic mode of analysis software, the analysis of a polynominal approximation was performed. As a result, the modified true stress-true strain diagram was obtained for the sintered steel with the densification. Afterwards, 3D FEM analysis of backward extrusion was carried out using the modified true stress-true strain diagram. It was confirmed that both the shape and density of the sintered steel analyzed by new FEM analysis that we suggest correspond well with experimental ones.

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 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.

Double coating protection of Nd-Fe-B magnets: Intergranular phosphating treatment and copper plating

NASA Astrophysics Data System (ADS)

Zheng, Jingwu; Chen, Haibo; Qiao, Liang; Lin, Min; Jiang, Liqiang; Che, Shenglei; Hu, Yangwu

2014-12-01

In this work, a double coating protection technique of phosphating treatment and copper plating was made to improve the corrosion resistance of sintered Nd-Fe-B magnets. In other words, the intergranular region of sintered Nd-Fe-B is allowed to generate passive phosphate conversion coating through phosphating treatment, followed by the copper coating on the surface of sintered Nd-Fe-B. The morphology and corrosion resistance of the phosphated sintered Nd-Fe-B were observed using SEM and electrochemical method respectively. The phosphate conversion coating was formed more preferably on the intergranular region of sintered Nd-Fe-B than on the main crystal region; just after a short time of phosphating treatment, the intergranular region of sintered Nd-Fe-B has been covered by the phosphate conversion coating and the corrosion resistance is significantly improved. With the synergistic protection of the intergranular phosphorization and the followed copper electrodeposition, the corrosion resistance of the sintered Nd-Fe-B is significantly better than that with a single phosphate film or single plating protection.

Consolidation & Factors Influencing Sintering Process in Polymer Powder Based Additive Manufacturing

NASA Astrophysics Data System (ADS)

Sagar, M. B.; Elangovan, K.

2017-08-01

Additive Manufacturing (AM) is two decade old technology; where parts are build layer manufacturing method directly from a CAD template. Over the years, AM techniques changes the future way of part fabrication with enhanced intricacy and custom-made features are aimed. Commercially polymers, metals, ceramic and metal-polymer composites are in practice where polymers enhanced the expectations in AM and are considered as a kind of next industrial revolution. Growing trend in polymer application motivated to study their feasibility and properties. Laser sintering, Heat sintering and Inhibition sintering are the most successful AM techniques for polymers but having least application. The presentation gives up selective sintering of powder polymers and listed commercially available polymer materials. Important significant factors for effective processing and analytical approaches to access them are discussed.

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.

40 CFR 63.7851 - Who implements and enforces this subpart?

Code of Federal Regulations, 2012 CFR

2012-07-01

... defined in § 63.90, except for approval of an alternative method for the oil content of the sinter plant feedstock or volatile organic compound measurements for the sinter plant windbox exhaust stream stack as...

40 CFR 63.7851 - Who implements and enforces this subpart?

Code of Federal Regulations, 2011 CFR

2011-07-01

... defined in § 63.90, except for approval of an alternative method for the oil content of the sinter plant feedstock or volatile organic compound measurements for the sinter plant windbox exhaust stream stack as...

40 CFR 63.7851 - Who implements and enforces this subpart?

Code of Federal Regulations, 2014 CFR

2014-07-01

... defined in § 63.90, except for approval of an alternative method for the oil content of the sinter plant feedstock or volatile organic compound measurements for the sinter plant windbox exhaust stream stack as...

40 CFR 63.7851 - Who implements and enforces this subpart?

Code of Federal Regulations, 2013 CFR

2013-07-01

... defined in § 63.90, except for approval of an alternative method for the oil content of the sinter plant feedstock or volatile organic compound measurements for the sinter plant windbox exhaust stream stack as...

Method of preparing uranium nitride or uranium carbonitride bodies

DOEpatents

Wilhelm, Harley A.; McClusky, James K.

1976-04-27

Sintered uranium nitride or uranium carbonitride bodies having a controlled final carbon-to-uranium ratio are prepared, in an essentially continuous process, from U.sub.3 O.sub.8 and carbon by varying the weight ratio of carbon to U.sub.3 O.sub.8 in the feed mixture, which is compressed into a green body and sintered in a continuous heating process under various controlled atmospheric conditions to prepare the sintered bodies.

Method of making a composite refractory material

DOEpatents

Morrow, Marvin S.; Holcombe, Cressie E.

1995-01-01

A composite refractory material is prepared by combining boron carbide with furan resin to form a mixture containing about 8 wt. % furan resin. The mixture is formed into a pellet which is placed into a grit pack comprising an oxide of an element such as yttrium to form a sinterable body. The sinterable body is sintered under vacuum with microwave energy at a temperature no greater than 2000.degree. C. to form a composite refractory material.

Method of making a composite refractory material

DOEpatents

Morrow, M.S.; Holcombe, C.E.

1995-09-26

A composite refractory material is prepared by combining boron carbide with furan resin to form a mixture containing about 8 wt. % furan resin. The mixture is formed into a pellet which is placed into a grit pack comprising an oxide of an element such as yttrium to form a sinterable body. The sinterable body is sintered under vacuum with microwave energy at a temperature no greater than 2000 C to form a composite refractory material.

Pressure induced superconductivity in very lightly doped LaFeAsO0.975F0.025

NASA Astrophysics Data System (ADS)

Miyoshi, K.; Otsuka, K.; Shiota, A.; Shimojo, Y.; Motoyama, G.; Fujiwara, K.; Kitagawa, H.; Nishigori, S.

2018-05-01

We have investigated whether or not superconductivity is induced by the application of pressure in very lightly F-doped LaFeAsO1-xFx , which shows spin density wave (SDW) state at ambient pressure, through the measurements of DC magnetization and electrical resistivity under pressure using pulse current sintered (PCS) high density polycrystalline specimens. It has been confirmed that the specimens with x = 0.025 shows superconductivity with Tcdia ∼ 15 K under pressure above ∼ 1.3 GPa. The pressure induced superconductivity can be explained by the lattice compression along c-axis, which enhances the electron doping from LaO layers to FeAs layers.

Development of nano-structured duplex and ferritic stainless steels by pulverisette planetary milling followed by pressureless sintering

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

R, Shashanka, E-mail: shashankaic@gmail.com; Chaira, D., E-mail: chaira.debasis@gmail.com

Nano-structured duplex and ferritic stainless steel powders are prepared by planetary milling of elemental Fe, Cr and Ni powder for 40 h and then consolidated by conventional pressureless sintering. The progress of milling and the continuous refinement of stainless steel powders have been confirmed by means of X-ray diffraction and scanning electron microscopy. Activation energy for the formation of duplex and ferritic stainless steels is calculated by Kissinger method using differential scanning calorimetry and is found to be 159.24 and 90.17 KJ/mol respectively. Both duplex and ferritic stainless steel powders are consolidated at 1000, 1200 and 1400 °C in argonmore » atmosphere to study microstructure, density and hardness. Maximum sintered density of 90% and Vickers microhardness of 550 HV are achieved for duplex stainless steel sintered at 1400 °C for 1 h. Similarly, 92% sintered density and 263 HV microhardness are achieved for ferritic stainless steel sintered at 1400 °C. - Highlights: • Synthesized duplex and ferritic stainless steels by pulverisette planetary milling • Calculated activation energy for the formation of duplex and ferritic stainless steels • Studied the effect of sintering temperature on density, hardness and microstructure • Duplex stainless steel exhibits 90% sintered density and microhardness of 550 HV. • Ferritic stainless steel shows 92% sintered density and 263 HV microhardness.« less

Thermal method for fabricating a hydrogen separation membrane on a porous substrate

DOEpatents

Song, Sun-Ju [Orland Park, IL; Lee, Tae H [Naperville, IL; Chen, Ling [Woodridge, IL; Dorris, Stephen E [LaGrange Park, IL; Balachandran, Uthamalingam [Hinsdale, IL

2009-10-20

A thermal method of making a hydrogen permeable composition is disclosed. A mixture of metal oxide powder and ceramic oxide powder and optionally a pore former is formed and pressed to form an article. The article is dried at elevated temperatures and then sintered in a reducing atmosphere to provide a dense hydrogen permeable portion near the surface of the sintered mixture. The dense hydrogen permeable portion has a higher initial concentration of metal than the remainder of the sintered mixture and is present in the range of from about 20 to about 80 percent by volume of the dense hydrogen permeable portion.

Synthesis and high (pressure, temperature) stability of ZnTiO3 polymorphs studied by Raman spectroscopy

NASA Astrophysics Data System (ADS)

Bernert, T.; Ruiz-Fuertes, J.; Bayarjargal, L.; Winkler, B.

2015-05-01

The phase-purity of ilmenite-type ZnTiO3 prepared by the ceramic method was investigated in dependence of the conditions during ball milling. The previously proposed addition of 2 ml ethanol to the starting materials led to a significant contamination of the product phase after a subsequent sintering process at 1073 K. However, by omitting ethanol this synthesis route led to a phase-pure sample of ZnTiO3 as confirmed by X-ray powder diffraction and Raman spectroscopy. High-temperature high-pressure experiments gave an ilmenite-type to perovskite-type phase boundary with a slope of dT/dP∼-135 K GPa-1 crossing ambient temperature conditions at ∼ 24 GPa in good agreement with previous calculations. Room-temperature high-pressure Raman spectroscopy experiments have shown the stability of the ilmenite-type phase up to a pressure of at least 38.5 GPa, the highest pressure applied in this study, indicating the presence of a kinetic barrier in this phase transition. The synthesis of ferroelectric LiNbO3-type ZnTiO3 was confirmed by second harmonic generation.

Surface-structured diffuser by iterative down-size molding with glass sintering technology.

PubMed

Lee, Xuan-Hao; Tsai, Jung-Lin; Ma, Shih-Hsin; Sun, Ching-Cherng

2012-03-12

In this paper, a down-size sintering scheme for making high-performance diffusers with micro structure to perform beam shaping is presented and demonstrated. By using down-size sintering method, a surface-structure film is designed and fabricated to verify the feasibility of the sintering technology, in which up to 1/8 dimension reduction has been achieved. Besides, a special impressing technology has been applied to fabricate diffuser film with various materials and the transmission efficiency is as high as 85% and above. By introducing the diffuser into possible lighting applications, the diffusers have been shown high performance in glare reduction, beam shaping and energy saving.

High density, uniformly distributed W/UO2 for use in Nuclear Thermal Propulsion

NASA Astrophysics Data System (ADS)

Tucker, Dennis S.; Barnes, Marvin W.; Hone, Lance; Cook, Steven

2017-04-01

An inexpensive, quick method has been developed to obtain uniform distributions of UO2 particles in a tungsten matrix utilizing 0.5 wt percent low density polyethylene. Powders were sintered in a Spark Plasma Sintering (SPS) furnace at 1600 °C, 1700 °C, 1750 °C, 1800 °C and 1850 °C using a modified sintering profile. This resulted in a uniform distribution of UO2 particles in a tungsten matrix with high densities, reaching 99.46% of theoretical for the sample sintered at 1850 °C. The powder process is described and the results of this study are given below.

Fabrication of thin layer beta alumina

NASA Technical Reports Server (NTRS)

Tennenhouse, G. J.

1977-01-01

Beta alumina tubes having walls 700 microns, 300 microns, and 140 microns were processed by extrusion and sintering utilizing Ford proprietary binder and fabrication systems. Tubes prepared by this method have properties similar to tubes prepared by isostatic pressing and sintering, i.e. density greater than 98% of theoretical and a helium leak rate less than 3 x 10 to the -9th power cc/sq cm/sec. Ford ultrasonic bonding techniques were used for bonding beta alumina end caps to open ended beta -alumina tubes prior to sintering. After sintering, the bond was hermetic, and the integrity of the bonded area was comparable to the body of the tube.

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.

Silicon carbide sintered products and a method for their manufacturing

NASA Technical Reports Server (NTRS)

Suzuki, K.

1986-01-01

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

Nuclear Rocket Ceramic Metal Fuel Fabrication Using Tungsten Powder Coating and Spark Plasma Sintering

NASA Technical Reports Server (NTRS)

Barnes, M. W.; Tucker, D. S.; Hone, L.; Cook, S.

2017-01-01

Nuclear thermal propulsion is an enabling technology for crewed Mars missions. An investigation was conducted to evaluate spark plasma sintering (SPS) as a method to produce tungsten-depleted uranium dioxide (W-dUO2) fuel material when employing fuel particles that were tungsten powder coated. Ceramic metal fuel wafers were produced from a blend of W-60vol% dUO2 powder that was sintered via SPS. The maximum sintering temperatures were varied from 1,600 to 1,850 C while applying a 50-MPa axial load. Wafers exhibited high density (>95% of theoretical) and a uniform microstructure (fuel particles uniformly dispersed throughout tungsten matrix).

Influence of sulfur dioxide-related interactions on PM2.5 formation in iron ore sintering.

PubMed

Ji, Zhiyun; Fan, Xiaohui; Gan, Min; Chen, Xuling; Lv, Wei; Li, Qiang; Zhou, Yang; Tian, Ye; Jiang, Tao

2017-04-01

The formation of PM 2.5 (aerosol particulate matter less than 2.5 µm in aerodynamic diameter) in association with SO 2 emission during sintering process has been studied by dividing the whole sintering process into six typical sampling stages. A low-pressure cascade impactor was used to collect PM 2.5 by automatically segregating particulates into six sizes. It was found that strong correlation existed between the emission properties of PM 2.5 and SO 2 . Wet mixture layer (overwetted layer and raw mixture layer) had the function to simultaneously capture SO 2 and PM 2.5 during the early sintering stages, and released them back into flue gas mainly in the flue gas temperature-rising period. CaSO 4 crystals constituted the main SO 2 -related PM 2.5 during the disappearing process of overwetted layer, which was able to form perfect individual crystals or to form particles with complex chemical compositions. Besides the existence of individual CaSO 4 crystals, mixed crystals of K 2 SO 4 -CaSO 4 in PM 2.5 were also found during the first half of the temperature-rising period of flue gas. The interaction between fine-grained Ca-based fluxes, potassium vapors, and SO 2 was the potential source of SO 2 -related PM 2.5 . The emission property of PM 2.5 and SO 2 throughout the sintering process exhibited well similarity. This phenomenon tightened the relationship between the formation of PM 2.5 and the emission of SO 2 . Through revealing the properties of SO 2 -related PM 2.5 during sintering process, the potential interaction between fine-grained Ca-based fluxes, potassium vapors, and SO 2 was found to be the source of SO 2 -related PM 2.5 . This information can serve as the guidance to develop efficient techniques to control the formation and emission of PM 2.5 in practical sintering plants.

Method for preparing boron-carbide articles

DOEpatents

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

1975-10-21

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

FUEL ELEMENTS FOR NUCLEAR REACTORS

DOEpatents

Blainey, A.; Lloyd, H.

1961-07-11

A method of sheathing a tubular fuel element for a nuclear reactor is described. A low melting metal core member is centered in a die, a layer of a powdered sheathing substance is placed on the bottom of the die, the tubular fuel element is inserted in the die, the space between the tubular fuel element and the die walls and core member is filled with the same powdered sheathing substance, a layer of the same substance is placed over the fissile material, and the charge within the die is subjected to pressure in the direction of the axis of the fuel element at the sintering temperature of the protective substance.

Investigation on the effect of sintering temperature on kaolin hollow fibre membrane for dye filtration.

PubMed

Mohtor, Nur Hamizah; Othman, Mohd Hafiz Dzarfan; Ismail, Ahmad Fauzi; Rahman, Mukhlis A; Jaafar, Juhana; Hashim, Nur Awanis

2017-07-01

Despite its extraordinary price, ceramic membrane can still be able to surpass polymeric membrane in the applications that require high temperature and pressure conditions, as well as harsh chemical environment. In order to alleviate the high cost of ceramic material that still becomes one of the major factors that contributes to the high production cost of ceramic membrane, various attempts have been made to use low cost ceramic materials as alternatives to well-known expensive ceramic materials such as alumina, silica, and zirconia in the fabrication of ceramic membrane. Thus, local Malaysian kaolin has been chosen as the ceramic material in this study for the preparation of kaolin hollow fibre membrane since it is inexpensive and naturally abundant in Malaysia. Due to the fact that the sintering process plays a prominent role in obtaining the desired morphology, properties, and performances of prepared ceramic membrane, the aim of this work was to study the effect of different sintering temperatures applied (ranging from 1200 to 1500 °C) in the preparation of kaolin hollow fibre membrane via dry/wet phase inversion-based spinning technique and sintering process. The morphology and properties of membrane were then characterised by SEM, AFM, FTIR, XRD, and three-point bending test, while the performances of membrane were investigated by conducting water permeation and Reactive Black 5 (RB5) dye rejection tests. From the experimental results obtained, the sintering temperature of 1400 °C could be selected as the optimum sintering temperature in preparing the kaolin hollow fibre membrane with the dense sponge-like structure of separation layer that resulted in the good mechanical strength of 70 MPa with the appreciable water permeation of 75 L/h m 2  bar and RB5 rejection of 68%.

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.

X-ray photoelectron spectroscopy (XPS) investigation of the surface film on magnesium powders.

PubMed

Burke, Paul J; Bayindir, Zeynel; Kipouros, Georges J

2012-05-01

Magnesium (Mg) and its alloys are attractive for use in automotive and aerospace applications because of their low density and good mechanical properties. However, difficulty in forming magnesium and the limited number of available commercial alloys limit their use. Powder metallurgy may be a suitable solution for forming near-net-shape parts. However, sintering pure magnesium presents difficulties due to surface film that forms on the magnesium powder particles. The present work investigates the composition of the surface film that forms on the surface of pure magnesium powders exposed to atmospheric conditions and on pure magnesium powders after compaction under uniaxial pressing at a pressure of 500 MPa and sintering under argon at 600 °C for 40 minutes. Initially, focused ion beam microscopy was utilized to determine the thickness of the surface layer of the magnesium powder and found it to be ~10 nm. The X-ray photoelectron analysis of the green magnesium sample prior to sintering confirmed the presence of MgO, MgCO(3)·3H(2)O, and Mg(OH)(2) in the surface layer of the powder with a core of pure magnesium. The outer portion of the surface layer was found to contain MgCO(3)·3H(2)O and Mg(OH)(2), while the inner portion of the layer is primarily MgO. After sintering, the MgCO(3)·3H(2)O was found to be almost completely absent, and the amount of Mg(OH)(2) was also decreased significantly. This is postulated to occur by decomposition of the compounds to MgO and gases during the high temperature of sintering. An increase in the MgO content after sintering supports this theory.

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.

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.

Low-cost optical fabrication of flexible copper electrode via laser-induced reductive sintering and adhesive transfer

NASA Astrophysics Data System (ADS)

Back, Seunghyun; Kang, Bongchul

2018-02-01

Fabricating copper electrodes on heat-sensitive polymer films in air is highly challenging owing to the need of expensive copper nanoparticles, rapid oxidation of precursor during sintering, and limitation of sintering temperature to prevent the thermal damage of the polymer film. A laser-induced hybrid process of reductive sintering and adhesive transfer is demonstrated to cost-effectively fabricate copper electrode on a polyethylene film with a thermal resistance below 100 °C. A laser-induced reductive sintering process directly fabricates a high-conductive copper electrode onto a glass donor from copper oxide nanoparticle solution via photo-thermochemical reduction and agglomeration of copper oxide nanoparticles. The sintered copper patterns were transferred in parallel to a heat-sensitive polyethylene film through self-selective surface adhesion of the film, which was generated by the selective laser absorption of the copper pattern. The method reported here could become one of the most important manufacturing technologies for fabricating low-cost wearable and disposable electronics.

Fabrication and Analysis of the Wear Properties of Hot-Pressed Al-Si/SiCp + Al-Si-Cu-Mg Metal Matrix Composite

NASA Astrophysics Data System (ADS)

Bang, Jeongil; Oak, Jeong-Jung; Park, Yong Ho

2016-01-01

The aim of this study was to characterize microstructures and mechanical properties of aluminum metal matrix composites (MMC's) prepared by powder metallurgy method. Consolidation of mixed powder with gas atomized Al-Si/SiCp powder and Al-14Si-2.5Cu-0.5Mg powder by hot pressing was classified according to sintering temperature and sintering time. Sintering condition was optimized using tensile properties of sintered specimens. Ultimate tensile strength of the optimized sintered specimen was 228 MPa with an elongation of 5.3% in longitudinal direction. In addition, wear properties and behaviors of the sintered aluminum-based MMC's were analyzed in accordance with vertical load and linear speed. As the linear speed and vertical load of the wear increased, change of the wear behavior occurred in order of oxidation of Al-Si matrix, formation of C-rich layer, Fe-alloying to matrix, and melting of the specimen

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.

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.

Toward Interpreting Failure in Sintered-Silver Interconnection Systems

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

Wereszczak, Andrew A; Waters, Shirley B

2016-01-01

The mechanical strength and subsequent reliability of a sintered-silver interconnection system is a function of numerous independent parameters. That system is still undergoing process development. Most of those parameters (e.g., choice of plating) are arguably and unfortunately taken for granted and are independent of the silver s cohesive strength. To explore such effects, shear strength testing and failure analyses were completed on a simple, mock sintered-silver interconnection system consisting of bonding two DBC ceramic substrates. Silver and gold platings were part of the test matrix, as was pre-drying strategies, and the consideration of stencil-printing vs. screen-printing. Shear strength of sintered-silvermore » interconnect systems was found to be was insensitive to the choice of plating, drying practice, and printing method provided careful and consistent processing of the sintered-silver are practiced. But if the service stress in sintered silver interconnect systems is anticipated to exceed ~ 60 MPa, then the system will likely fail.« 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.

Influence of Grain Refinement on Microstructure and Mechanical Properties of Tungsten Carbide/Zirconia Nanocomposites

NASA Astrophysics Data System (ADS)

Nasser, Ali; Kassem, Mohamed A.; Elsayed, Ayman; Gepreel, Mohamed A.; Moniem, Ahmed A.

2016-11-01

WC-W2C/ZrO2 nanocomposites were synthesized by pressure-less sintering (PS) and spark plasma sintering (SPS) of tungsten carbide/yttria-stabilized tetragonal zirconia, WC/TZ-3Y. Prior to sintering, WC/TZ-3Y powders were totally ball-milled for 20 and 120 h to obtain targeted nano (N) and nano-nano (N-N) structures, indicated by transmission electron microscopy and powder x-ray diffraction (PXRD). The milled powders were processed via PS at temperatures of 1773 and 1973 K for 70 min and SPS at 1773 K for 10 min. PXRD as well as SEM-EDS indicated the formation of WC-W2C/ZrO2 composites after sintering. The mechanical properties were characterized via Vicker microhardness and nanoindentation techniques indicating enhancements for sufficiently consolidated composites with high W2C content. The effects of reducing particle sizes on phase transformation, microstructure and mechanical properties are reported. In general, the composites based on the N structure showed higher microhardness than those for N-N structure, except for the samples PS-sintered at 1773 K. For instance, after SPS at 1773 K, the N structure showed a microhardness of 18.24 GPa. Nanoindentation measurements revealed that nanoscale hardness up to 22.33 and 25.34 GPa and modulus of elasticity up to 340 and 560 GPa can be obtained for WC-W2C/ZrO2 nanocomposites synthesized by the low-cost PS at 1973 K and by SPS at 1773 K, respectively.

Clean recycle and utilization of hazardous iron-bearing waste in iron ore sintering process.

PubMed

Gan, Min; Ji, Zhiyun; Fan, Xiaohui; Chen, Xuling; Zhou, Yang; Wang, Guojing; Tian, Ye; Jiang, Tao

2018-04-18

Applying recycled iron-bearing waste materials (RIM) into iron ore sintering process is the general disposal approach worldwide, while its use is still a thorny problem. Results showed that adding RIM increased contents of hazardous elements (K, Na, Pb, Zn, and Cl) in sinter product, and also enhanced emission concentration of PM 2.5 in flue gas; increasing reaction temperature, and contents of CaO & coke breeze in raw mixtures improved hazardous elements removal. Based on these features, a novel method through granulating natural iron ores and RIM separately and distributing granulated RIM in bottom sintering layers was proposed for clean RIM cycle. When recycling 5% RIM, granulating RIM separately with higher contents of CaO and coke breeze removed hazardous elements effectively, the contents of which in sinter were reduced to comparable level of the case without RIM. Moreover, distributing RIM in bottom sintering layer reached intensive release of hazardous elements and PM 2.5 during sintering, which reduced the flue gas volume needing purification by about 2/3. Through activated carbon purification, about 60% of PM 2.5 comprised high contents of hazardous elements was removed. Novel technique eliminated the negative impact of RIM and has the prospect to reach clean recycle in sinter-making plants. Copyright © 2018. Published by Elsevier B.V.

Wettability of eutectic NaLiCO3 salt on magnesium oxide substrates at 778 K

NASA Astrophysics Data System (ADS)

Li, Chuan; Li, Qi; Cao, Hui; Leng, Guanghui; Li, Yongliang; Wang, Li; Zheng, Lifang; Ding, Yulong

2018-06-01

We investigated the wetting behavior of a eutectic carbonate salt of NaLiCO3 on MgO substrates at an elevated temperature of 778 K by measuring contact angle with a sessile drop method. Both sintered and non-sintered MgO were prepared and used as the substrates. The sintered substrates were obtained by sintering compacted MgO powders at 500-1300 °C. For comparison purposes, a single crystal MgO substrate was also used in the work. The different sintering temperatures provided MgO substrates with different structures, allowing their effects on salt penetration and hence wettability and surface energy to be investigated. A scanning electron microscope equipped with energy dispersive spectrometry and an atomic force microscope were used to observe the morphology and structures of the MgO substrates as well as the salt penetration. The results showed a good wettability of the carbonate salt on both the sintered and non-sintered MgO substrates and the wettability depended strongly on the structure of the substrates. The non-sintered MgO substrate has a loose surface particle packing with large pores and crevices, leading to significant salt infiltration, and the corresponding contact angle was measured to be ∼25°. The contact angle of the salt on the sintered MgO substrates increased with an increase in the sintering temperature of the MgO substrate, and the contact angle of the salt on the single crystal substrate was the highest at ∼40°. The effect of the sintering temperature for making the MgO substrate could be linked to the surface energy, and the linkage is validated by the AFM measurements of the adhesion forces of the MgO substrates.

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.

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

Sudiana, I. Nyoman, E-mail: sudiana75@yahoo.com; Ngkoimani, La Ode; Usman, Ida

Microwave sintering of materials has attracted much research interest because of its significant advantages (e.g. reduced sintering temperatures and soaking times) over the conventional heating. Most researchers compared processes that occurred during the microwave and conventional heating at the same temperature and time. The enhancements found in the former method are indicated as a 'non-thermal effect' which is usually used for explaining the phenomena in microwave processing. Numerous recent studies have been focused on the effect to elucidate the microwave interaction mechanism with materials. Moreover, recent progress on microwave sources such as gyrotrons has opened the possibility for processing materialsmore » by using a higher microwave frequency. Therefore, the technology is expected to exhibit a stronger non-thermal effect. This paper presents results from a series of experiments to study the non-thermal effect on microwave sintered alumina. Sintering by using a wide rage of microwave frequencies up to 300 GHz as well as a conventional furnace was carried out. The linear shrinkages of samples for each sintering method were measured. Pores and grains taken from scanning electron microstructure (SEM) images of cut surfaces were also examined. The results of a comparative study of the shrinkages and microstructure evolutions of the sintered samples under annealing in microwave heating systems and in an electric furnace were analyzed. A notably different behavior of the shrinkages and microstructures of alumina after being annealed was found. The results suggested that microwave radiations provided an additional force for mass transports. The results also indicated that the sintering process depended on microwave frequencies.« less

Electrical Conductivity Measurement of Granulite Under Mid to Lower Crustal Pressure-Temperature Conditions

NASA Astrophysics Data System (ADS)

Fuji-Ta, K.; Katsura, T.; Tainosho, Y.

2003-12-01

We have developed a technique to measure electrical conductivity of crustal rocks with relatively low conductivity and complicated mineral components in order to compare with results given by Magneto-Telluric (MT) measurements. A granulite from Hidaka Metamorphic Belt (HMB) in Hokkaido, Japan at high temperature and pressure conditions was obtained. The granulite sample was ground and sintered under the conditions similar to those of mid to lower crust. We have observed smooth and reversible change of conductivity with temperature up to about 900 K at 1 GPa. Through the qualitative and quantitative evaluations using Electron Probe Micro Analysis (EPMA), microstructures of the sintered sample were inspected. This inspection is essential to confirm the sample was not affected by chemical interaction of minerals. We also examined the role of accessory minerals in the rock, and the mechanisms of electrical conductivity paths in _gdry_h or _gbasic_h rocks should be reconsidered. Finally, results from electrical conductivity measurements were consistent with the electrical conductivity structures suggested by the former MT data analysis.

Unusual effects of manual grinding and subsequent annealing process observed in Gd5.09Ge2.03Si1.88 compound

NASA Astrophysics Data System (ADS)

Carvalho, A. M. G.; Alves, C. S.; Trevizoli, P. V.; dos Santos, A. O.; Gama, S.; Coelho, A. A.

2018-03-01

The Gd5.09Ge2.03Si1.88 compound, as well as other magnetocaloric materials, certainly will not be used in their un-manufactured as-cast condition in future magnetic refrigeration applications or other devices. In this work, we have studied the Gd5.09Ge2.03Si1.88 compound processed in different ways, mainly, the as-cast powder, the annealed powder, and the pressed and sintered powder. The annealed powder (1370 K/20 h) does not present the monoclinic phase and the first-order magneto-structural transition observed in the as-cast powder. The pressed and sintered powder also do not present the first-order transition. Furthermore, the compacting pressure shifts the second-order magnetic transition to lower temperatures. The behavior of cell parameters as a function of the compacting pressure indicates that T C is directly affected by parameter c change.

Design of experiment (DOE) study of biodegradable magnesium alloy synthesized by mechanical alloying using fractional factorial design

NASA Astrophysics Data System (ADS)

Salleh, Emee Marina; Ramakrishnan, Sivakumar; Hussain, Zuhailawati

2014-06-01

The biodegradable nature of magnesium (Mg) makes it a most highlighted and attractive to be used as implant materials. However, rapid corrosion rate of Mg alloys especially in electrolytic aqueous environment limits its performance. In this study, Mg alloy was mechanically milled by incorporating manganese (Mn) as alloying element. An attempt was made to study both effect of mechanical alloying and subsequent consolidation processes on the bulk properties of Mg-Mn alloys. 2k-2 factorial design was employed to determine the significant factors in producing Mg alloy which has properties closes to that of human bones. The design considered six factors (i.e. milling time, milling speed, weight percentage of Mn, compaction pressure, sintering temperature and sintering time). Density and hardness were chosen as the responses for assessing the most significant parameters that affected the bulk properties of Mg-Mn alloys. The experimental variables were evaluated using ANOVA and regression model. The main parameter investigated was compaction pressure.

Shock synthesized and static sintered boron nitride cutting tool

NASA Astrophysics Data System (ADS)

Araki, M.; Kuroyama, Y.

1986-05-01

Shock synthesis of wBN (wurtzite phase boron nitride) on an industrial scale was achieved by Nippon Oil & Fats and Showa Denko in 1971. It seemed that the resultant wBN powder might display excellent qualities as a cutting tool material when it was sintered under very high static pressure and temperature because of its polycrystalline nature. Attempts to produce a wBN cutting tool material were commenced by the Tokyo Institute of Technology and Nippon Oil & Fats in 1976 and commercially available wBN cutting tools were first sold in 1980. Meanwhile, a new type of explosion chamber designed to eliminate explosion sound and earth vibration problems, novel high pressure vessels and other peripheral apparatuses have been developed. Now, WURZIN (trademark for the wBN cutting tool) is used in many aspects of the steel cutting field because it is durable when cutting various steels from mild steels to superalloys under high speed, interrupt and precision cutting conditions.

Investigation of Thermoelectric Parameters of Bi2Te3: TEGs Assembled using Pressure-Assisted Silver Powder Sintering-Based Joining Technology

NASA Astrophysics Data System (ADS)

Stranz, Andrej; Waag, Andreas; Peiner, Erwin

2015-06-01

Operation of thermoelectric generator (TEG) modules based on bismuth telluride alloys at temperatures higher than 250°C is mostly limited by the melting point of the assembly solder. Although the thermoelectric parameters of bismuth telluride materials degrade for temperatures >130°C, the power output of the module can be enhanced with an increase in the temperature difference. For this, a temperature-stable joining technique, especially for the hot side of the modules, is required. Fabrication and process parameters of TEG modules consisting of bismuth telluride legs, alumina ceramics and copper interconnects using a joining technique based on pressure-assisted silver powder sintering are described. Measurements of the thermal force, electrical resistance, and output power are presented that were performed for hot side module temperatures up to 350°C and temperature differences higher than 300°C. Temperature cycling and results measured during extended high-temperature operation are addressed.

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.

[The influence of different opaque thickness on the bond strength of porcelain-fused-to metal restoration].

PubMed

Xu, Kan; He, Fan; Geng, Yi

2009-12-01

To study the influence of different opaque thickness on the bond strength of porcelain-fused-to metal (PFM) restorations. The testing sheets were made as the samples of ISO9693. With different sintering temperature and different opaque thickness on the bond strength of PFM restorations, the primary pressure of porcelain crack was measured by using three-points-bending test. Statistical analysis was carried out using a SPSS 10.0 software package. A post hoc multiple comparison test (Student-Newman-Keuls) was performed to evaluate the differences between the individual groups. In low sintering temperature group, the thin layer of opaque significantly improved the bond strength compared with thick layer of opaque (P<0.05). In high sintering temperature group, the thickness of opaque has no significant influence on the PFM bonding strength. Using the opaque, the bonding strength was better than those without opaque. The thickness of opaque has a little influence on the PFM bonding strength.

Crystallization behavior and properties of BaO-Al2O3-2SiO2 glass matrices

NASA Technical Reports Server (NTRS)

Drummond, Charles H., III; Bansal, Narottam P.

1990-01-01

Glass of stoichiometric celsian composition, BaO-Al2O3-SiO2, has a density of 3.39 g/cu cm, a thermal expansion coefficient of 6.6 x 10 to the -6th/C, a glass-transition temperature of 910 C, and a dilatometric softening point of 925 C. On heat treatment, only hexacelsian crystallized out on the surface, but both celsian and hexacelsian were present in the bulk. Effects of cold isostatic pressing (CIP), sintering, and hot-pressing, in the presence and absence of an additive, on the formation of the celsian phase in the glass have been studied. CIP'd samples, after appropriate heat treatments, always crystallized out as celsian, whereas presence of 5-10 wt pct of an additive was necessary for formation of celsian in sintered as well as hot-pressed specimens. Green density increased with CIP'ing pressure but had no effect on sintered density. Hot-pressing resulted in fully dense samples.

Spark Plasma Sintering of Commercial Zirconium Carbide Powders: Densification Behavior and Mechanical Properties

PubMed Central

Wei, Xialu; Back, Christina; Izhvanov, Oleg; Khasanov, Oleg L.; Haines, Christopher D.; Olevsky, Eugene A.

2015-01-01

Commercial zirconium carbide (ZrC) powder is consolidated by Spark Plasma Sintering (SPS). Processing temperatures range from 1650 to 2100 °C. Specimens with various density levels are obtained when performing single-die SPS at different temperatures. Besides the single-die tooling setup, a double-die tooling setup is employed to largely increase the actual applied pressure to achieve higher densification in a shorter processing time. In order to describe the densification mechanism of ZrC powder under SPS conditions, a power-law creep constitutive equation is utilized, whose coefficients are determined by the inverse regression of the obtained experimental data. The densification of the selected ZrC powder is shown to be likely associated with grain boundary sliding and dislocation glide controlled creep. Transverse rupture strength and microhardness of sintered specimens are measured to be up to 380 MPa and 24 GPa, respectively. Mechanical properties are correlated with specimens’ average grain size and relative density to elucidate the co-factor dependencies. PMID:28793550

Recycling of SmCo5 magnets by HD process

NASA Astrophysics Data System (ADS)

Eldosouky, Anas; Škulj, Irena

2018-05-01

Hydrogen decrepitation process has been applied for the first time for the direct recycling of SmCo5 magnets. Industrially produced sintered SmCo5 magnets were decrepitated by hydrogen gas at a pressure of 1 bar to 9.5 bar at room temperature in a planetary rotating jar. After decrepitation, the starting sintered magnets were reduced to a powder with a particle size of less than 200 μm. The produced powder was used for the preparation of recycled SmCo5 magnets. Scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction studies and magnetic measurements were used to follow the decrepitation and the sintering processes. The measured remanence and maximum energy product of the recycled magnet are 0.94 T and 171.1 kJ/m3, respectively, in comparison with 0.91 T and 156.8 kJ/m3, respectively for the original magnet before recycling. It was also observed that, there is refinement in the microstructure after recycling in comparison to the original magnet.

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

DOE PAGES

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

2017-07-14

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

A Review of Metal Injection Molding- Process, Optimization, Defects and Microwave Sintering on WC-Co Cemented Carbide

NASA Astrophysics Data System (ADS)

Shahbudin, S. N. A.; Othman, M. H.; Amin, Sri Yulis M.; Ibrahim, M. H. I.

2017-08-01

This article is about a review of optimization of metal injection molding and microwave sintering process on tungsten cemented carbide produce by metal injection molding process. In this study, the process parameters for the metal injection molding were optimized using Taguchi method. Taguchi methods have been used widely in engineering analysis to optimize the performance characteristics through the setting of design parameters. Microwave sintering is a process generally being used in powder metallurgy over the conventional method. It has typical characteristics such as accelerated heating rate, shortened processing cycle, high energy efficiency, fine and homogeneous microstructure, and enhanced mechanical performance, which is beneficial to prepare nanostructured cemented carbides in metal injection molding. Besides that, with an advanced and promising technology, metal injection molding has proven that can produce cemented carbides. Cemented tungsten carbide hard metal has been used widely in various applications due to its desirable combination of mechanical, physical, and chemical properties. Moreover, areas of study include common defects in metal injection molding and application of microwave sintering itself has been discussed in this paper.

Cantilever testing of sintered-silver interconnects

DOE PAGES

Wereszczak, Andrew A.; Chen, Branndon R.; Jadaan, Osama M.; ...

2017-10-19

Cantilever testing is an underutilized test method from which results and interpretations promote greater understanding of the tensile and shear failure responses of interconnects, metallizations, or bonded joints. The use and analysis of this method were pursued through the mechanical testing of sintered-silver interconnects that joined Ni/Au-plated copper pillars or Ti/Ni/Ag-plated silicon pillars to Ag-plated direct bonded copper substrates. Sintered-silver was chosen as the interconnect test medium because of its high electrical and thermal conductivities and high-temperature capability—attractive characteristics for a candidate interconnect in power electronic components and other devices. Deep beam theory was used to improve upon the estimationsmore » of the tensile and shear stresses calculated from classical beam theory. The failure stresses of the sintered-silver interconnects were observed to be dependent on test-condition and test-material-system. In conclusion, the experimental simplicity of cantilever testing, and the ability to analytically calculate tensile and shear stresses at failure, result in it being an attractive mechanical test method to evaluate the failure response of interconnects.« less

Microwave-Assisted Synthesis of High Dielectric Constant CaCu3Ti4O12 from Sol-Gel Precursor

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Cao, Peng; Huang, Saifang; Zhang, Weijun; Huang, Zhaohui; Gao, Wei

2015-07-01

CaCu3Ti4O12 (CCTO) powders derived from sol-gel precursors were calcined and sintered via microwave radiation. The obtained CCTO powders were compared with that obtained via a conventional heating method. For microwave heating, 89.1 wt.% CCTO was achieved from the sol-gel precursor, after only 17 min at 950°C. In contrast, the conventional calcination method required 3 h to generate 87.6 wt.% CCTO content at 1100°C. In addition, the CCTO powders prepared through 17 min of microwave calcination exhibited a small particle size distribution of D50 = 3.826 μm. It was found that a lengthy hold time of 1 h by microwave sintering is required to obtain a high dielectric constant (3.14 × 103 at 102 Hz) and a reasonably low dielectric loss (0.161) in the sintered CCTO ceramic. Based upon the distinct microstructures, the dielectric responses of the CCTO samples sintered by different methods are attributed to space charge polarization and internal barrier layer capacitor mechanism.

Cantilever testing of sintered-silver interconnects

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

Wereszczak, Andrew A.; Chen, Branndon R.; Jadaan, Osama M.

Cantilever testing is an underutilized test method from which results and interpretations promote greater understanding of the tensile and shear failure responses of interconnects, metallizations, or bonded joints. The use and analysis of this method were pursued through the mechanical testing of sintered-silver interconnects that joined Ni/Au-plated copper pillars or Ti/Ni/Ag-plated silicon pillars to Ag-plated direct bonded copper substrates. Sintered-silver was chosen as the interconnect test medium because of its high electrical and thermal conductivities and high-temperature capability—attractive characteristics for a candidate interconnect in power electronic components and other devices. Deep beam theory was used to improve upon the estimationsmore » of the tensile and shear stresses calculated from classical beam theory. The failure stresses of the sintered-silver interconnects were observed to be dependent on test-condition and test-material-system. In conclusion, the experimental simplicity of cantilever testing, and the ability to analytically calculate tensile and shear stresses at failure, result in it being an attractive mechanical test method to evaluate the failure response of interconnects.« less

Design and Fabrication of an Experimental Microheater Array Powder Sintering Printer

NASA Astrophysics Data System (ADS)

Holt, Nicholas; Zhou, Wenchao

2018-03-01

Microheater array powder sintering (MAPS) is a novel additive manufacturing process that uses an array of microheaters to selectively sinter powder particles. MAPS shows great promise as a new method of printing flexible electronics by enabling digital curing of conductive inks on a variety of substrates. For MAPS to work effectively, a microscale air gap needs to be maintained between the heater array and the conductive ink. In this article, we present an experimental MAPS printer with air gap control for printing conductive circuits. First, we discuss design aspects necessary to implement MAPS. An analysis is performed to validate that the design can maintain the desired air gap between the microheaters and the sintering layer, which consists of a silver nanoparticle ink. The printer is tested by printing conductive lines on a flexible plastic substrate with silver nanoparticle ink. Results show MAPS performs on par with or better than the existing fabrication methods for printed electronics in terms of both the print quality (conductivity of the printed line) and print speed, which shows MAPS' great promise as a competitive new method for digital production of printed electronics.

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.

Si-Ca species modification and microwave sintering for NiZn ferrites

NASA Astrophysics Data System (ADS)

Yang, Yin-Ju; Sheu, Ching-Iuan; Cheng, Syh-Yuh; Chang, Horng-Yi

2004-12-01

NiZn ferrite particles were precoated with Si-Ca precursor by sol-gel method. Thus convention-sintered particles exhibited small grain size about 2 μm and lowered magnetic permeability as well as increased coercive magnetic field effectively. Microwave sintering could suppress grain growth as the same result of conventional sintering specimens with SiO2-CaO precoating. In microwave process, the grain growth inhibition expressed more obviously for the SiO2-CaO precoated specimens. The magnetic permeability (∼300) after SiO2-CaO precoating became lower than original ferrite (∼800) without SiO2-CaO precoating in conventional sintering. However, the magnetic permeability was lowered no matter whether SiO2-CaO precoating in microwave process. On the other hand, microwave sintering possessed short processing time, for example, 1250 °C/5 min, to prohibit ZnO volatilization in accompanied with grain size reduction. Therefore, such contribution increased resistivity to about 12×106 Ω cm compared to 3×106 Ω cm of original NiZn ferrite. The large coercive magnetic field (Hc) was ascribed to the superposition of small grain size and stress induced by microwave sintering.

Characterizing Sintered Nano-Hydroxyapatite Sol-Gel Coating Deposited on a Biomedical Ti-Zr-Nb Alloy

NASA Astrophysics Data System (ADS)

Jafari, Hassan; Hessam, Hamid; Shahri, Seyed Morteza Ghaffari; Assadian, Mahtab; Shairazifard, Shahin Hamtaie Pour; Idris, Mohd Hasbullah

2016-03-01

In this study, sol-gel dip-coating method was used to coat nano-hydroxyapatite on specimens of Ti-14Zr-13Nb alloy for orthopedic applications. The coated specimens were sintered at three different temperatures and time spans to evaluate the impact of sintering process on microstructure, mechanical, bio-corrosion, and bioactivity properties of the coating. Field-emission scanning electron microscopy and x-ray diffraction were used to analyze the coating microstructure. Coating adhesion and mechanical performance were also investigated by scratch testing. Besides, electrochemical corrosion and immersion tests were performed in simulated body fluid to examine the sintering effect on corrosion performance and bioactivity of the coatings, respectively. The evaluations of coated specimens displayed that sintering at elevated temperatures leads to higher surface integrity and improves crystallinity of the nano-hydroxyapatite to approximately 89% which brings about distinctively enhanced mechanical properties. Similarly, it improved the corrosion rate for about 17 times through sintering at 700 °C. Immersion test proved that the coating increased the bioactivity resulted from the dissolution of calcium phosphates into the corresponding environment. It is noticeable that sintering the dip-coated specimens in the nano-hydroxyapatite improves corrosion performance and maintains bioactive behaviors as well.

Method of electrode fabrication for solid oxide electrochemical cells

DOEpatents

Jensen, R.R.

1990-11-20

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

Method of electrode fabrication for solid oxide electrochemical cells

DOEpatents

Jensen, Russell R.

1990-01-01

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

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.

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.

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

NASA Astrophysics Data System (ADS)

Hussain, Mansoor M.; Morris, David R.

1989-02-01

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

NONDESTRUCTIVE QUALITY CONTROL: SOME SPECIAL METHODS OF IRRADIATION TESTING

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

Van der Klis, T.

1961-06-10

S>Various methods, using open radioactive sources are discussed. In one method, oil is used containing Pd/sup 109/ which is adsorbed by Mg compounds with which the object to be tested is covered after it has been enveloped in a photographic film. Another method consists of coking the material in the radioactive oil and then scanning it with a suitable detector. A third method, applied especially to porous materials, uses pressure to promote the penetration of the radioactive oil into the cracks and fissures. The filtered particle technique is also used for detection of cracks or cavities in porous materials, suchmore » as ceramics, cement, graphite pressed powdered metals, and sintered carbides. In this method, radioactive liquids are used along with fluid fluorescent substances. Finally, a method is mentioned in which radioactive powder is made to adhere to the surface of the investigated objects by means of an electrostatic charge. This method is used for quality control of china, glass, email, and electric insulation material. (OID)« less

PATHFINDER ATOMIC POWER PLANT. FILTRATION OF ALUMINUM CORROSION PRODUCTS PRODUCED IN HIGH-TEMPERATURE, HIGH PURITY WATER SYSTEMS

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

Noble, J.H.; Davie, R.L.

1961-05-01

Filter tests were conducted to determine the most suitable filter for removing large quantities of aluminum corrosion product (boehmite) from reactor water. Filters tested included the following: wire-wound, sintered filter elements, sintered ceramic fllter elements, cotton stringwound filter elements, felted-cotton filter elements, cation resin, adsorption resin, diatomaceous earth precoat filter, and a wood-cellulose precoat filter. Parameters measured were flow rate, filter-influent and -effluent boehmite concentration, pressure drop, and final filter load. The pressure drop and efficiency of the filters was correlated with boehmite load. Boehmite deposits on filters as a nonporous gelatinous cake, and causes a rapidly increasing pressure drop.more » Tests indicate that the optimum load with filter elements and precoat filters is achieved at a pressure drop of 25 psi. Very little additional load can be obtained by operating to a higher pressure drop. Of the filters tested, the precoat filter snd 40 to 60 mesh cation resin were the more effective in removing boehmite. The efficiency of the precoat filter was in excess of 99%, and the efficiency of the cation resin was for the most part in excess of 95%. For various reasons, the other filters were eliminated from final consideration. The test program and available literature indicated that an element type precoat filter using wood cellulose as the precoat media would be most suitable for the proposed application. (auth)« less

Synthesis of alloys with controlled phase structure

DOEpatents

Guthrie, Stephen Everett; Thomas, George John; Bauer, Walter; Yang, Nancy Yuan Chi

1999-04-20

A method for preparing controlled phase alloys useful for engineering and hydrogen storage applications. This novel method avoids melting the constituents by employing vapor transport, in a hydrogen atmosphere, of an active metal constituent, having a high vapor pressure at temperatures .apprxeq.300 C. and its subsequent condensation on and reaction with the other constituent (substrate) of an alloy thereby forming a controlled phase alloy and preferably a single phase alloy. It is preferred that the substrate material be a metal powder such that diffusion of the active metal constituent, preferably magnesium, and reaction therewith can be completed within a reasonable time and at temperatures .apprxeq.300 C. thereby avoiding undesirable effects such as sintering, local compositional inhomogeneities, segregation, and formation of unwanted second phases such as intermetallic compounds.

Synthesis of alloys with controlled phase structure

DOEpatents

Guthrie, S.E.; Thomas, G.J.; Bauer, W.; Yang, N.Y.C.

1999-04-20

A method is described for preparing controlled phase alloys useful for engineering and hydrogen storage applications. This novel method avoids melting the constituents by employing vapor transport, in a hydrogen atmosphere, of an active metal constituent, having a high vapor pressure at temperatures {approx_equal}300 C and its subsequent condensation on and reaction with the other constituent (substrate) of an alloy thereby forming a controlled phase alloy and preferably a single phase alloy. It is preferred that the substrate material be a metal powder such that diffusion of the active metal constituent, preferably magnesium, and reaction therewith can be completed within a reasonable time and at temperatures {approx_equal}300 C thereby avoiding undesirable effects such as sintering, local compositional inhomogeneities, segregation, and formation of unwanted second phases such as intermetallic compounds. 4 figs.

Porous calcium polyphosphate bone substitutes: additive manufacturing versus conventional gravity sinter processing-effect on structure and mechanical properties.

PubMed

Hu, Youxin; Shanjani, Yaser; Toyserkani, Ehsan; Grynpas, Marc; Wang, Rizhi; Pilliar, Robert

2014-02-01

Porous calcium polyphosphate (CPP) structures proposed as bone-substitute implants and made by sintering CPP powders to form bending test samples of approximately 35 vol % porosity were machined from preformed blocks made either by additive manufacturing (AM) or conventional gravity sintering (CS) methods and the structure and mechanical characteristics of samples so made were compared. AM-made samples displayed higher bending strengths (≈1.2-1.4 times greater than CS-made samples), whereas elastic constant (i.e., effective elastic modulus of the porous structures) that is determined by material elastic modulus and structural geometry of the samples was ≈1.9-2.3 times greater for AM-made samples. X-ray diffraction analysis showed that samples made by either method displayed the same crystal structure forming β-CPP after sinter annealing. The material elastic modulus, E, determined using nanoindentation tests also showed the same value for both sample types (i.e., E ≈ 64 GPa). Examination of the porous structures indicated that significantly larger sinter necks resulted in the AM-made samples which presumably resulted in the higher mechanical properties. The development of mechanical properties was attributed to the different sinter anneal procedures required to make 35 vol % porous samples by the two methods. A primary objective of the present study, in addition to reporting on bending strength and sample stiffness (elastic constant) characteristics, was to determine why the two processes resulted in the observed mechanical property differences for samples of equivalent volume percentage of porosity. An understanding of the fundamental reason(s) for the observed effect is considered important for developing improved processes for preparation of porous CPP implants as bone substitutes for use in high load-bearing skeletal sites. Copyright © 2013 Wiley Periodicals, Inc.

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

NASA Astrophysics Data System (ADS)

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

2014-02-01

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

Feasibility study of the welding of SiC

NASA Technical Reports Server (NTRS)

Moore, T. J.

1985-01-01

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

Structure and tribological properties of composite materials based on Al-Cu-Fe formed at high pressure

NASA Astrophysics Data System (ADS)

Golovkova, E. A.; Ekimov, E. A.; Ivanov, A. S.; Kruglov, V. S.; Pal', A. F.; Ryabinkin, A. N.; Serov, A. O.; Starostin, A. N.; Tsetlin, M. B.

2017-11-01

The use of high pressure ( 8 GPa) in the formation of composite quasi-crystalline materials from powders made it possible to create practically poreless samples with a density close to the maximum known for this type of quasi-crystals. For samples with a nickel binder, sintered at a temperature of 550°C, a very low coefficient of friction was obtained, which retain its value during the testing.

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.

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.

Effect of sintering temperature on the microstructure and properties of foamed glass-ceramics prepared from high-titanium blast furnace slag and waste glass

NASA Astrophysics Data System (ADS)

Chen, Chang-hong; Feng, Ke-qin; Zhou, Yu; Zhou, Hong-ling

2017-08-01

Foamed glass-ceramics were prepared via a single-step sintering method using high-titanium blast furnace slag and waste glass as the main raw materials The influence of sintering temperature (900-1060°C) on the microstructure and properties of foamed glass-ceramics was studied. The results show that the crystal shape changed from grainy to rod-shaped and finally turned to multiple shapes as the sintering temperature was increased from 900 to 1060°C. With increasing sintering temperature, the average pore size of the foamed glass-ceramics increased and subsequently decreased. By contrast, the compressive strength and the bulk density decreased and subsequently increased. An excessively high temperature, however, induced the coalescence of pores and decreased the compressive strength. The optimal properties, including the highest compressive strength (16.64 MPa) among the investigated samples and a relatively low bulk density (0.83 g/cm3), were attained in the case of the foamed glass-ceramics sintered at 1000°C.

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.

Low sintering temperature glass waste forms for sequestering radioactive iodine

DOEpatents

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

2012-09-11

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

Role of cold isostatic pressing in the formation of the properties of ZrO{sub 2}-base ceramics obtained from ultradisperse powders

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

Akimov, G.Y.; Prokhorov, I.Y.; Gorelik, I.V.

1995-09-01

The physicomechanical properties of ceramics obtained from plasmachemical and sol-gel powders of partially stabilized (3% Y{sub 2}O{sub 3}) zirconia (PSZ) and its compositions with 20% Al{sub 2}O{sub 3} by cold isostatic pressing (CIP) at a pressure of at most 2 GPa and sintering at 1300-1650{degrees}C are investigated. It is established that plasmachemical PSZ exhibits its best properties (K{sub 1c} = 7.8 MPa {center_dot} m{sup 1/2}, a strength of 650 MPa) only after complete disintegration at a CIP of 0.1 GPa and a sintering temperature of 1650{degrees}C, when the material is sintered to a density of 5.5 g/cm{sup 3}. After partialmore » stabilization and CIP at 0.1 GPa the plasmachemical composition of PSZ + 20% Al{sub 2}O{sub 3} is sintered at 1650{degrees}C to a density of 4.7 g/cm{sup 3}, but has K{sub 1c} = 8.5 MPa {center_dot} m{sup 1/2} and a strength of 700 MPa. The deagglomerated sol-gel powder exhibits properties at a level of K{sub 1c} = 12.4 MPa {center_dot} m{sup 1/2} and a strength of 950 MPa at a density above 6.0 g/cm{sup 3} after CIP at 0.3 GPa and sintering at 1450{degrees}C. The latter obviously has the best mechanical properties of all the investigated materials.« less

PREPARATION OF COMPACTS MADE FROM URANIUM AND BERYLLIUM BY SINTERING

DOEpatents

Angier, R.P.

1961-04-11

A powder metallurgical method for making high-density compacts of uranium and beryllium is reported. Powdered UBe/sub 9/ and powdered Be are blended, compacted, and then sintered by rapidly heating to a temperature of approximately 1220 to 1280 deg C in an inert atmosphere.

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.

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.

Improvement of mechanical strength of sintered Mo alloyed steel by optimization of sintering and cold-forging processes with densification

NASA Astrophysics Data System (ADS)

Kamakoshi, Y.; Shohji, I.; Inoue, Y.; Fukuda, S.

2017-10-01

Powder metallurgy (P/M) materials have been expected to be spread in automotive industry. Generally, since sintered materials using P/M ones contain many pores and voids, mechanical properties of them are inferior to those of conventional wrought materials. To improve mechanical properties of the sintered materials, densification is effective. The aim of this study is to improve mechanical strength of sintered Mo-alloyed steel by optimizing conditions in sintering and cold-forging processes. Mo-alloyed steel powder was compacted. Then, pre-sintering (PS) using a vacuum sintering furnace was conducted. Subsequently, coldforging (CF) by a backward extrusion method was conducted to the pre-sintered specimen. Moreover, the cold-forged specimen was heat treated by carburizing, tempering and quenching (CQT). Afterwards, mechanical properties were investigated. As a result, it was found that the density of the PS specimen is required to be more than 7.4 Mg/m3 to strengthen the specimen by heat treatment after CF. Furthermore, density and the microstructure of the PS specimen are most important factors to make the high density and strength material by CF. At the CF load of 1200 kN, the maximum density ratio reached approximately 99% by the use of the PS specimen with proper density and microstructure. At the CF load of 900 kN, although density ratio was high like more than 97.8%, transverse rupture strength decreased sharply. Since densification caused high shear stress and stress concentration in the surface layer, microcracks occurred by the damages of inter-particle sintered connection of the surface layer. On the contrary, in case of the CF load of 1200 kN, ultra-densification of the surface layer occurred by a sufficient plastic flow. Such sufficient compressed specimens regenerated the sintered connections by high temperature heat treatment and thus the high strength densified material was obtained. These processes can be applicable to near net shape manufacturing without surface machining.

Highly conductive electrolyte composites containing glass and ceramic, and method of manufacture

DOEpatents

Hash, M.C.; Bloom, I.D.

1992-10-13

An electrolyte composite is manufactured by pressurizing a mixture of sodium ion conductive glass and an ionically conductive compound at between 12,000 and 24,000 pounds per square inch to produce a pellet. The resulting pellet is then sintered at relatively lower temperatures (800--1200 C), for example 1000 C, than are typically required (1400 C) when fabricating single constituent ceramic electrolytes. The resultant composite is 100 percent conductive at 250 C with conductivity values of 2.5 to 4[times]10[sup [minus]2](ohm-cm)[sup [minus]1]. The matrix exhibits chemical stability against sodium for 100 hours at 250 to 300 C. 1 figure.

Highly conductive electrolyte composites containing glass and ceramic, and method of manufacture

DOEpatents

Hash, Mark C.; Bloom, Ira D.

1992-01-01

An electrolyte composite is manufactured by pressurizing a mixture of sodium ion conductive glass and an ionically conductive compound at between 12,000 and 24,000 pounds per square inch to produce a pellet. The resulting pellet is then sintered at relatively lower temperatures (800.degree. C.-1200.degree. C.), for example 1000.degree. C., than are typically required (1400.degree. C.) when fabricating single constituent ceramic electrolytes. The resultant composite is 100 percent conductive at 250.degree. C. with conductivity values of 2.5 to 4.times.10.sup.-2 (ohm-cm).sup.-1. The matrix exhibits chemical stability against sodium for 100 hours at 250.degree. to 300.degree. C.

Influence of Osmotic Drying with an Aqueous Poly(ethylene Glycol) Liquid Desiccant on Alumina Objects Gelcast with Gelatin

DOE PAGES

Hammel, E. C.; Campa, J. A.; Armbrister, C. E.; ...

2017-09-06

Gelcasting and liquid desiccant drying are novel forming and drying methods used to mitigate common issues associated with the fabrication of complex advanced ceramic objects. Here, the molecular weight and osmotic pressure of aqueous poly(ethylene glycol) (PEG) desiccant solutions were simultaneously varied to understand their influence on the net mass loss rates of gelcast alumina samples prepared using gelatin as a gelling agent. Additionally, the amount of PEG diffusion and water diffusion to and from the ceramic samples after 150 min of immersion in the liquid desiccant was correlated to the solution properties as was the final bulk density ofmore » the sintered samples. Furthermore, solutions with high molecular weight and low osmotic pressure resulted in low PEG gain and low water loss, while solutions with low molecular weight and high osmotic pressure resulted in high PEG gain and high water loss. In some cases, more than 40 wt% of the total water per sample was removed through the liquid desiccant drying process.« less

Additive Manufacturing Thermal Performance Testing of Single Channel GRCop-84 SLM Components

NASA Technical Reports Server (NTRS)

Garcia, Chance P.; Cross, Matthew

2014-01-01

The surface finish found on components manufactured by sinter laser manufacturing (SLM) is rougher (0.013 - 0.0006 inches) than parts made using traditional fabrication methods. Internal features and passages built into SLM components do not readily allow for roughness reduction processes. Alternatively, engineering literature suggests that the roughness of a surface can enhance thermal performance within a pressure drop regime. To further investigate the thermal performance of SLM fabricated pieces, several GRCop-84 SLM single channel components were tested using a thermal conduction rig at MSFC. A 20 kW power source running at 25% duty cycle and 25% power level applied heat to each component while varying water flow rates between 2.1 - 6.2 gallons/min (GPM) at a supply pressure of 550 to 700 psi. Each test was allowed to reach quasi-steady state conditions where pressure, temperature, and thermal imaging data were recorded. Presented in this work are the heat transfer responses compared to a traditional machined OHFC Copper test section. An analytical thermal model was constructed to anchor theoretical models with the empirical data.

Influence of Osmotic Drying with an Aqueous Poly(ethylene Glycol) Liquid Desiccant on Alumina Objects Gelcast with Gelatin

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

Hammel, E. C.; Campa, J. A.; Armbrister, C. E.

Gelcasting and liquid desiccant drying are novel forming and drying methods used to mitigate common issues associated with the fabrication of complex advanced ceramic objects. Here, the molecular weight and osmotic pressure of aqueous poly(ethylene glycol) (PEG) desiccant solutions were simultaneously varied to understand their influence on the net mass loss rates of gelcast alumina samples prepared using gelatin as a gelling agent. Additionally, the amount of PEG diffusion and water diffusion to and from the ceramic samples after 150 min of immersion in the liquid desiccant was correlated to the solution properties as was the final bulk density ofmore » the sintered samples. Furthermore, solutions with high molecular weight and low osmotic pressure resulted in low PEG gain and low water loss, while solutions with low molecular weight and high osmotic pressure resulted in high PEG gain and high water loss. In some cases, more than 40 wt% of the total water per sample was removed through the liquid desiccant drying process.« less

Method of making an air electrode material having controlled sinterability

DOEpatents

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

1994-01-01

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

Method of making an air electrode material having controlled sinterability

DOEpatents

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

1994-08-30

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

Process for microwave sintering boron carbide

DOEpatents

Holcombe, C.E.; Morrow, M.S.

1993-10-12

A method of microwave sintering boron carbide comprises leaching boron carbide powder with an aqueous solution of nitric acid to form a leached boron carbide powder. The leached boron carbide powder is coated with a glassy carbon precursor to form a coated boron carbide powder. The coated boron carbide powder is consolidated in an enclosure of boron nitride particles coated with a layer of glassy carbon within a container for microwave heating to form an enclosed coated boron carbide powder. The enclosed coated boron carbide powder is sintered within the container for microwave heating with microwave energy.

Process for microwave sintering boron carbide

DOEpatents

Holcombe, Cressie E.; Morrow, Marvin S.

1993-01-01

A method of microwave sintering boron carbide comprises leaching boron carbide powder with an aqueous solution of nitric acid to form a leached boron carbide powder. The leached boron carbide powder is coated with a glassy carbon precursor to form a coated boron carbide powder. The coated boron carbide powder is consolidated in an enclosure of boron nitride particles coated with a layer of glassy carbon within a container for microwave heating to form an enclosed coated boron carbide powder. The enclosed coated boron carbide powder is sintered within the container for microwave heating with microwave energy.

Hot isostatic pressing of silicon nitride Sisub3n4 containing zircon, or zirconia and silica

NASA Technical Reports Server (NTRS)

Somiya, S.; Yoshimura, M.; Suzuki, T.; Nishimura, H.

1980-01-01

A hydrothermal synthesis apparatus with a 10 KB cylinder was used to obtain a sintered body of silicon nitride. The sintering auxiliary agents used were zircon (ZrSiO4) and a mixture of zirconia (ZrO2) and silica (SiO2). Experiments were conducted with the amounts of ZrSi04 or ArO2 and SiO2 varying over a wide range and the results compared to discover the quantity of additive which produced sintering in silicon nitride by the hot pressing method.

Application of spark plasma sintering for fabricating Nd-Fe-B composite

NASA Astrophysics Data System (ADS)

Sivkov, A. A.; Ivashutenko, A. S.; Lomakina, A. A.

2015-10-01

Constant magnets are applied in such fields as electric equipment and electric generators with fixed rotor. Rare earth metal neodymium is well known as promising material. Production of magnets by sintering three elements (neodymium, iron and boron) is one the most promising methods. But there are difficulties in choosing the right temperature for sintering and further processing. Structure and properties of the product, consisted of rare earth metals, was analyzed. X-ray analysis of the resulting product and the finished constant magnet was performed. Vickers microhardness was obtained.

Formation of obsidian pyroclasts by sintering of ash particles in the volcanic conduit

NASA Astrophysics Data System (ADS)

Gardner, James E.; Llewellin, Edward W.; Watkins, James M.; Befus, Kenneth S.

2017-02-01

The ranges in intensity and style of volcanic eruptions, from highly explosive Plinian eruptions to quiescent lava extrusions, depend on the style and efficiency of gas loss from ascending magma. Obsidian pyroclasts - small, glassy pieces of quenched magma found in some volcanic tephra beds - may preserve valuable information about magma degassing in their vesicle textures and volatile contents. Accurate interpretation of their textures and volatiles, however, requires understanding the mechanism of formation of the pyroclasts. Obsidian pyroclasts from the ca. 1325-1350 C.E. North Mono eruption of Mono Craters (CA, USA) were analyzed and found to have H2O and CO2 contents indicating that they were formed at pressures in the approximate range of 3-40 MPa. Many also contain domains with differing vesicle textures, separated by boundaries containing xenocrystic material, indicating that they are composed of smaller fragments that have sutured together. More than half of the pyroclasts analyzed contained small (∼10 μm), highly distorted vesicles, with multi-cuspate morphology, interpreted as the remnants of interstitial gas trapped amongst sintered fragments of melt/glass. Rounded vesicles are also common and are interpreted to result from surface tension-driven relaxation of the distorted vesicles. Calculated timescales of sintering and relaxation are consistent with timescales for pyroclast formation indicated by H2O re-equilibration within the heterogeneous pyroclasts. This sintering model for the origin of obsidian pyroclasts is further supported by the observation that spherical vesicles are found mainly in H2O-rich pyroclasts, and distorted vesicles mainly in H2O-poor pyroclasts. We conclude that obsidian pyroclasts generated during the North Mono eruption were formed by cycles of fragmentation, sintering/suturing, and relaxation, over a very wide range of depths within the conduit; we find no evidence to support pumice (foam) collapse as the formation mechanism. Similar textures, and the occurrence of xenolithic material, in obsidian pyroclasts in other eruptions suggest that sintering may be generally responsible for the origin of obsidian pyroclasts. Our conceptual model indicates that volatile contents in obsidian pyroclasts reflect both degassing of bubbly magma and the composition of gas trapped between sintering particles.

Method of making sintered ductile intermetallic-bonded ceramic composites

DOEpatents

Plucknett, Kevin; Tiegs, Terry N.; Becher, Paul F.

1999-01-01

A method of making an intermetallic-bonded ceramic composite involves combining a particulate brittle intermetallic precursor with a particulate reactant metal and a particulate ceramic to form a mixture and heating the mixture in a non-oxidizing atmosphere at a sufficient temperature and for a sufficient time to react the brittle intermetallic precursor and the reactant metal to form a ductile intermetallic and sinter the mixture to form a ductile intermetallic-bonded ceramic composite.

Fabrication of Titanium-Niobium-Zirconium-Tantalium Alloy (TNZT) Bioimplant Components with Controllable Porosity by Spark Plasma Sintering

PubMed Central

Rechtin, Jack; Torresani, Elisa; Ivanov, Eugene; Olevsky, Eugene

2018-01-01

Spark Plasma Sintering (SPS) is used to fabricate Titanium-Niobium-Zirconium-Tantalum alloy (TNZT) powder—based bioimplant components with controllable porosity. The developed densification maps show the effects of final SPS temperature, pressure, holding time, and initial particle size on final sample relative density. Correlations between the final sample density and mechanical properties of the fabricated TNZT components are also investigated and microstructural analysis of the processed material is conducted. A densification model is proposed and used to calculate the TNZT alloy creep activation energy. The obtained experimental data can be utilized for the optimized fabrication of TNZT components with specific microstructural and mechanical properties suitable for biomedical applications. PMID:29364165

Microstructure and hardness of the Cu-SiC and Cu-diamond composites produced by vacuum hot pressing

NASA Astrophysics Data System (ADS)

Krishna, S. Chenna; Vikram, T.; Viswanath, S.; Subramanian, P. K.; Janardhana Reddy, J.

2018-03-01

In the present investigation, Cu-SiC and Cu-diamond composites with different volume percent of reinforcements were produced by vacuum hot pressing. Copper powder with different amount of SiC and diamond were hot pressed at 1000°C for 0.5 h at an applied pressure of 32 MPa. The achieved sintered density of the composites was in the range of 94-98 %. The sintered density decreased with an increase in the amount of SiC and diamond. Hardness of the composites improved with an increase in the volume percent of the reinforcements. Hardness of the Cu-30 vol.% diamond and Cu-30vol. % SiC composites was 88 VHN and 104 VHN, respectively.

Tribological behaviour and statistical experimental design of sintered iron-copper based composites

NASA Astrophysics Data System (ADS)

Popescu, Ileana Nicoleta; Ghiţă, Constantin; Bratu, Vasile; Palacios Navarro, Guillermo

2013-11-01

The sintered iron-copper based composites for automotive brake pads have a complex composite composition and should have good physical, mechanical and tribological characteristics. In this paper, we obtained frictional composites by Powder Metallurgy (P/M) technique and we have characterized them by microstructural and tribological point of view. The morphology of raw powders was determined by SEM and the surfaces of obtained sintered friction materials were analyzed by ESEM, EDS elemental and compo-images analyses. One lot of samples were tested on a "pin-on-disc" type wear machine under dry sliding conditions, at applied load between 3.5 and 11.5 × 10-1 MPa and 12.5 and 16.9 m/s relative speed in braking point at constant temperature. The other lot of samples were tested on an inertial test stand according to a methodology simulating the real conditions of dry friction, at a contact pressure of 2.5-3 MPa, at 300-1200 rpm. The most important characteristics required for sintered friction materials are high and stable friction coefficient during breaking and also, for high durability in service, must have: low wear, high corrosion resistance, high thermal conductivity, mechanical resistance and thermal stability at elevated temperature. Because of the tribological characteristics importance (wear rate and friction coefficient) of sintered iron-copper based composites, we predicted the tribological behaviour through statistical analysis. For the first lot of samples, the response variables Yi (represented by the wear rate and friction coefficient) have been correlated with x1 and x2 (the code value of applied load and relative speed in braking points, respectively) using a linear factorial design approach. We obtained brake friction materials with improved wear resistance characteristics and high and stable friction coefficients. It has been shown, through experimental data and obtained linear regression equations, that the sintered composites wear rate increases with increasing applied load and relative speed, but in the same conditions, the frictional coefficients slowly decrease.

Magnesium Powder Injection Molding (MIM) of Orthopedic Implants for Biomedical Applications

NASA Astrophysics Data System (ADS)

Wolff, M.; Schaper, J. G.; Suckert, M. R.; Dahms, M.; Ebel, T.; Willumeit-Römer, R.; Klassen, T.

2016-04-01

Metal injection molding (MIM) has a high potential for the economic near-net-shape mass production of small-sized and complex-shaped parts. The motivation for launching Mg into the MIM processing chain for manufacturing biodegradable medical implants is related to its compatibility with human bone and its degradation in a non-toxic matter. It has been recognized that the load-bearing capacity of MIM Mg parts is superior to that of biodegradable polymeric components. However, the choice of appropriate polymeric binder components and alloying elements enabling defect-free injection molding and sintering is a major challenge for the use of MIM Mg parts. This study considered the full processing chain for MIM of Mg-Ca alloys to achieve ultimate tensile strength of up to 141 MPa with tensile yield strength of 73 MPa, elongation at fracture Af of 7% and a Young's modulus of 38 GPa. To achieve these mechanical properties, a thermal debinding study was performed to determine optimal furnace and atmosphere conditions, sintering temperature, heating rates, sintering time and pressure.

Crystallization behavior and properties of BaO-Al2O3-2SiO2 glass matrices

NASA Technical Reports Server (NTRS)

Drummond, Charles H., III; Bansal, Narottam P.

1990-01-01

Glass of stoichiometric celsian composition, BaO-Al2O3-2SiO2, is a potential glass-ceramic matrix for high-temperature composites. The glass has a density of 3.39 g/cu cm, thermal expansion coefficient of 6.6 x 10(exp -6)/deg C glass transition temperature of 910 C, and dilatometric softening point of 925 C. On heat treatment, only hexacelsian crystallized out on the surface, but both celsian and hexacelsian were present in the bulk. Effects of cold isostatic pressing (CIP), sintering, and hot pressing, in the presence and absence of an additive, on the formation of the celsian phase in the glass were studied. CIP'ed samples, after appropriate heat treatments, always crystallized out as celsian whereas the presence of 5 to 10 weight percent of an additive was necessary for formation of celsian in sintered as well as hot pressed specimens. Green density increased with CIP'ing pressure but had no effect on sintered density. Hot pressing resulted in fully dense samples.

Influence of different heat treatment methods of titania film on performance of DSSCs

NASA Astrophysics Data System (ADS)

More, Venumadhav; Mokurala, Krishna; Bhargava, Parag

2018-04-01

Titania mesoporous film is a key component of dye-sensitized solar cells (DSSCs) as it transfers electrons from dye molecule to external circuit through the transparent conducting oxide (TCO). Interparticle connectivity, porosity and cracks in the titania films play an important role in determining the performance of DSSCs. The heating schedule with respect to the repetitive coating to build up titania film thickness impacts the titania film characteristics. In the present study, experiments were designed to carry out heat treatments with expectation of improving connectivity and healing cracks. Repetitive screen printing was carried out with either heat treatment after each print step (multiple sintering) or the heat treatment was carried out just once after the desired thickness had been attained (single-step sintering). Interconnectivity of the titania particles in the sintered titania film was analyzed by impedance spectroscopy and nanoindentation. Titania films sintered by MS showed better performance in terms of higher efficiency for the corresponding DSSCs than those prepared using titania films sintered by SS.

Peridynamic Theory as a New Paradigm for Multiscale Modeling of Sintering

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

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

2017-09-01

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

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.

Installation and certification of continuous VOC emissions monitoring systems for a steel mill sinter plant

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

Taylor, K.L.; Macak, J.J. III; Cioffi, J.

1999-07-01

The counties of Lake, Porter, and LaPorte in Northwest Indiana are classified as severe non-attainment for the ozone National Ambient Air Quality Standard (NAAQS). In response to the non-attainment problem, the Indiana Department of Environmental Management (IDEM) promulgated a number of regulations over the last several years. One of these rules requires steel mills with sinter plants to control and continuously monitor volatile organic compound (VOC) emissions from the facilities. One of the accepted compliance methods is to install and certify Continuous Emission Monitoring Systems (CEMS) to monitor VOC emissions and volumetric flow rate in order to generate a VOCmore » emission number in units of pounds per hour. Compliance with the regulation also requires that the sinter plants accurately monitor sinter production in order to determine compliance during the winter months, when the limits are based on pounds of VOC emissions per ton of sinter produced.« less

Effect of Silver Flakes in Silver Paste on the Joining Process and Properties of Sandwich Power Modules (IGBTs Chip/Silver Paste/Bare Cu)

NASA Astrophysics Data System (ADS)

Zhao, Su-Yan; Li, Xin; Mei, Yun-Hui; Lu, Guo-Quan

2016-11-01

In this study, a silver paste has been introduced for attaching chips onto bare Cu substrates (without coating) without applying pressure. Small nano-thickness Ag flakes, measuring 1 μm-5 μm length, were embedded uniformly in Ag nanoparticles for improving the density of the material. The presence of silver flakes in the silver paste affected the joining process and its microstructure. Microstructure characterization revealed that densification of the silver layer was affected by the presence of silver flakes as the flakes coarsened and formed reactive in situ nanoparticles, which facilitated the sintering between the flakes and the incorporated nanoparticles. Coarsening of silver flakes depended on the sintering temperature, time, and the atmosphere, which affected the decomposition and burning out of organics presented on the surface of the flakes. A high-density silver layer was obtained due to the presence of compact silver flakes. With an increase in the microstructure density, a higher bonding strength and a lower thermal impedance of the sintered joints were achieved. On performing pressureless sintering at 270°C for 30 min under 99.99% N2 or 4% H2/N2, the bonding strength and thermal impedance for 11 × 11 mm2 chips were excellent, measuring approximately 21.9 MPa and 0.077°C/W, respectively.

Applying "Spark Plasma Sintering" Technology to Enhance the Resistance to Contact Fatigue of Sintered Steel Based on Astaloy CRL

NASA Astrophysics Data System (ADS)

Rodziňák, D.; Čerňan, J.; Puchý, V.

2017-12-01

The article deals with the effect of porosity on the contact fatigue of sintered material type Astaloy CrL with 0.3 and 0.4% C. Sets of samples were used with densities beginning from the value of 7000 kg.m-3 to the value of almost 7859 kg.m-3 which represents almost zero porosity (compact material). It has been found out that the increase of compacting pressure applied simultaneously with temperature results in the reduction of porosity from the value of 9.10% to 0.0005% and increase in hardness from 145 to 193 HV10, depending on the carbon content. Logically there is also an increase in the fatigue life by the contact fatigue tests for the value of 50×106 cycles from the value of 900 MPa to 1150 MPa for samples with 0.3% of C and from 900 MPa to 1300 MPa for samples with 0.4% C. These investigations were also carried out in the past, but to achieve the reduction of porosity, different technonologies were used at each level such as double pressing, hot pressing, saturation, hot forging, etc. In this case, the single technology of "spark plasma sintering" making use of compacting at high temperatures is capable to continuously reduce porosity to zero.

77 FR 44204 - Approval and Promulgation of Air Quality Implementation Plans; Maryland; Control of Iron and...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-07-27

... to approve revisions to the Maryland State Implementation Plan (SIP) submitted by the Maryland... (Sparrows Point) is the only sintering plant located in the State of Maryland, and therefore the only source... compliance with specified pressure drop and flow rate operating parameters. EPA is approving these revisions...

77 FR 44146 - Approval and Promulgation of Air Quality Implementation Plans; Maryland; Control of Iron and...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-07-27

... taking direct final action to approve revisions to the Maryland State Implementation Plan (SIP) submitted... steelmaking facility (Sparrows Point) is the only sintering plant located in the State of Maryland. The... emissions of particulate matter, continuously monitoring compliance with specified pressure drop and flow...

Prototype Development of Remote Operated Hot Uniaxial Press (ROHUP) to Fabricate Advanced Tc-99 Bearing Ceramic Waste Forms - 13381

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

Alaniz, Ariana J.; Delgado, Luc R.; Werbick, Brett M.

The objective of this senior student project is to design and build a prototype construction of a machine that simultaneously provides the proper pressure and temperature parameters to sinter ceramic powders in-situ to create pellets of rather high densities of above 90% (theoretical). This ROHUP (Remote Operated Hot Uniaxial Press) device is designed specifically to fabricate advanced ceramic Tc-99 bearing waste forms and therefore radiological barriers have been included in the system. The HUP features electronic control and feedback systems to set and monitor pressure, load, and temperature parameters. This device operates wirelessly via portable computer using Bluetooth{sup R} technology.more » The HUP device is designed to fit in a standard atmosphere controlled glove box to further allow sintering under inert conditions (e.g. under Ar, He, N{sub 2}). This will further allow utilizing this HUP for other potential applications, including radioactive samples, novel ceramic waste forms, advanced oxide fuels, air-sensitive samples, metallic systems, advanced powder metallurgy, diffusion experiments and more. (authors)« less

Bench-scale synthesis of nanoscale materials

NASA Technical Reports Server (NTRS)

Buehler, M. F.; Darab, J. G.; Matson, D. W.; Linehan, J. C.

1994-01-01

A novel flow-through hydrothermal method used to synthesize nanoscale powders is introduced by Pacific Northwest Laboratory. The process, Rapid Thermal Decomposition of precursors in Solution (RTDS), uniquely combines high-pressure and high-temperature conditions to rapidly form nanoscale particles. The RTDS process was initially demonstrated on a laboratory scale and was subsequently scaled up to accommodate production rates attractive to industry. The process is able to produce a wide variety of metal oxides and oxyhydroxides. The powders are characterized by scanning and transmission electron microscopic methods, surface-area measurements, and x-ray diffraction. Typical crystallite sizes are less than 20 nanometers, with BET surface areas ranging from 100 to 400 sq m/g. A description of the RTDS process is presented along with powder characterization results. In addition, data on the sintering of nanoscale ZrO2 produced by RTDS are included.

Low temperature sintering of fluorapatite glass-ceramics.

PubMed

Denry, Isabelle; Holloway, Julie A

2014-02-01

Fluorapatite glass-ceramics have been shown to be excellent candidates as scaffold materials for bone grafts, however, scaffold production by sintering is hindered by concurrent crystallization of the glass. Objective, our goal was to investigate the effect of Ca/Al ratio on the sintering behavior of Nb-doped fluorapatite-based glasses in the SiO2-Al2O3-P2O5-MgO-Na2O-K2O-CaO-CaF2 system. Methods, glass compositions with Ca/Al ratio of 1 (A), 2 (B), 4 (C) and 19 (D) were prepared by twice melting at 1525°C for 3h. Glasses were either cast as cylindrical ingots or ground into powders. Disk-shaped specimens were prepared by either sectioning from the ingots or powder-compacting in a mold, followed by heat treatment at temperatures ranging between 700 and 1050°C for 1h. The density was measured on both sintered specimens and heat treated discs as controls. The degree of sintering was determined from these measurements. Results and Significance XRD showed that fluorapatite crystallized in all glass-ceramics. A high degree of sintering was achieved at 775°C for glass-ceramic D (98.99±0.04%), and 900°C for glass-ceramic C (91.31±0.10). Glass-ceramics A or B were only partially sintered at 1000°C (63.6±0.8% and 74.1±1.5%, respectively). SEM revealed a unique microstructure of micron-sized spherulitic fluorapatite crystals in glass-ceramics C and D. Increasing the Ca/Al ratio promoted low temperature sintering of fluorapatite glass-ceramics, which are traditionally difficult to sinter. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Sintering polycrystalline olivine and polycrystalline clinopyroxene containing trace amount of graphite from natural crystals

NASA Astrophysics Data System (ADS)

Tsubokawa, Yumiko; Ishikawa, Masahiro

2017-09-01

Graphite-bearing polycrystalline olivine and polycrystalline clinopyroxene with submicron to micron grain size were successfully sintered from a single crystal of naturally occurring olivine (Fo88-92Fa12-8: Mg1.76-1.84Fe0.16-0.24SiO4) and a single crystal of naturally occurring clinopyroxene (Di99Hed1: Ca0.92Na0.07Mn0.01Mg0.93Fe0.01Al0.06Si2O6). The milled powders of both these crystals were sintered under argon gas flow at temperatures ranging from 1130 to 1350 °C for 2 h. As the sintering temperature increased, the average grain size of olivine increased from 0.2 to 1.4 µm and that of clinopyroxene increased from 0.1 to 2.4 µm. The porosity of sintered samples remained at an almost-constant volume of 2-5% for olivine and 3-4% for clinopyroxene. The samples sintered from powders milled with ethanol exhibited trace amount of graphite, identified via Raman spectroscopy analysis. As the sintering temperature increased, the intensity of the graphite Raman peak decreased, compared with both olivine and clinopyroxene peaks. The carbon content of the sintered samples was estimated to be a few hundred ppm. The in-plane size ( L a ) of graphite in the sintered olivine was estimated to be <15 nm. Our experiments demonstrate new possibilities for preparing graphite-bearing silicate-mantle mineral rocks, and this method might be useful in understanding the influence of the physical properties of graphite on grain-size-sensitive rheology or the seismic velocity of the Earth's mantle.[Figure not available: see fulltext.

Thermal and Electrical Characterization of Alumina Substrate for Microelectronic Applications

NASA Astrophysics Data System (ADS)

Ahmad, S.; Ibrahim, A.; Alias, R.; Shapee, S. M.; Ambak, Z.; Zakaria, S. Z.; Yahya, M. R.; Mat, A. F. A.

2010-03-01

This paper reports the effect of sintering temperature on thermal and electrical properties of alumina material as substrate for microelectronic devices. Alumina materials in the form of green sheet with 1 mm thickness were sintered at 1100° C, 1300° C and 1500° C for about 20 hours using heating and cooling rates of 2° C/min. The densities were measured using densitometer and the microstructures of the samples were analyzed using SEM micrographs. Meanwhile thermal and electrical properties of the samples were measured using flash method and impedance analyzer respectively. It was found that thermal conductivity and thermal diffusivity of the substrate increases as sintering temperature increases. It was found also that the dielectric constant of alumina substrate increases as the sintering temperature increases.

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

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

Patil, J.Y.; Mulla, I.S.; Suryavanshi, S.S., E-mail: sssuryavanshi@rediffmail.com

2013-02-15

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

Numerical Study of the Features of Ti-Nb Alloy Crystallization during Selective Laser Sintering

NASA Astrophysics Data System (ADS)

Dmitriev, A. I.; Nikonov, A. Y.

2016-07-01

The demand for implants with individual shape requires the development of new methods and approaches to their production. The obvious advantages of additive technologies and selective laser sintering are the capabilities to form both the external shape of the product and its internal structure. Recently appeared and attractive from the perspective of biomechanical compatibility are beta alloys of titanium-niobium that have similar mechanical properties to those of cortical bone. This paper studies the processes occurring at different stages of laser sintering using computer simulation on atomic scale. The effect of cooling rate on the resulting crystal structure of Ti-Nb alloy was analysed. Also, the dependence of tensile strength of sintered particles on heating time and cooling rate was studied. It was shown that the main parameter, which determines the adhesive properties of sintered particles, is the contact area obtained during sintering process. The simulation results can both help defining the technological parameters of the process to provide the desired mechanical properties of the resulting products and serve as a necessary basis for calculations on large scale levels in order to study the behaviour of actually used implants.

[Rapid prototyping: a very promising method].

PubMed

Haverman, T M; Karagozoglu, K H; Prins, H-J; Schulten, E A J M; Forouzanfar, T

2013-03-01

Rapid prototyping is a method which makes it possible to produce a three-dimensional model based on two-dimensional imaging. Various rapid prototyping methods are available for modelling, such as stereolithography, selective laser sintering, direct laser metal sintering, two-photon polymerization, laminated object manufacturing, three-dimensional printing, three-dimensional plotting, polyjet inkjet technology,fused deposition modelling, vacuum casting and milling. The various methods currently being used in the biomedical sector differ in production, materials and properties of the three-dimensional model which is produced. Rapid prototyping is mainly usedforpreoperative planning, simulation, education, and research into and development of bioengineering possibilities.

METHOD FOR PREPARATION OF SINTERABLE BERYLLIUM OXIDE

DOEpatents

Sturm, B.J.

1963-08-13

High-purity beryllium oxide for nuclear reactor applications can be prepared by precipitation of beryllium oxalate monohydrate from aqueous solution at a temperature above 50 deg C and subsequent calcination of the precipitate. Improved purification with respect to metallic impurities is obtained, and the product beryllium oxide sinters reproducibly to a high density. (AEC)

Microwave sintering of boron carbide

DOEpatents

Blake, R.D.; Katz, J.D.; Petrovic, J.J.; Sheinberg, H.

1988-06-10

A method for forming boron carbide into a particular shape and densifying the green boron carbide shape. Boron carbide in powder form is pressed into a green shape and then sintered, using a microwave oven, to obtain a dense boron carbide body. Densities of greater than 95% of theoretical density have been obtained. 1 tab.

Lunar in situ resource utilization by activated thermites

NASA Astrophysics Data System (ADS)

Hobosyan, Mkhitar; Martirosyan, Karen

2011-10-01

NASA's anticipated returns to the Moon by 2020, subsequent establishment of lunar in situ resource utilization technologies are essential. The surface of Moon is covered with small eroded particles of regolith called lunar dust that adheres electro-statically to everything coming in contact with it, and is of much concern for future lunar base because of its continual mitigation. The next major concern is the protection of equipment and personnel in long term expeditions from harmful UV radiation, which can be made by constructing protective buildings. For construction of permanent structures it is highly desired to have regular shaped sintered regolith with utilization of local materials and with minimum energy consumption. In this study the concept of sintering of lunar regolith with activated thermite reactions is discussed. The thermodynamic calculations as well as the experimental procedure is provided to prove the effectiveness of activated thermites for regolith sintering using local lunar resources with a low (15 wt. %) concentration of aluminum or magnesium. The thermite method is much more energy efficient than the other sintering methods suggested in literature.

Microstructures and mechanical properties of powder injection molded Ti-6Al-4V/HA powder.

PubMed

Thian, E S; Loh, N H; Khor, K A; Tor, S B

2002-07-01

Taguchi method with an L9 orthogonal array was employed to investigate the sintered properties of Ti-6Al-4V/HA tensile bars produced by powder injection molding. The effects of sintering factors at the 90% significance level: sintering temperature (1050 degrees C, 1100 degrees C and 1150 degrees C), heating rate (5 degrees C/min, 7.5 degrees C/min and 10 degrees C/min), holding time (30, 45 and 60 min) and cooling rate (5 degrees C/min, 20 degrees C/min and 40 degrees C/min) were investigated. Results showed that sintering temperature, heating rate and cooling rate have significant effects on sintered properties, whereas the influence of holding time was insignificant. It was found that a sintering temperature of 1100 degrees C, a heating rate of 7.5 degrees C/min and a cooling rate of 5 degrees C/min increased the relative density, Vicker's microhardness, flexural strength and flexural modulus. However, a further increment of sintering temperature to 1150 degrees C did not show any discernable improvement in the relative density and Vicker's microhardness, but there was a slight increase of 0.6% and 0.9% in the flexural strength and flexural modulus, respectively. Mechanically strong Ti-6Al-4V/HA parts with an open porosity of around 50% were developed.

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.

Method of making sintered ductile intermetallic-bonded ceramic composites

DOEpatents

Plucknett, K.; Tiegs, T.N.; Becher, P.F.

1999-05-18

A method of making an intermetallic-bonded ceramic composite involves combining a particulate brittle intermetallic precursor with a particulate reactant metal and a particulate ceramic to form a mixture and heating the mixture in a non-oxidizing atmosphere at a sufficient temperature and for a sufficient time to react the brittle intermetallic precursor and the reactant metal to form a ductile intermetallic and sinter the mixture to form a ductile intermetallic-bonded ceramic composite. 2 figs.

A new 6-axis apparatus to squeeze the Kawai-cell of sintered diamond cubes

NASA Astrophysics Data System (ADS)

Ito, Eiji; Katsura, Tomoo; Yamazaki, Daisuke; Yoneda, Akira; Tado, Masashi; Ochi, Takahiro; Nishibara, Eiichi; Nakamura, Akihiro

2009-05-01

In order to overcome disadvantages of the DIA type press in squeezing the Kawai-cell, such as uneven compression between the upper and lower anvils and the four surrounding anvils and frictional loss of applied load in the guide block, we have developed a new 6-axis apparatus in which the movements of the six anvils are controlled by a servo mechanism. It is possible to keep the Kawai-cell cubic within an accuracy of ±2 μm during compression and decompression. Pressure generation using sintered diamond cubic anvils with edge length of 14.0 mm and a truncation of 1.5 mm has been carried out up to ca. 60 GPa by measuring electrical resistance of GaP, Zr, and Fe 2O 3. The results are compared with our previous calibration, carried out using an almost the same sample setup for identical anvils at SPring-8, by means of in situ X-ray observation. It is demonstrated that a significant amount of the applied load is lost by friction when the Kawai-cell is squeezed in the DIA type press. The load loss increases with increasing load, or pressure, and amounts to 45% at ca. 60 GPa. Therefore the 6-axis apparatus is very advantageous to generate higher pressures in the Kawai-cell. However, individual control of the anvils sometimes induces a runaway advancement of the anvils which brings about an abrupt increase of pressure.

Effects of Ceramic Density and Sintering Temperature on the Mechanical Properties of a Novel Polymer-Infiltrated Ceramic-Network Zirconia Dental Restorative (Filling) Material.

PubMed

Li, Weiyan; Sun, Jian

2018-05-10

BACKGROUND Polymer-infiltrated ceramic-network (PICN) dental material is a new and practical development in orthodontics. Sintering is the process of forming a stable solid mass from a powder by heating without melting. The aim of this study was to evaluate the effects of sintering temperature on the mechanical properties of a PICN zirconia dental material. MATERIAL AND METHODS A dense zirconia ceramic and four PICN zirconia dental materials, with varying porosities, were sintered at three different temperatures; 12 PICN zirconia dental materials based on these porous ceramics were prepared, as well as a pure polymer. After the specimen preparation, flexural strength and elastic modulus values were measured using the three-point bending test, and fracture toughness were determined by the single-edge notched beam (SENB) method. The Vickers hardness test method was used with an indentation strength (IS) test. Scanning electron microscopy (SEM) was used to examine the microstructure of the ceramic surface and the fracture surface. RESULTS Mechanical properties of the PICN dental materials, including flexural strength, elastic modulus, fracture toughness, and hardness, were more similar to the properties of natural teeth when compared with traditional dental ceramic materials, and were affected by the density and sintering temperature. SEM showed that the porous ceramic network became cohesive and that the length of cracks in the PICN dental material was reduced. CONCLUSIONS PICN zirconia dental materials were characterized by similar mechanical properties to natural dental tissues, but further studies are required continue to improve the similarities with natural human enamel and dentin.

Effects of Ceramic Density and Sintering Temperature on the Mechanical Properties of a Novel Polymer-Infiltrated Ceramic-Network Zirconia Dental Restorative (Filling) Material

PubMed Central

Li, Weiyan

2018-01-01

Background Polymer-infiltrated ceramic-network (PICN) dental material is a new and practical development in orthodontics. Sintering is the process of forming a stable solid mass from a powder by heating without melting. The aim of this study was to evaluate the effects of sintering temperature on the mechanical properties of a PICN zirconia dental material. Material/Methods A dense zirconia ceramic and four PICN zirconia dental materials, with varying porosities, were sintered at three different temperatures; 12 PICN zirconia dental materials based on these porous ceramics were prepared, as well as a pure polymer. After the specimen preparation, flexural strength and elastic modulus values were measured using the three-point bending test, and fracture toughness were determined by the single-edge notched beam (SENB) method. The Vickers hardness test method was used with an indentation strength (IS) test. Scanning electron microscopy (SEM) was used to examine the microstructure of the ceramic surface and the fracture surface. Results Mechanical properties of the PICN dental materials, including flexural strength, elastic modulus, fracture toughness, and hardness, were more similar to the properties of natural teeth when compared with traditional dental ceramic materials, and were affected by the density and sintering temperature. SEM showed that the porous ceramic network became cohesive and that the length of cracks in the PICN dental material was reduced. Conclusions PICN zirconia dental materials were characterized by similar mechanical properties to natural dental tissues, but further studies are required continue to improve the similarities with natural human enamel and dentin. PMID:29746449

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).

Processing of uranium dioxide nuclear fuel pellets using spark plasma sintering

NASA Astrophysics Data System (ADS)

Ge, Lihao

Uranium dioxide (UO2), one of the most common nuclear fuels, has been applied in most of the nuclear plant these days for electricity generation. The main objective of this research is to introduce a novel method for UO 2 processing using spark plasma sintering technique (SPS). Firstly, an investigation into the influence of processing parameters on densification of UO2 powder during SPS is presented. A broad range of sintering temperatures, hold time and heating rates have been systematically varied to investigate their influence on the sintered pellet densification process. The results revealed that up to 96% theoretical density (TD) pellets can be obtained at a sintering temperature of 1050 °C for 30s hold time and a total run time of only 10 minutes. A systematic study is performed by varying the sintering temperature between 750°C to 1450°C and hold time between 0.5 min to 20 min to obtain UO2 pellets with a range of densities and grain sizes. The microstructure development in terms of grain size, density and porosity distribution is investigated. The Oxygen/Uranium (O/U) ratio of the resulting pellets is found to decrease after SPS. The mechanical and thermal properties of UO2 are evaluated. For comparable density and grain size, Vickers hardness and Young's modulus are in agreement with the literature value. The thermal conductivity of UO2 increases with the density but the grain size in the investigated range has no significant influence. Overall, the mechanical and thermal properties of UO2 are comparable with the one made using conventional sintering methods. Lastly, the influence of chromium dioxide (Cr2O3) and zirconium diboride (ZrB2) on the grain size of doped UO 2 fuel pellet is performed to investigate the feasibility of producing large-grain-size nuclear fuel using SPS. The benefits of using SPS over the conventional sintering of UO2 are summarized. The future work of designing macro-porous UO2 pellet and thorium dioxide (ThO 2) cored UO2 pellet is also proposed.

Sintering of beta-type alumina bodies using alpha-alumina encapsulation

DOEpatents

McEntire, Bryan J.; Virkar, Anil V.

1981-01-01

A method of sintering a shaped green, beta-type alumina body comprising: (A) inserting said body into an open chamber prepared by exposing the interior surface of a container consisting essentially of at least about 50 weight percent of alpha-alumina and a remainder of other refractory material to a sodium oxide or sodium oxide producing environment; (B) sealing the chamber; and heating the chamber with the shaped body encapsulated therein to a temperature and for a time necessary to sinter said body to the desired density. The encapsulation chamber prepared as described above is also claimed.

Raman analysis of non stoichiometric Ni1-δO

NASA Astrophysics Data System (ADS)

Dubey, Paras; Choudhary, K. K.; Kaurav, Netram

2018-04-01

Thermal decomposition method was used to synthesize non-stoichiometric nickel oxide at different sintering temperatures upto 1100 °C. The structure of synthesized compounds were analyzed by X ray diffraction analysis (XRD) and magnetic ordering was studied with the help of Raman scattering spectroscopy for the samples sintered at different temperature. It was found that due to change in sintering temperature the stoichiometry of the sample changes and hence intensity of two magnon band changes. These results were interpreted as the decomposition temperature increases, which heals the defects present in the non-stoichiometric nickel oxide and antiferromagnetic spin correlation changes accordingly.

Method and apparatus for radio frequency ceramic sintering

DOEpatents

Hoffman, Daniel J.; Kimrey, Jr., Harold D.

1993-01-01

Radio frequency energy is used to sinter ceramic materials. A coaxial waveguide resonator produces a TEM mode wave which generates a high field capacitive region in which a sample of the ceramic material is located. Frequency of the power source is kept in the range of radio frequency, and preferably between 60-80 MHz. An alternative embodiment provides a tunable radio frequency circuit which includes a series input capacitor and a parallel capacitor, with the sintered ceramic connected by an inductive lead. This arrangement permits matching of impedance over a wide range of dielectric constants, ceramic volumes, and loss tangents.

Method and apparatus for radio frequency ceramic sintering

DOEpatents

Hoffman, D.J.; Kimrey, H.D. Jr.

1993-11-30

Radio frequency energy is used to sinter ceramic materials. A coaxial waveguide resonator produces a TEM mode wave which generates a high field capacitive region in which a sample of the ceramic material is located. Frequency of the power source is kept in the range of radio frequency, and preferably between 60-80 MHz. An alternative embodiment provides a tunable radio frequency circuit which includes a series input capacitor and a parallel capacitor, with the sintered ceramic connected by an inductive lead. This arrangement permits matching of impedance over a wide range of dielectric constants, ceramic volumes, and loss tangents. 6 figures.

Freeze drying vs microwave drying-methods for synthesis of sinteractive thoria powders

NASA Astrophysics Data System (ADS)

Annie, D.; Chandramouli, V.; Anthonysamy, S.; Ghosh, Chanchal; Divakar, R.

2017-02-01

Thoria powders were synthesized by oxalate precipitation from an aqueous solution of the nitrate. The filtered precipitates were freeze dried or microwave dried before being calcined at 1073 K. The thoria powders obtained were characterized for crystallite size, specific surface area, bulk density, particle size distribution and residual carbon. Microstructure of the product was studied using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Sinterability of the synthesized powders was studied by measuring the density of the sintered compacts. Powders that can be consolidated and sintered to densities ∼96% theoretical density (TD) at 1773 K were obtained.

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.

Effects of in situ synthesized mullite whisker on mechanical properties of Al2O3-SiC composite by microwave sintering

NASA Astrophysics Data System (ADS)

Dang, Xudan; Wei, Meng; Fan, Bingbing; Guan, Keke; Zhang, Rui; Long, Weimin; Zhang, Hongsong

2017-06-01

In situ synthesis of mullite whisker was introduced to Al2O3-SiC composite by microwave sintering. The effects of sintering parameters (sintering temperature, holding time and SiC particle size) on thermal shock resistance of Al2O3-SiC composite were also studied in this paper. Original SiC particles coated with SiO2 by a sol-gel method were reacted with Al2O3 particles, resulting in the in situ growth of mullite. The phase composition was identified by x-ray diffraction (XRD). The bridging of mullite whisker between Al2O3 and SiC particles was observed by scanning electron microscopy (SEM) analysis. The thermal shock resistance of samples was investigated through the combination of water quenching and three-point bending methods. The results show that the thermal shock resistance of Al2O3-SiC composite with mullite whisker reinforced remarkably, indicating better mechanical properties than the Al2O3-SiC composite without mullite whisker. Finally, the optimum process parameters (the sintering temperature of 1500 °C, the holding time of 30 min, and the SiC particle size of 5 µm) for toughening Al2O3-SiC composite by in situ synthesized mullite whisker were obtained.

The Oxidation Rate of SiC in High Pressure Water Vapor Environments

NASA Technical Reports Server (NTRS)

Opila, Elizabeth J.; Robinson, R. Craig

1999-01-01

CVD SiC and sintered alpha-SiC samples were exposed at 1316 C in a high pressure burner rig at total pressures of 5.7, 15, and 25 atm for times up to 100h. Variations in sample emittance for the first nine hours of exposure were used to determine the thickness of the silica scale as a function of time. After accounting for volatility of silica in water vapor, the parabolic rate constants for Sic in water vapor pressures of 0.7, 1.8 and 3.1 atm were determined. The dependence of the parabolic rate constant on the water vapor pressure yielded a power law exponent of one. Silica growth on Sic is therefore limited by transport of molecular water vapor through the silica scale.

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

DOE PAGES

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

2017-03-10

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

Vitrification of radioactive contaminated soil by means of microwave energy

NASA Astrophysics Data System (ADS)

Yuan, Xun; Qing, Qi; Zhang, Shuai; Lu, Xirui

2017-03-01

Simulated radioactive contaminated soil was successfully vitrified by microwave sintering technology and the solidified body were systematically studied by Raman, XRD and SEM-EDX. The Raman results show that the solidified body transformed to amorphous structure better at higher temperature (1200 °C). The XRD results show that the metamictization has been significantly enhanced by the prolonged holding time at 1200 °C by microwave sintering, while by conventional sintering technology other crystal diffraction peaks, besides of silica at 2θ = 27.830°, still exist after being treated at 1200 °C for much longer time. The SEM-EDX discloses the micro-morphology of the sample and the uniform distribution of Nd element. All the results show that microwave technology performs vitrification better than the conventional sintering method in solidifying radioactive contaminated soil.

IMPROVEMENTS IN OR RELATING TO THE PRODUCTION OF SINTERED URANIUM DIOXIDE

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

Russell, L.E.; Harrison, J.D.L.; Brett, N.H.

A method is described for producing a dense sintered body of uranium dioxide or a mixture thereof with plutonium dioxide. Compacted uranium dioxide or a compacted uranium dioxide-plutonium dioxide mixture is heated to at least 1300 deg C in an atmosphere of carbon dioxide or carbon dioxide mixed with carbon monoxide. (R.J.S.)

Studies of reaction geometry in oxidation and reduction of the alkaline silver electrode

NASA Technical Reports Server (NTRS)

Butler, E. A.; Blackham, A. U.

1971-01-01

Two methods of surface area estimations of sintered silver electrodes have given roughness factors of 58 and 81. One method is based on constant current oxidation, the other is based on potentiostatic oxidation. Examination of both wire and sintered silver electrodes via scanning electron microscopy at various stages of oxidation have shown that important structural features are mounds of oxide. In potentiostatic oxidations these appear to form on sites instantaneously nucleated while in constant current oxidations progressive nucleation is indicated.

High temperature strain gages

NASA Technical Reports Server (NTRS)

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

2011-01-01

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

Positron annihilation studies of zirconia doped with metal cations of different valence

NASA Astrophysics Data System (ADS)

Prochazka, I.; Cizek, J.; Melikhova, O.; Konstantinova, T. E.; Danilenko, I. A.; Yashchishyn, I. A.; Anwand, W.; Brauer, G.

2013-06-01

New results obtained by applying positron annihilation spectroscopy to the investigation of zirconia-based nanomaterials doped with metal cations of different valence are reported. The slow-positron implantation spectroscopy combined with Doppler broadening measurements was employed to study the sintering of pressure-compacted nanopowders of tetragonal yttria-stabilised zirconia (t-YSZ) and t-YSZ with chromia additive. Positronium (Ps) formation in t-YSZ was proven by detecting 3γ-annihilations of ortho-Ps and was found to gradually decrease with increasing sintering temperature. A subsurface layer with enhanced 3γ-annihilations, compared to the deeper regions, could be identified. Addition of chromia was found to inhibit Ps formation. In addition, first results of positron lifetime measurements on nanopowders of zirconia phase-stabilised with MgO and CeO2 are presented.

WELDING PROCESS

DOEpatents

Zambrow, J.; Hausner, H.

1957-09-24

A method of joining metal parts for the preparation of relatively long, thin fuel element cores of uranium or alloys thereof for nuclear reactors is described. The process includes the steps of cleaning the surfaces to be jointed, placing the sunfaces together, and providing between and in contact with them, a layer of a compound in finely divided form that is decomposable to metal by heat. The fuel element members are then heated at the contact zone and maintained under pressure during the heating to decompose the compound to metal and sinter the members and reduced metal together producing a weld. The preferred class of decomposable compounds are the metal hydrides such as uranium hydride, which release hydrogen thus providing a reducing atmosphere in the vicinity of the welding operation.

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.

Porous metals from sintering of nanoparticles

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

Cappillino, Patrick J.; Robinson, David B.

A method including encapsulating or capping metallic nanoparticles by a dendrimer or a polymer with binding sites for metal particless or metal ions dispersed in a fluid; modifying the fluid to disrupt the interaction of the dendrimer or polymer with the particles; and subsequently or concomitantly sintering or partially consolidating the zero valent metal. A method including introducing a first metal salt and a second metal salt into a dendrimer or a polymer with binding sites for metals or metal ions; reducing a metal ion of the first metal salt to a zero valent first metal and a metal ionmore » of the second metal salt to a zero valend second metal; disrupting an interaction between the dendrimer or the polymer and the first metal and the second metal; and sintering or partially consolidating the first metal and the second metal.« less

Influence of temperature and aging time on HA synthesized by the hydrothermal method.

PubMed

Kothapalli, C R; Wei, M; Legeros, R Z; Shaw, M T

2005-05-01

The influence of temperature and aging time on the morphology and mechanical properties of nano-sized hydroxyapatite (HA) synthesized by a hydrothermal method is reported here. The pre-mixed reactants were poured into a stirred autoclave and reacted at temperatures between 25-250 degrees C for 2-10 h. HA powders thus obtained were examined using X-ray diffraction (XRD), high-resolution field emission scanning electron microscopy (FESEM) and a particle size analyzer. It was found that the aspect ratio of the particles increased with the reaction temperature. The length of the HA particles increased with the reaction temperature below 170 degrees C, but it decreased when the temperature was raised above 170 degrees C. The agglomerates of HA particles were formed during synthesis, and their sizes were strongly dependent on reaction temperatures. As the reaction temperature increased, the agglomerate size decreased (p = 0.008). The density of the discs pressed from these samples reached 85-90% of the theoretical density after sintering at 1200 degrees C for 1 h. No decomposition to other calcium phosphates was detected at this sintering temperature. A correlation existed (p = 0.05) between the agglomerate sizes of HA particles synthesized at various conditions and their sintered densities. With the increase of the agglomerate size, the sintered density of the HA compact decreased. It was found that both the sintered density and flexural strength increased with increasing aging time and reaction temperature. A maximum flexural strength of 78 MPa was observed for the samples synthesized at 170 degrees C for 5 h with the predicted average at these conditions being 65 MPa. These samples attained an average sintered density of 88%.

Development of high Tc (greater than 110K) Bi, Tl and Y-based materials as superconducting circuit elements

NASA Technical Reports Server (NTRS)

Haertling, Gene H.; Lee, Burtrand; Grabert, Gregory; Gilmour, Phillip

1991-01-01

This report is presented in two parts. Part 1 deals primarily with Bi-based materials and a small amount of work on a Y-based composition while Part 2 covers work on Tl-based materials. In Part 1, a reliable and reproducible process for producing bulk bismuth-based superconductors has been developed. It is noted however, that a percentage of the tapecast material experiences curling and fracturing after a 30 hour sintering period and is thus in need of further examination. The Bi-Sr-Ca-Cu-O (BSCCO) material has been characterized by critical temperature data, X-ray diffraction data, and surface morphology. In the case of T sub c, it is not critical to anneal the material. It appears that the BSCCO material has the possibility of producing a better grounding strap than that of the 123 material. Attempts to reproduce near room temperature superconductors in the Y-Ba-Cu-O system were unsuccessful. In Part 2, several methods of processing the high temperature superconductor Tl2Ba2Ca2Cu3O10 were investigated; i.e., different precursor compositions were sintered at various sintering times and temperatures. The highest superconductig temperature was found to be 117.8K when fired at 900 C for three hours. Higher sintering temperatures produced a melted sample which was nonsuperconducting at liquid nitrogen temperature. Also, a preliminary study found Li2O substitutions for copper appeared to increase the transition temperature and create fluxing action upon sintering. It was suggested that lower sintering temperatures might be obtained with lithium additions to produce reliable Tl2Ba2Ca2Cu3O10 processing methods.

Integrated-fin gasket for palm cubic-anvil high pressure apparatus

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

Cheng, J.-G.; Beijing National Laboratory for Condensed Matter Physics and Institute of Physics, Chinese Academy of Sciences, Beijing 100190; Matsubayashi, K.

2014-09-15

We described an integrated-fin gasket technique for the palm cubic-anvil apparatus specialized for the high-pressure and low-temperature measurements. By using such a gasket made from the semi-sintered MgO ceramics and the tungsten-carbide anvils of 2.5 mm square top, we successfully generate pressures over 16 GPa at both room and cryogenic temperatures down to 0.5 K. We observed a pressure self-increment for this specific configuration and further characterized the thermally induced pressure variation by monitoring the antiferromagnetic transition temperature of chromium up to 12 GPa. In addition to enlarge the pressure capacity, such a modified gasket also improves greatly the survivingmore » rate of electrical leads hanging the sample inside a Teflon capsule filled with the liquid pressure-transmitting medium. These improvements should be attributed to the reduced extrusion of gasket materials during the initial compression.« less

Controlling Vapor Pressure In Hanging-Drop Crystallization

NASA Technical Reports Server (NTRS)

Carter, Daniel C.; Smith, Robbie

1988-01-01

Rate of evaporation adjusted to produce larger crystals. Device helps to control vapor pressure of water and other solvents in vicinity of hanging drop of solution containing dissolved enzyme protein. Well of porous frit (sintered glass) holds solution in proximity to drop of solution containing protein or enzyme. Vapor from solution in frit controls evaporation of solvent from drop to control precipitation of protein or enzyme. With device, rate of nucleation limited to decrease number and increase size (and perhaps quality) of crystals - large crystals of higher quality needed for x-ray diffraction studies of macromolecules.

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.

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

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.

[Studies on sintering of dental porcelain. (Part 1) Binary system sintering of alumina and low fusing frit (author's transl)].

PubMed

Kuwayama, N; Kon, M

1981-04-01

Dental porcelains were made from frit and glass powder with electro fused alumina powder addition in the range from 20 to 60 wt% using sintering method at the temperature from 500 degree C to 1 000 degree C, and the effects of alumina content and firing temperature on firing processes of sintered composite were investigated. Shrinkage curves of the powder compacts varied with kind of frit and content of alumina. Particulary, powder compact with alumina addition in the range from 50 to 55% was found to have a remarkable influence for extention of firing temperature range. The densification of the powder compacts was considered to be accelerated by the dissolution of a small a mount of alumina particle into the frit and glass above 900 degree C. Expansion coefficient value of sintered composite of alumina and Pyrex glass powder gradually increased with increase of alumina content. Inversely, expansion coefficient of soda-lime-silica glass showed the minimum value at 40 wt% alumina content and then had a tendency of slight increases with increase of alumina content.

Development of 2024 AA-Yttrium composites by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Vidyasagar, CH S.; Karunakar, D. B.

2018-04-01

The method of fabrication of MMNCs is quite a challenge, which includes advanced processing techniques like Spark Plasma Sintering (SPS), etc. The objective of the present work is to fabricate aluminium based MMNCs with the addition of small amounts of yttrium using Spark Plasma Sintering and to evaluate their mechanical and microstructure properties. Samples of 2024 AA with yttrium ranging from 0.1% to 0.5 wt% are fabricated by Spark Plasma Sintering (SPS). Hardness of the samples is determined using Vickers hardness testing machine. The metallurgical characterization of the samples is evaluated by Optical Microscopy (OM), Field Emission Scanning Electron Microscopy (FE-SEM). Unreinforced 2024 AA sample is also fabricated as a benchmark to compare its properties with those of the composite developed. It is found that the yttrium addition increases the above mentioned properties by altering the precipitation kinetics and intermetallic formation to some extent and then decreases gradually when yttrium wt% increases beyond 0.3 wt%. High density (˂ 99.75) is achieved in the samples and highest hardness achieved is 114 Hv, fabricated by spark plasma sintering and uniform distribution of yttrium is observed.

Preparation of micro-porous bioceramic containing silicon-substituted hydroxyapatite and beta-tricalcium phosphate.

PubMed

Fuh, Lih-Jyh; Huang, Ya-Jing; Chen, Wen-Cheng; Lin, Dan-Jae

2017-06-01

Dimensional instability caused by sintering shrinkage is an inevitable drawback for conventional processing of hydroxyapatite (HA). A new preparation method for biphasic calcium phosphates was developed to increase micro pores and biodegradation without significant dimensional change. Powder pressed HA discs, under 100MPa, were immersed in a colloidal mixture of tetraethoxysilane (TEOS) and ammonium hydroxide for 10min, followed by drying, and then were sintered at 900°C, 1050°C, and 1200°C, respectively. Comparing with pure HA discs, the newly prepared product sintered up to 1200°C contained silicon substituted HA, beta-tricalcium phosphate, and calcium silicate with better micro-porosity, high specific surface area, less sintering shrinkage and the strength maintained. The cytocompatibility test demonstrated a better viability for D1 mice stem cells cultured on TEOS treated HA for 14days compared to the pure HA. This simple TEOS sol-gel pretreatment has the potential to be applied to any existing manufacturing process of HA scaffold for better control of sintering shrinkage, create micropores, and increase biodegradation. Copyright © 2017 Elsevier B.V. All rights reserved.

Sinter of uniform, predictable, blemish-free nickel plaque for large aerospace nickel cadmium cells

NASA Technical Reports Server (NTRS)

Seiger, H. N.

1975-01-01

A series of nickel slurry compositions were tested. Important slurry parameters were found to be the nature of the binder, a pore former and the method of mixing. A slow roll mixing which is non-turbulent successfully eliminated entrapped air so that bubbles and pockets were avoided in the sinter. A slurry applicator was developed which enabled an equal quantity of slurry to be applied to both sides of the grid. Sintering in a furnace having a graded atmosphere characteristic, ranging from oxidizing to strongly reducing, improved adhesion of porous sinter to grid and resulted in a uniform welding of nickel particles to each other throughout the plaque. Sintering was carried out in a horizontal furnace having three heating zones and 16 heating control circuits. Tests used for plaque evaluation include (1) appearance, (2) grid location and adhesion, (3) mechanical strength, (4) thickness, (5) weight per unit area, (6) void volume per unit area, (7) surface area and (8) electrical resistance. Plaque material was impregnated using Heliotek proprietary processes and 100 AH cells were fabricated.

Effect of fiber addition on slow crack growth of a dental porcelain.

PubMed

de Araújo, Maico Dutra; Miranda, Ranulfo Benedito de Paula; Fredericci, Catia; Yoshimura, Humberto Naoyuki; Cesar, Paulo Francisco

2015-04-01

To evaluate the effect of the processing method (conventional sintering, S, and heat-pressing, HP) and addition of potassium titanate fibers, PTF, on the microstructure, mechanical properties (flexural strength, σf, and Weibull parameters, m and σ5%), slow crack growth parameters n (stress corrosion susceptibility coefficient), and optical properties (translucency parameter, TP, and opalescence index, OI) of a feldsphatic dental porcelain. Disks (n = 240, Ø12 × 1 mm) of porcelain (Vintage-Halo, Shofu) were produced using S and HP methods with and without addition of 10 wt% (conventional sintering) or 5 wt% (heat-pressing) of PTF. For the S method, porcelain was sintered in a conventional furnace. In the HP technique, refractory molds were produced by lost wax technique. The porcelain slurry was dry-pressed (3t/30s) to form a cylinder with 12 mm (diameter) and 20mm (height), which was heat-pressed for 5 min/3.5 bar into the mold. Specimens were tested for biaxial flexural strength in artificial saliva at 37°C. Weibull analysis was used to determine m and σ5%. Slow crack growth (SCG) parameters were determined by the dynamic fatigue test, and specimens were tested in biaxial flexure at five stress rates: 10(-2), 10(-1), 10(0), 10(1) and 10(2)MPa/s (n=10), immersed in artificial saliva at 37°C. Parameter n was calculated and statistically analyzed according to ASTM F394-78. Optical properties were determined in a spectrophotometer in the diffuse reflectance mode. The highest n value was obtained by the combination of heat-pressing with fiber addition (37.1) and this value was significantly higher than those obtained by both sintered groups (26.2 for control group and 27.7 for sintered with fiber). Although heat-pressing alone also resulted in higher n values compared to the sintered groups, there were no significant differences among them. Fiber addition had no effect on mechanical strength, but it resulted in decreased TP values and increased OI values for both processing methods. Heat-pressing alone was able to reduce the porosity level of the porcelain. Addition of PTF combined with heat-pressing can reduce strength degradation of a dental porcelain compared to sintered materials with or without fibers. Heat-pressing (HP) alone should be considered as a good alternative for clinical cases where high translucency is required. Copyright © 2014 Elsevier Ltd. All rights reserved.

Low temperature synthesis and sintering of d-UO2 nanoparticles.

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

Nenoff, Tina Maria; Ferreira, Summer Rhodes; Robinson, David B.

We report on the novel room temperature method of synthesizing advanced nuclear fuels; a method that virtually eliminates any volatility of components. This process uses radiolysis to form stable nanoparticle (NP) nuclear transuranic (TRU) fuel surrogates and in-situ heated stage TEM to sinter the NPs. The radiolysis is performed at Sandia's Gamma Irradiation Facility (GIF) 60Co source (3 x 10{sup 6} rad/hr). Using this method, sufficient quantities of fuels for research purposes can be produced for accelerated advanced nuclear fuel development. We are focused on both metallic and oxide alloy nanoparticles of varying compositions, in particular d-U, d-U/La alloys andmore » d-UO2 NPs. We present detailed descriptions of the synthesis procedures, the characterization of the NPs, the sintering of the NPs, and their stability with temperature. We have employed UV-vis, HRTEM, HAADF-STEM imaging, single particle EDX and EFTEM mapping characterization techniques to confirm the composition and alloying of these NPs.« less