Nondestructive evaluation of structural ceramics by photoacoustic microscopy

NASA Technical Reports Server (NTRS)

Khandelwal, Pramod K.

1987-01-01

A photoacoustic microscopy (PAM) digital imaging system was developed and utilized to characterize silicon nitride material at the various stages of the ceramic fabrication process. Correlation studies revealed that photoacoustic microscopy detected failure initiating defects in substantially more specimens than microradiography and ultrasonic techniques. Photoacoustic microscopy detected 10 to 100 micron size surface and subsurface pores and inclusions, respectively, up to 80 microns below the interrogating surface in machined sintered silicon nitride. Microradiography detected 50 micron diameter fracture controlling pores and inclusions. Subsurface holes were detected up to a depth of 570 microns and 1.00 mm in sintered silicon nitride and silicon carbide, respectively. Seeded voids of 20 to 30 micron diameters at the surface and 50 microns below the interrogating surface were detected by photoacoustic microscopy and microradiography with 1 percent X-ray thickness sensitivity. Tight surface cracks of 96 micron length x 48 micron depth were detected by photoacoustic microscopy. PAM volatilized and removed material in the green state which resulted in linear shallow microcracks after sintering. This significantly limits the use of PAM as an in-process NDE technique.

Characterization and sintering of MoO{sub 3} prepared by thermal decomposition of hexaammonium heptamolybdate tetrahydrate

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

Honma, K.; Hirota, K.; Yamaguchi, O.

1997-01-01

MoO{sub 3} powders with plate particles have been prepared by heating hexaammonium heptamolybdate tetrahydrate ((NH{sub 4}){sub 6}Mo{sub 7}O{sub 24} {center_dot} 4H{sub 2}O) for 1 h at 650 C. Densification has been performed by hot pressing for 2 h at 630 C and 30 MPa. Grain-oriented MoO{sub 3} ceramics (>98% of theoretical) are fabricated, in which the <010> axis is parallel to the hot pressing direction. Their electrical conductivities have been measured in the temperature range of 100 to 600 C. Sintered MoO{sub 3} is a ceramic semiconductor. Activation energies are determined to be 0.49 and 0.76 eV for initial andmore » final stages, respectively.« less

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.

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.

Selective Laser Sintering of Nano Al2O3 Infused Polyamide

PubMed Central

Warnakula, Anthony; Singamneni, Sarat

2017-01-01

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

40 CFR 63.7783 - When do I have to comply with this subpart?

Code of Federal Regulations, 2014 CFR

2014-07-01

... sinter cooler at an existing sinter plant. (b) If you have a new affected source and its initial startup... source and its initial startup date is after May 20, 2003, you must comply with each emission limitation and operation and maintenance requirement in this subpart that applies to you upon initial startup. (d...

40 CFR 63.7783 - When do I have to comply with this subpart?

Code of Federal Regulations, 2010 CFR

2010-07-01

... sinter cooler at an existing sinter plant. (b) If you have a new affected source and its initial startup... source and its initial startup date is after May 20, 2003, you must comply with each emission limitation and operation and maintenance requirement in this subpart that applies to you upon initial startup. (d...

40 CFR 63.7783 - When do I have to comply with this subpart?

Code of Federal Regulations, 2011 CFR

2011-07-01

... sinter cooler at an existing sinter plant. (b) If you have a new affected source and its initial startup... source and its initial startup date is after May 20, 2003, you must comply with each emission limitation and operation and maintenance requirement in this subpart that applies to you upon initial startup. (d...

Influence of metallic additives on manganese ferrites sintering

NASA Astrophysics Data System (ADS)

Shevelev, S. A.; Luchnikov, P. A.; Yarullina, A. R.

2018-01-01

Influence of cuprum nanopowder additive received by electric explosion on the process of manganese ferrites MgFe2O4 consolidating at thermal sintering was researched by dilatometry method. Cuprum nanopowder at a rate of 5 mass % was added into the original commercial-grade powder of manganese ferrite MgFe2O4. Powder mixture was numerously blended with screening for better blending before pressing. Powder compacts were formed by cold one-axle static pressing. It was proved that introduction of cuprum additive caused shrinkage increase at final heating stage. There was abnormal compact enlarging at sintering in the air at isothermal stage; the specified process was not observed in vacuum. This difference can be explained by changes in conditions of gaseous discharge from volume of pores.

Evolving microstructure, magnetic properties and phase transition in a mechanically alloyed Ni0.5Zn0.5Fe2O4 single sample

NASA Astrophysics Data System (ADS)

Ismail, Ismayadi; Hashim, Mansor; Kanagesan, Samikannu; Ibrahim, Idza Riati; Nazlan, Rodziah; Wan Ab Rahman, Wan Norailiana; Abdullah, Nor Hapishah; Mohd Idris, Fadzidah; Bahmanrokh, Ghazaleh; Shafie, Mohd Shamsul Ezzad; Manap, Masni

2014-02-01

We report on an investigation to unravel the dependence of magnetic properties on microstructure while they evolve in parallel under the influence of sintering temperature of a single sample of Ni0.5Zn0.5Fe2O4 synthesized via mechanical alloying. A single sample, instead of the normally practiced approach of using multiple samples, was sintered at various sintering temperatures from 500 °C to 1400 °C. The morphology of the samples was studied by means of scanning electron microscopy (SEM) equipped with EDX; density measurement was conducted using the Archimedes principle; and hysteresis measurement was carried out using a B-H hysteresisgraph system. XRD data showed that the first appearance of a single phase was at 800 °C and an amorphous phase was traced at lower sintering temperatures. We correlated the microstructure and the magnetic properties and showed that the important grain-size threshold for the appearance of significant ordered magnetism (mainly ferromagnetism) was about ≥0.3 µm. We found that there were three stages of magnetic phase evolution produced via the sintering process with increasing temperatures. The first stage was dominated by paramagnetic states with some superparamagnetic behavior; the second stage was influenced by moderately ferromagnetic states and some paramagnetic states; and the third stage consisted of strongly ferromagnetic states with negligible paramagnetic states. We found that three factors sensitively influenced the sample's content of ordered magnetism—the ferrite-phase crystallinity degree, the number of grains above the critical grain size and the number of large enough grains for domain wall accommodation.

Effects of particle packing on the sintered microstructure

NASA Astrophysics Data System (ADS)

Barringer, E. A.; Bowen, H. K.

1988-04-01

The sintering process is shown to be critically dependent on particle-packing density and porosity uniformity. Sintering experiments were conducted on compacts consisting of monodisperse, spherical TiO2 particles. Densification kinetics and microstructure evolution for two initial packing densities, 55% and 69% of theoretical, were investigated. The lower-density compacts sintered rapidly to theoretical density, yet improved particle-packing density and uniformity significantly enhanced densification.

Effects of Sintering and Extrusion on the Microstructures and Mechanical Properties of a SiC/Al-Cu Composite

NASA Astrophysics Data System (ADS)

Sun, Chao; Shen, Rujuan; Song, Min

2012-03-01

This article studied the effects of sintering and extrusion on the microstructures and mechanical properties of SiC particle reinforced Al-Cu alloy composite produced by powder metallurgy method. It has been shown that both extrusion and increasing sintering temperature can significantly improve the strength and plasticity of the composite. The extrusion and increase of the sintering temperature can break up the oxide coating on the matrix powder surfaces, decrease the number of pores, accelerate the elements' diffusion and increase the density and particle interfacial bonding strength, thus significantly improve the mechanical properties of the composite. The strength and hardness of the composite increase and the elongation decreases with increasing the aging time at under-aged stage, while the strength and hardness start to decrease and the elongation starts to increase with increasing the aging time at over-aged stage due to the formation and growth of the secondary strengthening precipitates in the Al-Cu matrix.

Apparatus and method for direct measurement of coal ash sintering and fusion properties at elevated temperatures and pressures

DOEpatents

Khan, M. Rashid

1990-01-01

A high-pressure microdilatometer is provided for measuring the sintering and fusion properties of various coal ashes under the influence of elevated pressures and temperatures in various atmospheres. Electrical resistivity measurements across a sample of coal ash provide a measurement of the onset of the sintering and fusion of the ash particulates while the contraction of the sample during sintering is measured with a linear variable displacement transducer for detecting the initiation of sintering. These measurements of sintering in coal ash at different pressures provide a mechanism by which deleterious problems due to the sintering and fusion of ash in various combustion systems can be minimized or obviated.

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

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

Walls, P

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

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.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

Spark plasma sintering and microstructural analysis of pure and Mo doped U3Si2 pellets

NASA Astrophysics Data System (ADS)

Lopes, Denise Adorno; Benarosch, Anna; Middleburgh, Simon; Johnson, Kyle D.

2017-12-01

U3Si2 has been considered as an alternative fuel for Light Water Reactors (LWRs) within the Accident Tolerant Fuels (ATF) initiative, begun after the Fukushima-Daiichi Nuclear accidents. Its main advantages are high thermal conductivity and high heavy metal density. Despite these benefits, U3Si2 presents an anisotropic crystallographic structure and low solubility of fission products, which can result in undesirable effects under irradiation conditions. In this paper, spark plasma sintering (SPS) of U3Si2 pellets is studied, with evaluation of the resulting microstructure. Additionally, exploiting the short sintering time in SPS, a molybdenum doped pellet was produced to investigate the early stages of the Mo-U3Si2 interaction, and analyze how this fission product is accommodated in the fuel matrix. The results show that pellets of U3Si2 with high density (>95% TD) can be obtained with SPS in the temperature range of 1200°C-1300 °C. Moreover, the short time employed in this technique was found to generate a unique microstructure for this fuel, composed mainly of closed nano-pores (<1 μm) and small average grain size (∼4.5 μm). The addition of Mo (1.5 at%) demonstrated no solubility of Mo in the U3Si2 matrix. The interaction of this fission product with the fuel matrix at 1200 °C formed, in the early stages, the stoichiometric U2Mo3Si4 ternary as well as precipitates of free uranium with small quantities of dissolved Si and Mo at the front of the reaction.

Sintering of polydisperse viscous droplets

NASA Astrophysics Data System (ADS)

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

2017-03-01

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

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.

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.

Fabrication of Natural Uranium UO 2 Disks (Phase II): Texas A&M Work for Others Summary Document

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

Gerczak, Tyler J.; Baldwin, Charles A.; Schmidlin, Joshua E.

The steps to fabricate natural UO 2 disks for an irradiation campaign led by Texas A&M University are outlined. The process was initiated with stoichiometry adjustment of parent, U 3O 8 powder. The next stage of sample preparation involved exploratory pellet pressing and sintering to achieve the desired natural UO 2 pellet densities. Ideal densities were achieved through the use of a bimodal powder size blend. The steps involved with disk fabrication are also presented, describing the coring and thinning process executed to achieve final dimensionality.

Computer simulation of low-temperature composites sintering processes for additive technologies

NASA Astrophysics Data System (ADS)

Tovpinets, A. O.; Leytsin, V. N.; Dmitrieva, M. A.

2017-12-01

This is impact research of mixture raw components characteristics on the low-temperature composites structure formation during the sintering process. The obtained results showed that the structure determination of initial compacts obtained after thermal destruction of the polymer binder lets quantify the concentrations of main components and the refractory crystalline product of thermal destruction. Accounting for the distribution of thermal destruction refractory product allows us to refine the forecast of thermal stresses in the matrix of sintered composite. The presented results can be considered as a basis for optimization of initial compositions of multilayer low-temperature composites obtained by additive technologies.

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.

40 CFR 63.7825 - How do I demonstrate initial compliance with the emission limitations that apply to me?

Code of Federal Regulations, 2014 CFR

2014-07-01

...-day rolling average of the volatile organic compound emissions from the sinter plant windbox exhaust... during the performance test in accordance with § 63.7824(b). (b) For each existing or new sinter plant... accordance with § 63.7824(d) is no more than 0.02 percent. For each existing or new sinter plant subject to...

40 CFR 63.7825 - How do I demonstrate initial compliance with the emission limitations that apply to me?

Code of Federal Regulations, 2012 CFR

2012-07-01

...-day rolling average of the volatile organic compound emissions from the sinter plant windbox exhaust... during the performance test in accordance with § 63.7824(b). (b) For each existing or new sinter plant... accordance with § 63.7824(d) is no more than 0.02 percent. For each existing or new sinter plant subject to...

40 CFR 63.7825 - How do I demonstrate initial compliance with the emission limitations that apply to me?

Code of Federal Regulations, 2013 CFR

2013-07-01

...-day rolling average of the volatile organic compound emissions from the sinter plant windbox exhaust... during the performance test in accordance with § 63.7824(b). (b) For each existing or new sinter plant... accordance with § 63.7824(d) is no more than 0.02 percent. For each existing or new sinter plant subject to...

Reduction of FeO contents in sinter under high bed operation

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

Fujii, K.; Hazama, K.; Hoshikuma, Y.

1996-12-31

High-bed operation (bed height more than 700 mm) is currently being carried out at the Kure No. 1 sintering plant. Before initiating this high-bed operation, the authors conducted sinter pot tests at various bed heights to investigate the effect of bed height on sintering. The following results were obtained from these pot tests: Heightening of the sinter bed increased yield at the upper layer, but at the lower layer, the yield reached a maximum value at a certain bed height. From observation of the sinter cakes, the reduction in yield is attributed to uneven burn caused by surplus heat atmore » the lower layers. Therefore, when high-bed operation is carried out, reduction of the burning energy (reduction of the FeO content in the sinter) is required. This high-bed operation with lower FeO content has enabled the company to reduce fuel consumption and SiO{sub 2} content, while maintaining high yield and high sinter quality.« less

Improved silicon carbide for advanced heat engines

NASA Technical Reports Server (NTRS)

Whalen, Thomas J.; Mangels, J. A.

1986-01-01

The development of silicon carbide materials of high strength was initiated and components of complex shape and high reliability were formed. The approach was to adapt a beta-SiC powder and binder system to the injection molding process and to develop procedures and process parameters capable of providing a sintered silicon carbide material with improved properties. The initial effort was to characterize the baseline precursor materials, develop mixing and injection molding procedures for fabricating test bars, and characterize the properties of the sintered materials. Parallel studies of various mixing, dewaxing, and sintering procedures were performed in order to distinguish process routes for improving material properties. A total of 276 modulus-of-rupture (MOR) bars of the baseline material was molded, and 122 bars were fully processed to a sinter density of approximately 95 percent. Fluid mixing techniques were developed which significantly reduced flaw size and improved the strength of the material. Initial MOR tests indicated that strength of the fluid-mixed material exceeds the baseline property by more than 33 percent. the baseline property by more than 33 percent.

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.

Enhancement of thermal shock resistance of reaction sintered mullite–zirconia composites in the presence of lanthanum oxide

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

Kumar, P.; Nath, M.; Ghosh, A.

2015-03-15

Mullite–zirconia composites containing 20 wt.% zirconia were prepared by reaction sintering of zircon flour, sillimanite beach sand and calcined alumina. 0 to 8 mol% of La{sub 2}O{sub 3} with respect to zirconia was used as sintering aid. The effect of additive on the various physical, microstructures, mechanical and thermo-mechanical properties was studied. Quantitative phase analysis shows the change in tetragonal zirconia content with incorporation of lanthanum oxide. La{sub 2}O{sub 3} addition has significantly improved the thermal shock resistance of the samples. Samples without additive retained only 20% of initial flexural strength after 5 cycles, whereas samples containing 5 mol% La{submore » 2}O{sub 3} retained almost 78% of its initial flexural strength even after 15 thermal shock cycles. - Highlights: • Mullite–zirconia composites were prepared by reaction sintering route utilizing zircon and sillimanite beach sand. • Lanthanum oxide was used as sintering aid. • The presence of lanthanum oxide decreased the densification temperature. • Lanthanum oxide significantly improved the thermal shock resistance of the composites.« less

Exothermic low temperature sintering of Cu nanoparticles

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

Mittal, Jagjiwan; Lin, Kwang-Lung, E-mail: matkllin@mail.ncku.edu.tw

2015-11-15

Sintering of the Cu nanoparticle at low temperatures resulted in exothermic behavior after its initiation. The calorimetry study of the heating of a 20 nm copper nanoparticles agglomerate revealed the evolution of 41.17 J/g of heat between 170 °C and 270 °C. High resolution transmission electron microscopy (HRTEM) images indicated that the heat generation was accompanied by sintering. The surface energy of the 20 nm copper nanoparticles was estimated to be 1.23 × 10{sup 3} erg/cm{sup 2} based on the heat released during sintering. The in situ high resolution transmission electron microscope (HRTEM) investigation showed that vigorous sintering occurred betweenmore » 217 and 234 °C, which took place through the dislocation sintering mechanism. - Highlights: • Calorimetry showed exothermic behavior during heating of Cu nanoparticles between 170 and 270 °C. • Heat released due to the sintering of Cu nanoparticles was demonstrated by HRTEM. • Surface energy of 20 nm copper nanoparticles was estimated to be 1.23 × 10{sup 3} erg/cm{sup 2} during sintering. • Growth in crystallite sizes during sintering is disclosed by X-ray diffraction. • In situ HRTEM heating study showed occurrence of sintering through dislocation mechanism.« less

Angiogenesis after sintered bone implantation in rat parietal bone.

PubMed

Ohtsubo, S; Matsuda, M; Takekawa, M

2003-01-01

We studied the effect of bone substitutes on revascularization and the restart of blood supply after sintered bone implantation in comparison with synthetic hydroxyapatite implantation and fresh autogenous bone transplantation (control) in rat parietal bones. Methods for the study included the microvascular corrosion cast method and immunohistochemical techniques were also used. The revascularization of the control group was the same as that for usual wound healing in the observations of the microvascular corrosion casts. The sintered bone implantation group was quite similar to that of the control group. In the synthetic hydroxyapatite group, immature newly-formed blood vessels existed even on the 21st day after implantation and the physiological process of angiogenesis was interrupted. Immunohistochemically, vascular endothelial growth factor (VEGF), which activates angiogenesis, appeared at the early stages of both the control group and the sintered bone implantation group. VEGF reduced parallel with the appearance of the transforming growth factor factor-beta-1 (TGF-beta-1), which obstructs angiogenesis, and the angiogenesis passed gradually into the mature stage. In the hydroxyapatite implantation group, TGF-beta-1 appeared at the early stage of the implants. The appearance of VEGF lagged and it existed around the pores of hydroxyapatite even on the 21st day of the implantation. Proliferation and wandering of endothelial cells continued without any maturing of the vessels. These findings suggest that the structure and the components of the implant material affect angiogenesis after implantation as well as new bone formation.

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.

Data on the influence of cold isostatic pre-compaction on mechanical properties of polycrystalline nickel sintered using Spark Plasma Sintering.

PubMed

Dutel, Guy-Daniel; Langlois, Patrick; Tingaud, David; Vrel, Dominique; Dirras, Guy

2017-04-01

Data regarding bulk polycrystalline nickel samples obtained by powder metallurgy using Spark Plasma Sintering (SPS) are presented, with a special emphasis on the influence of a cold isostatic pre-compaction on the resulting morphologies and subsequent mechanical properties. Three types of initial powders are used, nanometric powders, micrometric powders and a mixture of the formers. For each type of powder, the SPS cycle has been optimized for the powders without pre-compaction and the same cycle has been used to also sinter pre-compacted powders.

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.

Verification of the Skorohod-Olevsky Viscous Sintering (SOVS) Model

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

Lester, Brian T.

2017-11-16

Sintering refers to a manufacturing process through which mechanically pressed bodies of ceramic (and sometimes metal) powders are heated to drive densification thereby removing the inherit porosity of green bodies. As the body densifies through the sintering process, the ensuing material flow leads to macroscopic deformations of the specimen and as such the final configuration differs form the initial. Therefore, as with any manufacturing step, there is substantial interest in understanding and being able to model the sintering process to predict deformation and residual stress. Efforts in this regard have been pursued for face seals, gear wheels, and consumer productsmore » like wash-basins. To understand the sintering process, a variety of modeling approaches have been pursued at different scales.« less

The effect of processing parameters and solid concentration on the mechanical and microstructural properties of freeze-casted macroporous hydroxyapatite scaffolds.

PubMed

Farhangdoust, S; Zamanian, A; Yasaei, M; Khorami, M

2013-01-01

The design and fabrication of macroporous hydroxyapatite scaffolds, which could overcome current bone tissue engineering limitations, have been considered in recent years. In the current study, controlled unidirectional freeze-casting at different cooling rates was investigated. In the first step, different slurries with initial hydroxyapatite concentrations of 7-37.5 vol.% were prepared. In the next step, different cooling rates from 2 to 14 °C/min were applied to synthesize the porous scaffold. Additionally, a sintering temperature of 1350 °C was chosen as an optimum temperature. Finally, the phase composition (by XRD), microstructure (by SEM), mechanical characteristics, and the porosity of sintered samples were assessed. The porosity of the sintered samples was in a range of 45-87% and the compressive strengths varied from 0.4 MPa to 60 MPa. The mechanical strength of the scaffolds increased as a function of initial concentration, cooling rate, and sintering temperature. With regards to mechanical strength and pore size, the samples with the initial concentration and the cooling rate of 15 vol.% and 5 °C/min, respectively, showed better results. Copyright © 2012 Elsevier B.V. All rights reserved.

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.

40 CFR 63.7820 - By what date must I conduct performance tests or other initial compliance demonstrations?

Code of Federal Regulations, 2013 CFR

2013-07-01

... sinter plant feedstock in § 63.7790(d)(1) or alternative limit for volatile organic compound emissions from the sinter plant windbox exhaust stream in § 63.7790(d)(2). You must conduct the performance tests...

40 CFR 63.7820 - By what date must I conduct performance tests or other initial compliance demonstrations?

Code of Federal Regulations, 2012 CFR

2012-07-01

... sinter plant feedstock in § 63.7790(d)(1) or alternative limit for volatile organic compound emissions from the sinter plant windbox exhaust stream in § 63.7790(d)(2). You must conduct the performance tests...

40 CFR 63.7820 - By what date must I conduct performance tests or other initial compliance demonstrations?

Code of Federal Regulations, 2014 CFR

2014-07-01

... sinter plant feedstock in § 63.7790(d)(1) or alternative limit for volatile organic compound emissions from the sinter plant windbox exhaust stream in § 63.7790(d)(2). You must conduct the performance tests...

40 CFR 63.7820 - By what date must I conduct performance tests or other initial compliance demonstrations?

Code of Federal Regulations, 2011 CFR

2011-07-01

... sinter plant feedstock in § 63.7790(d)(1) or alternative limit for volatile organic compound emissions from the sinter plant windbox exhaust stream in § 63.7790(d)(2). You must conduct the performance tests...

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.

SINTERING OF NASCENT CALCIUM OXIDE

EPA Science Inventory

The paper discusses the measurement of the sintering rate of CaO in a nitrogen atmosphere at temperatures of 700-1100 C. CaO prepared from ultrapure CaCO3 was compared with an impure CaO derived from limestone. Both materials yielded an initial surface area of 104 sq m/g. The rat...

Effect of Bed Temperature on the Laser Energy Required to Sinter Copper Nanoparticles

NASA Astrophysics Data System (ADS)

Roy, N. K.; Dibua, O. G.; Cullinan, M. A.

2018-03-01

Copper nanoparticles (NPs), due to their high electrical conductivity, low cost, and easy availability, provide an excellent alternative to other metal NPs such as gold, silver, and aluminum in applications ranging from direct printing of conductive patterns on metal and flexible substrates for printed electronics applications to making three-dimensional freeform structures for interconnect fabrication for chip-packaging applications. Lack of research on identification of optimum sintering parameters such as fluence/irradiance requirements for sintering of Cu NPs serves as the primary motivation for this study. This article focuses on the identification of a good sintering irradiance window for Cu NPs on an aluminum substrate using a continuous wave (CW) laser. The study also includes the comparison of CW laser sintering irradiance windows obtained with substrates at different initial temperatures. The irradiance requirements for sintering of Cu NPs with the substrate at 150-200°C were found to be 5-17 times smaller than the irradiance requirements for sintering with the substrate at room temperature. These findings were also compared against the results obtained with a nanosecond (ns) laser and a femtosecond (fs) laser.

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

NASA Astrophysics Data System (ADS)

Knight, Travis Warren

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

Effects of loading modes on densification efficiency of spark plasma sintering: sample study of zirconium carbide consolidation

NASA Astrophysics Data System (ADS)

Wei, Xialu; Maximenko, Andrey L.; Back, Christina; Izhvanov, Oleg; Olevsky, Eugene A.

2017-07-01

Theoretical studies on the densification kinetics of the new spark plasma sinter-forging (SPS-forging) consolidation technique and of the regular SPS have been carried out based on the continuum theory of sintering. Both modelling and verifying experimental results indicate that the loading modes play important roles in the densification efficiency of SPS of porous ZrC specimens. Compared to regular SPS, SPS-forging is shown to be able to enhance the densification more significantly during later sintering stages. The derived analytical constitutive equations are utilised to evaluate the high-temperature creep parameters of ZrC under SPS conditions. SPS-forging and regular SPS setups are combined to form a new SPS hybrid loading mode with the purpose of reducing shape irregularity in the SPS-forged specimens. Loading control is imposed to secure the geometry as well as the densification of ZrC specimens during hybrid SPS process.

Stability study of cermet-supported solid oxide fuel cells with bi-layered electrolyte

NASA Astrophysics Data System (ADS)

Zhang, Xinge; Gazzarri, Javier; Robertson, Mark; Decès-Petit, Cyrille; Kesler, Olivera

Performance and stability of five cermet-supported button-type solid oxide fuel cells featuring a bi-layered electrolyte (SSZ/SDC), an SSC cathode, and a Ni-SSZ anode, were analyzed using polarization curves, impedance spectroscopy, and post-mortem SEM observation. The cell performance degradation at 650 °C in H 2/air both with and without DC bias conditions was manifested primarily as an increase in polarization resistance, approximately at a rate of 2.3 mΩ cm 2 h -1 at OCV, suggesting a decrease in electrochemical kinetics as the main phenomenon responsible for the performance decay. In addition, the initial series resistance was about ten times higher than the calculated resistance corresponding to the electrolyte, reflecting a possible inter-reaction between the electrolyte layers that occurred during the sintering stage. In situ and ex situ sintered cathodes showed no obvious difference in cell performance or decay rate. The stability of the cells with and without electrical load was also investigated and no significant influence of DC bias was recorded. Based on the experimental results presented, we preliminarily attribute the performance degradation to electrochemical and microstructural degradation of the cathode.

Effects of size reduction on deformation, microstructure, and surface roughness of micro components for micro metal injection molding

NASA Astrophysics Data System (ADS)

Liu, Lin; Wang, Xin-da; Li, Xiang; Qi, Xiao-tong; Qu, Xuan-hui

2017-09-01

The fabrication of 17-4PH micro spool mandrils by micro metal injection molding was described here. The effects of size reduction on deformation, microstructure and surface roughness were studied by comparing a ϕ500 μm micro post and a ϕ1.7 mm cylinder after debinding and sintering. Experimental results show that slumping of the micro posts occurred due to a dramatic increase in outlet vapor pressure initiated at the thermal degradation onset temperature and the moment of gravity. Asymmetrical stress distribution within the micro component formed during the cooling stage may cause warping. Prior solvent debinding and adjustment in a thermal debinding scheme were useful for preventing the deformation of the micro components. Smaller grain size and higher micro hardness due to impeded grain growth were observed for the micro posts compared with the ϕ1.7 mm cylinder. Surface roughness increased with distance from the gate of the micro spool mandril due to melt front advancement during mold filling and the ensuing pressure distribution. At each position, surface roughness was dictated by injection molding and increased slightly after sintering.

Sinter-vein correlations at Buckskin Mountain, National district, Humboldt County, Nevada

USGS Publications Warehouse

Vikre, P.G.

2007-01-01

At Buckskin Mountain (elev 2,650 m, 8,743 ft), Humboldt County, Nevada, a hydrothermal system, imposed on a middle Miocene volcanic sequence with contrasting permeabilities and tensile strengths, produced alteration assemblages controlled by elevation, from Hg-mineralized sinter to subjacent precious metal veins over a vertical distance exceeding 790 m. Sinter and epiclastic deposits, interpreted to be remnant paleosurface basinal strata enclosed by 16.6 to 16.1 Ma rhyolites, overlie older volcaniclastic basinal deposits and were part of a regional fluvial-lacustrine system developed among ca. 16 to 12 Ma basalt-rhyolite eruptive centers throughout the northern Great Basin. Because of contrasting erosional resistance among altered and unaltered rocks, Buckskin Mountain represents inverse topography with sinter and silicified epiclastic deposits at the summit. Sinter and veins, correlated by common elements, similar mineralogy, age constraints, textures, S isotope compositions, and fluid inclusion microthermometry, were deposited by sinter-vein fluid, the first of two sequential hydrothermal fluid regimes that evolved in response to magmatism, tectonism, hydrology, and topography. Thermal quenching of distally derived sinter-vein fluid in planar conduits caused deposition of banded quartz-silicate-selenide-sulfide veins ???270 to > 440 m below sinter at 16.1 Ma; vei??ns were initially enveloped by zoned selvages of proximal K-feldspar + K-mica + quartz + pyrite and distal illite + chlorite + calcite + pyrite. Mixing of sinter-vein fluid with local meteoric water in saturated basinal deposits caused deposition of silica, Hg-Se-S-Cl minerals, and precious metals in sinter and epiclastic deposits. Elevated ???Se/???S in sinter-vein fluid, and the relatively large stability fields of reduced aqueous selenide species in the temperature range of 250?? to <100??C, enabled (but was not the cause of) codeposition of selenide-sulfide minerals and common element associations in veins and sinter. Acid-sulfate fluid of the second fluid regime was derived from oxidation of H2S and other volatiles exsolved from sinter-vein fluid. Acid-sulfate fluid produced (1) a subhorizontal zone of partially leached basinal deposits and rhyolite from the paleosurface to a depth of ???60 m, and (2) laterally pervasive zones, ???100 to 200 m thick, of quartz + alunite ?? hematite and quartz + kaolinite + pyrite in volcaniclastic deposits immediately beneath partially leached rocks, but this fluid did not decompose selenide-sulfide-precious metal phases in sinter. Paragenetically late vein and wall-rock assemblages, including marcasite + pyrite, calcite, and kaolinite-replaced K minerals, record deeper transition of sinter-vein fluid into acid-sulfate fluid in vein conduits. This transition occurred as regional subsidence, manifested by the Goosey Lake depression immediately east of Buckskin Mountain, lowered the pieziometric surface at Buckskin Mountain, terminated sinter deposition, and caused boiling and/or degassing of sinter-vein fluid. The timing of subsidence is recorded by a decrease in alunite ages, from ca. 15.8 to 15.6 Ma, with depth below sinter. Lateral replacement of sinter and partially leached epiclastic deposits and rhyolite by opal-A marks the termination of the two hydrothermal regimes that lasted ???0.5 m.y. and followed rhyolitic volcanism of similar duration. Veins and sinter display textures that attest to plastic deformation, spalling, and gravitational settling, and indicate fluid-flow direction, velocity, and density stratification which, with conduit topology, may have influenced precious metal tenor in the veins. Components of sinter and veins were transported as colloids, formed in supersaturated sinter-vein fluid, that aggregated or coagulated as incompetent gelatinous layers in shallow pools and in underlying, near-vertical conduits in rhyolite and initially crystallized as opal and chalcedony. The low thermal conductivity of ho

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

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.

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.

Improved silicon carbide for advanced heat engines

NASA Technical Reports Server (NTRS)

Whalen, T. J.; Winterbottom, W. L.

1986-01-01

Work performed to develop silicon carbide materials of high strength and to form components of complex shape and high reliability is described. A beta-SiC powder and binder system was adapted to the injection molding process and procedures and process parameters developed capable of providing a sintered silicon carbide material with improved properties. The initial effort has been to characterize the baseline precursor materials (beta silicon carbide powder and boron and carbon sintering aids), develop mixing and injection molding procedures for fabricating test bars, and characterize the properties of the sintered materials. Parallel studies of various mixing, dewaxing, and sintering procedures have been carried out in order to distinguish process routes for improving material properties. A total of 276 MOR bars of the baseline material have been molded, and 122 bars have been fully processed to a sinter density of approximately 95 percent. The material has a mean MOR room temperature strength of 43.31 ksi (299 MPa), a Weibull characteristic strength of 45.8 ksi (315 MPa), and a Weibull modulus of 8.0. Mean values of the MOR strengths at 1000, 1200, and 14000 C are 41.4, 43.2, and 47.2 ksi, respectively. Strength controlling flaws in this material were found to consist of regions of high porosity and were attributed to agglomerates originating in the initial mixing procedures. The mean stress rupture lift at 1400 C of five samples tested at 172 MPa (25 ksi) stress was 62 hours and at 207 MPa (30 ksi) stress was 14 hours. New fluid mixing techniques have been developed which significantly reduce flaw size and improve the strength of the material. Initial MOR tests indicate the strength of the fluid-mixed material exceeds the baseline property by more than 33 percent.

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

2011-06-14

A hydrogen permeable membrane is disclosed. The membrane is prepared by forming a mixture of metal oxide powder and ceramic oxide powder and a pore former into 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.

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.

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.

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

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.

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

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

Chen, I-Wei

Solid oxide fuel cells and solid oxide electrolysis cells rely on solid electrolytes in which a large ionic current dominates. This project was initiated to investigate microstructural changes in such devices under electrochemical forces, because nominally insignificant processes may couple to the large ionic current to yield non-equilibrium phenomena that alter the microstructure. Our studies had focused on yttria-stabilized cubic zirconia (YSZ) widely used in these devices. The experiments have revealed enhanced grain growth at higher temperatures, pore and gas bubble migration at all temperatures, and the latter also lead to enhanced sintering of highly porous ceramics into fully densemore » ceramics at unprecedentedly low temperatures. These results have shed light on kinetic processes that fall completely outside the realm of classical ceramic processing. Other fast-oxygen oxide ceramics closely related to, and often used in conjunction with zirconia ceramics, have also be investigated, as are closely related scientific problems in zirconia ceramics. These include crystal structures, defects, diffusion kinetics, oxygen potentials, low temperature sintering, flash sintering, and coarsening theory, and all have resulted in greater clarity in scientific understanding. The knowledge is leveraged to provide new insight to electrode kinetics and near-electrode mixed conductivity and to new materials. In the following areas, our research has resulted in completely new knowledge that defines the state-of-the-art of the field. (a) Electrical current driven non-equilibrium phenomena, (b) Enhanced grain growth under electrochemically reducing conditions, (c) Development of oxygen potential polarization in electrically loaded electrolyte, (d) Low temperature sintering and grain growth, and (e) Structure, defects and cation kinetics of fluorite-structured oxides. Our research has also contributed to synthesis of new energy-relevant electrochemical materials and new understanding of flash sintering, which is a rapid sintering process initiated by a large electrical loading.« less

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.

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

NASA Technical Reports Server (NTRS)

Zhong, Zhi-Min; Goldsby, Jon C.

2005-01-01

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

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.

Marginal and internal fit of curved anterior CAD/CAM-milled zirconia fixed dental prostheses: an in-vitro study.

PubMed

Büchi, Dominik L; Ebler, Sabine; Hämmerle, Christoph H F; Sailer, Irena

2014-01-01

To test whether or not different types of CAD/CAM systems, processing zirconia in the densely and in the pre-sintered stage, lead to differences in the accuracy of 4-unit anterior fixed dental prosthesis (FDP) frameworks, and to evaluate the efficiency. 40 curved anterior 4-unit FDP frameworks were manufactured with four different CAD/CAM systems: DCS Precident (DCS) (control group), Cercon (DeguDent) (test group 1), Cerec InLab (Sirona) (test group 2), Kavo Everest (Kavo) (test group 3). The DCS System was chosen as the control group because the zirconia frameworks are processed in its densely sintered stage and there is no shrinkage of the zirconia during the manufacturing process. The initial fit of the frameworks was checked and adjusted to a subjectively similar level of accuracy by one dental technician, and the time taken for this was recorded. After cementation, the frameworks were embedded into resin and the abutment teeth were cut in mesiodistal and orobuccal directions in four specimens. The thickness of the cement gap was measured at 50× (internal adaptation) and 200× (marginal adaptation) magnification. The measurement of the accuracy was performed at four sites. Site 1: marginal adaptation, the marginal opening at the point of closest perpendicular approximation between the die and framework margin. Site 2: Internal adaptation at the chamfer. Site 3: Internal adaptation at the axial wall. Site 4: Internal adaptation in the occlusal area. The data were analyzed descriptively using the ANOVA and Bonferroni/ Dunn tests. The mean marginal adaptation (site 1) of the control group was 107 ± 26 μm; test group 1, 140 ± 26 μm; test group 2, 104 ± 40 μm; and test group 3, 95 ± 31 μm. Test group 1 showed a tendency to exhibit larger marginal gaps than the other groups, however, this difference was only significant when test groups 1 and 3 were compared (P = .0022; Bonferroni/Dunn test). Significantly more time was needed for the adjustment of the frameworks of test group 1 compared to the other test groups and the control group (21.1 min vs 3.8 min) (P < .0001; Bonferroni/Dunn test). For the adjustment of the frameworks of test groups 2 and 3, the same time was needed as for the frameworks of the control group. No differences of the framework accuracy resulting from the different CAM and CAD/CAM procedures were found; however, only after adjustment of the fit by an experienced dental technician. Hence, the influence of a manual correction of the fit was crucial, and the efforts differed for the tested systems. The CAM system led to lower initial accuracy of the frameworks than the CAD/CAM systems, which may be crucial for the dental laboratory. The stage of the zirconia materials used for the different CAD/CAM procedures, ie presintered or densely sintered, exhibited no influence.

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.

Compaction and sintering behaviors of a Nd-Fe-B permanent magnet alloy

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

Chin, T.; Hung, M.; Tsai, D.

1988-11-15

Extensive x-ray diffraction (XRD) and magnetic measurements were done on Nd/sub 15/ Fe/sub 77/ B/sub 8/ magnet alloy green compacts after cold isostatic pressing following a pulsed 2-T field (CIP) and die-pressing under a static 1.2-T perpendicular field (DP1) or parallel field (DP2), and on those after sintering. An alignment factor F, through the calculation of the integrated diffraction intensity ratio of the XRD patterns, was adopted as the effectiveness of magnetic alignment. At the green compact state, DP1 has the best alignment while CIP the worst. However, after sintering the alignment factor was such that CIP>DPI>DP2, the same ordermore » as the magnetic properties. Three mechanisms were proposed for the evolution of the alignment factor at different stages of sintering, i.e., that both the appearance of a liquid phase at low temperatures and preferred grain growth at high temperatures enhance F, while recrystallization at intermediate temperatures deteriorates F. CIP results in less-defect green compact, hence less recrystallization, leading to better resultant alignment« less

Characterization of Long SiAION Ceramic Tubes for Gun Barrel Applications

DTIC Science & Technology

2006-06-01

sintering kinetics during the sintering of regions with different starting densities can all lead to the production of tubes with gradients in strength and...variations of dimensions. These gradients and deviations from anticipated dimensions all detract from the ability of the manufactured product to be...characteristics of the tubes can be introduced at various steps in the production process. When the powder is initially loaded to be cold

Surface free energy predominates in cell adhesion to hydroxyapatite through wettability.

PubMed

Nakamura, Miho; Hori, Naoko; Ando, Hiroshi; Namba, Saki; Toyama, Takeshi; Nishimiya, Nobuyuki; Yamashita, Kimihiro

2016-05-01

The initial adhesion of cells to biomaterials is critical in the regulation of subsequent cell behaviors. The purpose of this study was to investigate a mechanism through which the surface wettability of biomaterials can be improved and determine the effects of biomaterial surface characteristics on cellular behaviors. We investigated the surface characteristics of various types of hydroxyapatite after sintering in different atmospheres and examined the effects of various surface characteristics on cell adhesion to study cell-biomaterial interactions. Sintering atmosphere affects the polarization capacity of hydroxyapatite by changing hydroxide ion content and grain size. Compared with hydroxyapatite sintered in air, hydroxyapatite sintered in saturated water vapor had a higher polarization capacity that increased surface free energy and improved wettability, which in turn accelerated cell adhesion. We determined the optimal conditions of hydroxyapatite polarization for the improvement of surface wettability and acceleration of cell adhesion. Copyright © 2016 Elsevier B.V. All rights reserved.

Developing Cost-Effective Dense Continuous SDC Barrier Layers for SOFCs

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

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

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

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.

Environment-oriented low-cost porous mullite ceramic membrane supports fabricated from coal gangue and bauxite.

PubMed

Lü, Qikai; Dong, Xinfa; Zhu, Zhiwen; Dong, Yingchao

2014-05-30

Porous mullite ceramic supports for filtration membrane were successfully fabricated via recycling of coal gangue and bauxite at sintering temperatures from 1100 to 1500°C with corn starch as pore-forming agent. The dynamic sintering behaviors, phase evolution, shrinkage, porosity and pore size, gas permeation flux, microstructure and mechanical property were systematically studied. A unique volume-expansion stage was observed at increased temperatures from 1276 to 1481°C caused by a mullitization-crystal-growth process. During this stage, open porosity increases and pore size distributions broaden, which result in a maximum of nitrogen gas flux at 1400°C. The X-ray diffraction results reveal that secondary mullitization took place from 1100°C and the major phase is mullite with a content of ∼84.7wt.% at 1400°C. SEM images show that the as-fabricated mullite supports have a porous microstructure composed of sintered glassy particles embedded with inter-locked mullite crystals, which grew gradually with increasing temperature from rod-like into blocky-like morphologies. To obtain mullite membrane supports with sufficient porosity and acceptable mechanical strength, the relationship between porosity and mechanical strength was investigated, which was fitted using a parabolic equation. Copyright © 2014 Elsevier B.V. All rights reserved.

Semiconductor structural damage attendant to contact formation in III-V solar cells

NASA Technical Reports Server (NTRS)

Fatemi, Navid S.; Weizer, Victor G.

1991-01-01

In order to keep the resistive losses in solar cells to a minimum, it is often necessary for the ohmic contacts to be heat treated to lower the metal-semiconductor contact resistivity to acceptable values. Sintering of the contacts, however can result in extensive mechanical damage of the semiconductor surface under the metallization. An investigation of the detailed mechanisms involved in the process of contact formation during heat treatment may control the structural damage incurred by the semiconductor surface to acceptable levels, while achieving the desired values of contact resistivity for the ohmic contacts. The reaction kinetics of sintered gold contacts to InP were determined. It was found that the Au-InP interaction involves three consecutive stages marked by distinct color changes observed on the surface of the Au, and that each stage is governed by a different mechanism. A detailed description of these mechanisms and options to control them are presented.

Low-temperature sintering behavior of nanocrystalline indium tin oxide prepared from polymer-containing sols

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

Koroesi, Laszlo, E-mail: l.korosi@chem.u-szeged.hu; Papp, Szilvia; Oszko, Albert

2012-04-15

Highlights: Black-Right-Pointing-Pointer The synthesis of ITO powders and thin films from PVP-containing sols is presented. Black-Right-Pointing-Pointer The nano- and microstructures of ITO are more compact when PVP is used. Black-Right-Pointing-Pointer PVP acts both as a steric stabilizer of the sol and as a pre-sintering agent. Black-Right-Pointing-Pointer The PVP-induced enhanced sintering results in ITO with lower electrical resistance. Black-Right-Pointing-Pointer The surface composition of the ITO films is independent of the initial PVP content. -- Abstract: Indium tin hydroxide (ITH) xerogel powders and thin films with different polyvinylpyrrolidone (PVP) contents (0-22%, w/w) were prepared by a classical sol-gel method. To obtain nanocrystallinemore » indium tin oxide (ITO), the ITH xerogels were calcined at 550 Degree-Sign C. The effect of the initial polymer content on the structure of the ITO powders was studied by means of N{sub 2}-sorption measurements, small-angle X-ray scattering (SAXS), transmission and scanning electron microscopy. The N{sub 2}-sorption measurements revealed that the ITO powders obtained contained micropores and both their porosity and specific surface area decreased with increasing PVP content of the ITH xerogels. The SAXS measurements confirmed the enhanced sintering of the particles in the presence of PVP. The calculated mass fractal dimensions of the ITO powders increased significantly, indicating a significant compaction in structure. The pre-sintered structure could be achieved at relatively low temperature, which induced a significant decreasing (three orders of magnitude) in the electrical resistance of the ITO films.« less

Joining of porous silicon carbide bodies

DOEpatents

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

1990-05-01

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

Effect of processing conditions on microstructural features in Mn–Si sintered steels

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

Oro, Raquel, E-mail: raqueld@chalmers.se; Hryha, Eduard, E-mail: hryha@chalmers.se; Campos, Mónica, E-mail: campos@ing.uc3m.es

2014-09-15

Sintering of steels containing oxidation sensitive elements is possible if such elements are alloyed with others which present lower affinity for oxygen. In this work, a master alloy powder containing Fe–Mn–Si–C, specifically designed to create a liquid phase during sintering, has been used for such purpose. The effect of processing conditions such as sintering temperature and atmosphere was studied with the aim of describing the microstructural evolution as well as the morphology and distribution of oxides in the sintered material, evaluating the potential detrimental effect of such oxides on mechanical properties. Chemical analyses, metallography and fractography studies combined with X-raymore » photoelectron spectroscopy analyses on the fracture surfaces were used to reveal the main mechanism of fracture and their correlation with the chemical composition of the different fracture surfaces. The results indicate that the main mechanism of failure in these steels is brittle fracture in the surrounding of the original master alloy particles due to degradation of grain boundaries by the presence of oxide inclusions. Mn–Si oxide inclusions were observed on intergranular decohesive facets. The use of reducing atmospheres and high sintering temperatures reduces the amount and size of such oxide inclusions. Besides, high heating and cooling rates reduce significantly the final oxygen content in the sintered material. A model for microstructure development and oxide evolution during different stages of sintering is proposed, considering the fact that when the master alloy melts, the liquid formed can dissolve some of the oxides as well as the surface of the surrounding iron base particles. - Highlights: • Oxide distribution in steels containing oxidation-sensitive elements • Mn, Si introduced in a master alloy powder, mixed with a base iron powder • Selective oxidation of Mn and Si on iron grain boundaries • Decohesive fracture caused by degradation of grain boundaries by oxide inclusions • Reducing agents efficient at low temperatures critical for avoiding oxide inclusions.« less

Dry Snow Metamorphism

DTIC Science & Technology

2012-09-19

behavior of snow during metamorphism and grain sintering using mathematical models. 2 Approach Our approach involved the collection and...examination of both types of specimens at various stages of metamorphism using the SEM and micro-CT. More specifically, the above approach involved...than 10ºC·m-1). 5. High-resolution images and X-ray spectra of snow specimens at various metamorphism stages were obtained using an SEM and EDS. 6

Sintering mechanism of the CaF2 on hydroxyapatite by a 10.6-l microm CO2 laser.

PubMed

Wu, Cheng-Chei; Roan, Rong-Tai; Chen, Jeng-Huey

2002-01-01

Laser has been reported as a heat source for melting and re-crystallization. Occurring at about 1100 degrees C, the melting of surface dental enamel along with re-crystallization might have an assistant role in the therapy of hypersensitive tooth, apical sealing of endodontic surgery in dentistry, preventive dentistry for pit and fissure sealing, and fluoridation. For laser to be accepted in clinical applications, it is desired that, studies must show the incorporation of CaF(2) into hydroxyapatite could reduce the sintering temperature for the sake of safety. In this study, the Sharplan 20XJ CO(2) laser with 10.6- microm wavelength was set under the following parameters: power, 5 W; repetitive mode, 0.1 second; beam, focused. Fluorite was added to hydroxyapatite as a synthetic compound to lower the sintering temperature. Human dental enamel without caries was used for in vitro sintering test. Scanning electron microscopy (SEM), X-ray diffractometer (XRD), Fourier transforming infrared spectroscopy (FTIR), and differential thermal analysis/thermogravimetric analysis (DAT/TGA) were used for the investigation of sintering mechanism of CaF(2). Fusion between hexagonal shape crystals and cubic shape crystals (CaF(2)) were observed under SEM study. Hexagonal shape crystals indicated the formation of fluorapatite under XRD analysis. Under FTIR study, we examined reductions of water (3445 cm(-1)) and hydroxyl bands (3567 and 627 cm(-1)) in irradiated compounds. From the DTA pattern of synthetic compound, it showed the endothermic reaction reaching its peak point around 1180 +/- 20 degrees C. It was attributed to the phase transformation and/or initial melting. In this study, we proposed the interrelationship of the eutectics between initiator (CaF(2)) and the reaction product (calcium hydroxide) that reduced the sintering temperature. It appeared that the co-eutectics interacted to reduce the sintering temperature of hydroxyapatite below 800 degrees C and that the key eutectic was calcium hydroxide. The clinical feasibility of the melting and re-crystallization of hydroxyapatite under 10.6-microm CO(2) laser would be therefore enhanced. Copyright 2002 Wiley-Liss, Inc.

Effect of sintering in a hydrogen atmosphere on the density and coercivity of (Sm,Zr)(Co,Cu,Fe)Z permanent magnets

NASA Astrophysics Data System (ADS)

Burkhanov, G. S.; Dormidontov, N. A.; Kolchugina, N. B.; Dormidontov, A. G.

2018-04-01

The effect of heat treatments in manufacturing (Sm,Zr)(Co,Cu,Fe)Z-based permanent magnets sintered in a hydrogen atmosphere on their properties has been studied. It was shown that the dynamics of the magnetic hardening of the studied magnets during heat treatments, in whole, corresponds to available concepts of phase transformations in five-component precipitation-hardened SmCo-based alloys. Peculiarities of the studied compositions consist in the fact that the coercive force magnitude of magnets quenched from the isothermal aging temperature is higher by an order of magnitude than those available in the literature. It was noted that, in using the selected manufacturing procedure, the increase in the density of samples does not finish at the sintering stage but continues in the course of solid-solution heat treatment.

Direct observation of grain rotations during coarsening of a semisolid Al–Cu alloy

PubMed Central

Dake, Jules M.; Oddershede, Jette; Sørensen, Henning O.; Werz, Thomas; Shatto, J. Cole; Uesugi, Kentaro; Schmidt, Søren; Krill, Carl E.

2016-01-01

Sintering is a key technology for processing ceramic and metallic powders into solid objects of complex geometry, particularly in the burgeoning field of energy storage materials. The modeling of sintering processes, however, has not kept pace with applications. Conventional models, which assume ideal arrangements of constituent powders while ignoring their underlying crystallinity, achieve at best a qualitative description of the rearrangement, densification, and coarsening of powder compacts during thermal processing. Treating a semisolid Al–Cu alloy as a model system for late-stage sintering—during which densification plays a subordinate role to coarsening—we have used 3D X-ray diffraction microscopy to track the changes in sample microstructure induced by annealing. The results establish the occurrence of significant particle rotations, driven in part by the dependence of boundary energy on crystallographic misorientation. Evidently, a comprehensive model for sintering must incorporate crystallographic parameters into the thermodynamic driving forces governing microstructural evolution. PMID:27671639

Valorization of lignite combustion residues and ferroalumina in the production of aggregates.

PubMed

Anagnostopoulos, I M; Stivanakis, V E; Angelopoulos, G N; Papamantellos, D C

2010-02-15

The present research study investigates the synergy of industrial solid by-products from lignite combustion (fly ash and bottom ash) and aluminum production (ferroalumina) in the production of lightweight aggregates (LWA). The process consists of two stages, pelletization and sintering. Bottom ash (BA) is used as the principal raw material in mixtures while ferroalumina (FAL) is added in lower percentages (5-30 wt%). BA carbon content is used as the fuel of sintering process in high temperatures, around 1250 degrees C, and gas generation is responsible for porous structure formation. Physical properties such as porosity, water absorption and bulk density, of sintering products are measured. Increase of FAL percentage in sintering mixtures results in decrease of porosity from 61% to 35% and of water absorption from 61% to 21% and in increase of bulk density from 1.02 g/cm(3) to 1.80 g/cm(3) of the produced aggregates. Aggregates produced by FAL addition up to 20 wt% are characterized as LWA. Aggregates formed are used in the production of concrete specimens. Compressive strength of concrete increases by increasing FAL addition in aggregates from 5 wt% to 15 wt% (highest strength value), while decrease by increasing FAL addition from 20 wt% to 30 wt%. FAL addition in lignite ashes sintering mixtures (up to 15 wt%) is considered as an important parameter for enhancing aggregates strength.

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

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

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

2009-11-01

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

Cyclic Failure Mechanisms of Thermal and Environmental Barrier Coating Systems Under Thermal Gradient Test Conditions

NASA Technical Reports Server (NTRS)

Zhu, Dongming; Lee, Kang N.; Miller, Robert A.

2002-01-01

Plasma-sprayed ZrO2-8wt%Y2O3 and mullite+BSAS/Si multilayer thermal and environmental barrier coating (TBC-EBC) systems on SiC/SiC ceramic matrix composite (CMC) substrates were thermally cyclic tested under high thermal gradients using a laser high-heat-flux rig in conjunction with furnace exposure in water-vapor environments. Coating sintering and interface damage were assessed by monitoring the real-time thermal conductivity changes during the laser heat-flux tests and by examining the microstructural changes after exposure. Sintering kinetics of the coating systems were also independently characterized using a dilatometer. It was found that the coating failure involved both the time-temperature dependent sintering and the cycle frequency dependent cyclic fatigue processes. The water vapor environments not only facilitated the initial coating conductivity increases due to enhanced sintering and interface reaction, but also promoted later conductivity reductions due to the accelerated coating cracking and delamination. The failure mechanisms of the coating systems are also discussed based on the cyclic test results and are correlated to the sintering and thermal stress behavior under the thermal gradient test conditions.

Laser Sintering Technology and Balling Phenomenon.

PubMed

Oyar, Perihan

2018-02-01

The aim of this review was to evaluate the balling phenomenon which occurs typically in Selective Laser Sintering (SLS). The balling phenomenon is a typical SLS defect, and observed in laser sintered powder, significantly reduces the quality of SLS, and hinders the further development of SLS Technology. Electronic database searches were performed using Google Scholar. The keywords "laser sintering, selective laser sintering, direct metal laser melting, and balling phenomenon" were searched in title/abstract of publications, limited to December 31, 2016. The inclusion criteria were SLS, balling phenomenon, some alloys (such as Cr-Co, iron, stainless steel, and Cu-based alloys) mechanical properties, microstructure and bond strength between metal-ceramic crown, laboratory studies, full text, and in English language. A total of 100 articles were found the initial search and yielded a total of 50 studies, 30 of which did not fulfill the inclusion criteria and were therefore excluded. In addition, 20 studies were found by screening the reference list of all included publications. Finally, 40 studies were selected for this review. The method in question is regulated by powder material characteristics and the conditions of laser processing. The procedure of formation, affecting factors, and the mechanism of the balling effect are very complex.

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.

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.

Simulation of Patterned Glass Film Formation in the Evaporating Colloidal Liquid under IR Heating

NASA Astrophysics Data System (ADS)

Kolegov, K. S.

2018-02-01

The paper theoretically studies the method of evaporative lithography in combination with external infrared heating. This method makes it possible to form solid microstructures of the required relief shape as a result of evaporation of the liquid film of the colloidal solution under the mask. The heated particles are sintered easier, so there are no cracks in the obtained structure, unlike the structure obtained employing the standard method of evaporative lithography. The paper puts forward a modification of the mathematical model which allows to describe not only heat and mass transfer at the initial stage of the process, but also the phase transition of colloidal solution into glass. Aqueous latex is taken as an example. The resulting final form of solid film is in good agreement with the experimental data of other authors.

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

The effect of precipitation and calcination parameters on oxalate derived ThO2 pellets

NASA Astrophysics Data System (ADS)

Wangle, Tadeas; Tyrpekl, Vaclav; Cagno, Simone; Delloye, Thierry; Larcher, Olivier; Cardinaels, Thomas; Vleugels, Jozef; Verwerft, Marc

2017-11-01

Thorium oxalate is easy to prepare, but the derived oxide powders retain the platelet morphology of the primary oxalate. This negatively impacts packing and sintering. If powder milling is to be avoided, powder synthesis needs to be optimized. That is the goal of this paper, where different precipitation strategies were used and their effect on powder characteristics and pellet synthesis was investigated. Oxalates prepared by adding a thorium nitrate solution to an oxalic acid solution proved most promising. Further optimizing of the calcination temperature revealed that with increasing calcination temperature the packing density improved significantly. This came at the cost of decreased early stage sintering and a higher frequency of end-capping during compaction. The calcination temperature at which the highest final density can be reached was dependent on the sintering cycle. Furthermore, the ThO2 powders had less surface area and thus adsorbed less gases during storage when calcined at higher temperatures.

Prediction of La0.6Sr0.4Co0.2Fe0.8O3 cathode microstructures during sintering: Kinetic Monte Carlo (KMC) simulations calibrated by artificial neural networks

NASA Astrophysics Data System (ADS)

Yan, Zilin; Kim, Yongtae; Hara, Shotaro; Shikazono, Naoki

2017-04-01

The Potts Kinetic Monte Carlo (KMC) model, proven to be a robust tool to study all stages of sintering process, is an ideal tool to analyze the microstructure evolution of electrodes in solid oxide fuel cells (SOFCs). Due to the nature of this model, the input parameters of KMC simulations such as simulation temperatures and attempt frequencies are difficult to identify. We propose a rigorous and efficient approach to facilitate the input parameter calibration process using artificial neural networks (ANNs). The trained ANN reduces drastically the number of trial-and-error of KMC simulations. The KMC simulation using the calibrated input parameters predicts the microstructures of a La0.6Sr0.4Co0.2Fe0.8O3 cathode material during sintering, showing both qualitative and quantitative congruence with real 3D microstructures obtained by focused ion beam scanning electron microscopy (FIB-SEM) reconstruction.

A primary study into graphene/polyether ether ketone (PEEK) nanocomposite for laser sintering

NASA Astrophysics Data System (ADS)

Chen, Binling; Berretta, Silvia; Evans, Ken; Smith, Kaylie; Ghita, Oana

2018-01-01

This paper proposes two methods of preparation of graphene/PEEK powders for Laser Sintering (LS) and investigates their behaviour in relation to their microstructure and their properties. Thin composite films were fabricated in an attempt to replicate the thin layer formation of the powder bed process. Both methods of composite powder preparation (wet and dry) led to enhanced mechanical performance of the composite films at 0.1 and 0.5 wt% graphene nano-platelets (GNP) concentrations. The TEM images show that the GNP act as a nucleation point in crystallisation of PEEK, being at the centre of the spherulites. The hot stage microscopy reveals a 20 s delay in the onset of GNP/PEEK nanocomposite coalescence in comparison with plain PEEK. This is a very important observation for laser sintering, as it will influence the build strategy and specific parameters (e.g. time between layers deposition, multiple exposures). The excellent electrical conductivity properties of graphene were noticeable in the nanocomposite films at concentrations above 1 wt% GNP.

Phenomenological analysis of densification mechanism during spark plasma sintering of MgAl2O4

NASA Astrophysics Data System (ADS)

Bernard-Granger, Guillaume; Benameur, Nassira; Addad, Ahmed; Nygren, Mats; Guizard, Christian; Deville, Sylvain

2009-05-01

Spark plasma sintering (SPS) of MgAl2O4 powder was investigated at temperatures between 1200 and 1300{\\deg}C. A significant grain growth was observed during densification. The densification rate always exhibits at least one strong minimum, and resumes after an incubation period. Transmission electron microscopy investigations performed on sintered samples never revealed extensive dislocation activity in the elemental grains. The densification mechanism involved during SPS was determined by anisothermal (investigation of the heating stage of a SPS run) and isothermal methods (investigation at given soak temperatures). Grain-boundary sliding, accommodated by an in-series {interface-reaction/lattice diffusion of the O$^2$-anions} mechanism controlled by the interface-reaction step, governs densification. The zero-densification-rate period, detected for all soak temperatures, arise from the difficulty of annealing vacancies, necessary for the densification to proceed. The detection of atomic ledges at grain boundaries and the modification of the stoichiometry of spinel during SPS could be related to the difficulty to anneal vacancies at temperature soaks.

Collisional disruption of porous weak sintered targets at low impact velocity

NASA Astrophysics Data System (ADS)

Setoh, M.; Nakamura, A. M.; Hirata, N.; Hiraoka, K.; Arakawa, M.

Porous structure is common in asteroids and satellites of outer planets In order to study the relation between structure of the small bodies and their thermal and collisional evolution we prepared porous sintered targets measured the compressive strength and determined their impact strength Previous studies showed using sintered glass beads Love et al 1993 the targets with higher compressive strength have higher impact strength and the targets with higher porosity have higher impact strength However in these experiments the porosity of the targets were changed according to the compressive strength Therefore we fixed the porosity while the compressive strength was varied Our experiments were performed with low impact velocity condition because low impact velocities are common among icy bodies far from the Earth We sintered soda lime glass beads of 50 micron diameter and 2 5g cm -3 nominal density at various temperatures and durations to produce targets with similar porosity sim 40 and different compressive strength 0 2 sim 7 8MPa We performed impact disruption experiments using a low velocity light-gas gun at Kobe University sim 100m s We used cylindrical polycarbonate projectiles 1 5 cm in height and 1 0 cm in diameter We determined the specific energy J kg of projectile kinetic energy per kilo gram initial target mass for the condition that the largest fragment mass being the half of the initial target mass is the threshold energy for collisional disruption Q Fujiwara et al 1989 Holsapple et al

Study of micropart fabrication via 17-4 PH stainless nanopowder injection molding.

PubMed

Tirta, Andy; Prasetyo, Yus; Baek, Eung-Ryul; Choi, Chul-Jin

2011-01-01

Micropart fabrication via 17-4 PH stainless nanopowder injection molding was investigated. The nanopowder was mixed with a binder that was based on wax to produce a feedstock composed of 45% powder and binder (the powder load). Initially, the fit and proper test was done before the micropart was made by making some bars of green samples, which the properties were examined after the sintering process. The examination involved the mechanical properties such as the porosity, hardness, and some of metallurgical aspects, such as the second-phase formation and the final compound after the sintering. The results showed that utilizing 17-4 PH stainless nanopowder is promising for micropart fabrication since it can form a nearly full-density sintered sample with a low porosity and good toughness, and can provide a smooth surface finish. After this, the investigations followed with the injection of the feedstock into the PDMS micromold that was formed by the nickel pattern from the X-Ray LIGA process. The green samples successfully produced a high-aspect-ratio sample with a thickness of up to 1 mm and an aspect ratio of 15 in the microchannel part. Then the green samples were sintered at 1,300 degrees C for 2 h, since from the initial test, they showed optimum parameters with nearly full density, low porosity, and a high degree of hardness. The research shows the excellent results of the application of the 17-4 PH stainless nanopowder to micropart fabrication.

Formation of Green compact structure of low-temperature ceramics with taking into account the thermal degradation of the binder

NASA Astrophysics Data System (ADS)

Tovpinets, A. O.; Leytsin, V. N.; Dmitrieva, M. A.; Ivonin, I. V.; Ponomarev, S. V.

2017-12-01

The solution of the tasks in the field of creating and processing materials for additive technologies requires the development of a single theory of materials for various applications and processes. A separate class of materials that are promising for use in additive technologies includes materials whose consolidation is ensured by the presence of low-melting components in the initial mixture which form a matrix at a temperature not exceeding the melting point, recrystallization or destruction of any of the responsible refractory components of the initial dispersion. The study of the contribution of the binder thermal destruction to the structure and phase composition of the initial compact of the future composite is essential for the development of modern technologies for the synthesis of low-temperature ceramics. This paper investigates the effect of the thermal destruction of a binder on the formation of a green compact of low-temperature ceramics and the structural-mechanical characteristics of sintered ceramics. The approach proposed in Ref. [1] for evaluating the structure and physical characteristics of sintered low-temperature ceramics is improved to clarify the structure of green compacts obtained after thermal destruction of the polymer binder, with taking into account the pores formed and the infusible residue. The obtained results enable a more accurate prediction of thermal stresses in the matrix of sintered ceramics and serve as a basis for optimization.

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.

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

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

A new in vivo screening model for posterior spinal bone formation: comparison of ten calcium phosphate ceramic material treatments.

PubMed

Wilson, Clayton E; Kruyt, Moyo C; de Bruijn, Joost D; van Blitterswijk, Clemens A; Oner, F Cumhur; Verbout, Abraham J; Dhert, Wouter J A

2006-01-01

This study presents a new screening model for evaluating the influence of multiple conditions on the initial process of bone formation in the posterior lumbar spine of a large animal. This model uses cages designed for placement on the decorticated transverse process of the goat lumbar spine. Five conduction channels per cage, each be defined by a different material treatment, are open to both the underlying bone and overlying soft tissue. The model was validated in ten adult Dutch milk goats, with each animal implanted with two cages containing a total of ten calcium phosphate material treatments according to a randomized complete block design. The ten calcium phosphate ceramic materials were created through a combination of material chemistry (BCP, TCP, HA), sintering temperature (low, medium, high), calcination and surface roughness treatments. To monitor the bone formation over time, fluorochrome markers were administered at 3, 5 and 7 weeks and the animals were sacrificed at 9 weeks after implantation. Bone formation in the conduction channels was investigated by histology and histomorphometry of non-decalcified sections using traditional light and epifluorescent microscopy. According to both observed and measured bone formation parameters, materials were ranked in order of increasing magnitude as follows: low sintering temperature BCP (rough and smooth) approximately medium sintering temperature BCP approximately = TCP > calcined low sintering temperature HA > non-calcined low sintering temperature HA > high sintering temperature BCP (rough and smooth) > high sintering temperature HA (calcined and non-calcined). These results agree closely with those obtained in previous studies of osteoconduction and bioactivity of ceramics thereby validating the screening model presented in this study.

Impact of annealing on features of BCP coating on NiTi shape memory alloy: Preparation and physicochemical characterization

NASA Astrophysics Data System (ADS)

Dulski, Mateusz; Dudek, Karolina; Grelowski, Michał; Kubacki, Jerzy; Hertlein, Justyna; Wojtyniak, Marcin; Goryczka, Tomasz

2018-04-01

A multifunctional composite structure consisting of resorbable tricalcium phosphate with non-resorbable hydroxyapatite and NiTi shape memory alloy (SMA) has been manufactured to develop a biocompatible system for long-term implant applications. The hybrid system has been vacuum sintered to consolidate and form chemical binding between phosphate biomaterials and NiTi SMA. In this context, the impact of sintering on biomaterial's features in relation to initial material has been analyzed using a combination of structural and surface sensitive approaches. Moreover, a partial decomposition of the NiTi parent phase to the equilibrium Ti2Ni with cubic structure, and non-equilibrium Ti3Ni4 with hexagonal structure has been detected. Moreover, a sintering has provided a reconstruction of the orthophosphate surface through the disintegration of calcium phosphate material and increase of hydroxyapatite with smaller particles in volume. The biomaterial surface has become more enriched in calcium in relation to the initial composition, with a simultaneous decline of the roughness parameters due to the gradual consolidation of orthophosphates. Finally, surface modification accompanied with heat treatment has led to an increase of surface Young's modulus as an effect of partial recrystallization of calcium phosphates.

Performance and Reliability of Bonded Interfaces for High-temperature Packaging: Annual Progress Report

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

DeVoto, Douglas J.

2017-10-19

As maximum device temperatures approach 200 °Celsius, continuous operation, sintered silver materials promise to maintain bonds at these high temperatures without excessive degradation rates. A detailed characterization of the thermal performance and reliability of sintered silver materials and processes has been initiated for the next year. Future steps in crack modeling include efforts to simulate crack propagation directly using the extended finite element method (X-FEM), a numerical technique that uses the partition of unity method for modeling discontinuities such as cracks in a system.

Enhancement of structural and magnetic properties of M-type hexaferrite permanent magnet based on synthesis temperature

NASA Astrophysics Data System (ADS)

Anjum, Safia; Sehar, Fatima; Mustafa, Zeeshan; Awan, M. S.

2018-01-01

The main purpose of this research work is to develop the single domain magnetic particles of M-type barium hexaferrite (BaFe12O19) using oxide precursors employing conventional powder metallurgy technique. The phase formation and magnetic performance of the powders and magnets will be optimized by adjusting calcination and sintering temperatures. The synthesis of M-type barium hexaferrite was carried out in two sections. A series of four samples have been prepared by initial wet mixed powders calcined at different temperatures, i.e., 750, 850, 950 and 1050 °C. On the basis of structural analysis, the sample calcined at 950 °C has been selected and further divided into four parts to sintered them at 1100, 1150, 1200 and 1250 °C. The structural measurements depict the confirmation of M-type barium hexaferrite structure. SEM micrographs show the hexagonal-shaped grains. The abrupt decrease in coercivity for the sample sintered at 1250 °C has been seen which may be due to high sintering temperature, at which the particles have multi-domain properties.

Effects of Ta2O5 Addition on Electrical Properties of ZnO-V2O5 Based Varistor Ceramics

NASA Astrophysics Data System (ADS)

Fan, J. W.; Zhao, H. J.; Zhang, X. L.

2018-05-01

ZnO varistors are widely used for the protection of electronic and electrical equipment against transient surges. ZnO–V2O5 based varistor system is a potential candidate which can co-fire with Ag, and avoids the use of expensive Pa and Pt as the inner electrode in making multilayer chip varistors. However, the study of ZnO–V2O5-based ceramics is still in the initial stage for practical applications. The current work reports the effects of Ta2O5 on the electrical properties of ZnO-V2O5 based varistor ceramics. It shows that within 850-925°C experimental sintering temperature, the addition of Ta2O5 (0.05-0.20 mol%) may not improve the nonlinear coefficient but reduces the breakdown field of ZnO–V2O5 varistor ceramics.

In situ microscopy of rapidly heated nano-Al and nano-Al/WO{sub 3} thermites

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

Sullivan, Kyle T.; Zachariah, Michael R.; Chiou, Wen-An

2010-09-27

The initiation and reaction mechanism of nano-Al and nano-Al thermites in rapid heating environments is investigated in this work. A semiconductor-based grid/stage was used, capable of in situ heating of a sample from room temperature to 1473 K, and at a rate of 10{sup 6} K/s, inside an electron microscope. Nano-Al was rapidly heated in a transmission electron microscope, and before and after images indicate that the aluminum migrates through the shell, consistent with a diffusion-based mechanism. A nano-Al/WO{sub 3} composite was then heated in a scanning electron microscope. The results indicate that a reactive sintering mechanism is occurring formore » the nano-Al/WO{sub 3} thermite, as the products are found to be in surface contact and significantly deformed after the heating pulse.« less

Utilization of lignite power generation residues for the production of lightweight aggregates.

PubMed

Anagnostopoulos, Iason M; Stivanakis, Victor E

2009-04-15

A novel process is proposed for the utilization of lignite combustion solid residues in the production of inflammable lightweight aggregates (LWA). The process consists of two stages, pelletization and sintering, and carbon contained in BA was used as the process fuel. The main residues bottom ash (BA) and fly ash (FA) from Megalopolis power plant were characterized, mixed in different proportions and treated through pelletization and sintering process. Sintering benefits from combustion of BA carbon content and the product is a hardened porous cake. The energy required for achievement of high temperatures, in the range of 1250 degrees C, was offered by carbon combustion and CO(2) evolution is responsible for porous structure formation. Selected physical properties of sintered material relevant to use as lightweight aggregates were determined, including bulk density, porosity and water absorption. Bulk density varies from 0.83 to 0.91 g/cm(3), porosity varies from 60% to 64% and water absorption varies from 66% to 80%. LWA formed is used for the production of lightweight aggregate concrete (LWAC). Thermal conductivity coefficient varies from 0.25 to 0.37 W/mK (lower than maximum limit 0.43 W/mK) and compressive strength varies from 19 to 23 MPa (higher than minimum limit 17 MPa). The results indicate that sintering of lignite combustion residues is an efficient method of utilization of carbon containing BA and production of LWA for structural and insulating purposes. Carbon content of BA is a key factor in LWA production. Finally, this research work comprises the first proposed application for utilization of BA in Greece.

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

NASA Astrophysics Data System (ADS)

Wang, Pauchiu Either

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

Application of CTLM method combining interfacial structure characterization to investigate contact formation of silver paste metallization on crystalline silicon solar cells

NASA Astrophysics Data System (ADS)

Xiong, Shenghu; Yuan, Xiao; Tong, Hua; Yang, Yunxia; Liu, Cui; Ye, Xiaojun; Li, Yongsheng; Wang, Xianhao; Luo, Lan

2018-04-01

Circular transmission line model (CTLM) measurements were applied to study the contact formation mechanism of the silver paste metallization on n-type emitter of crystalline silicon solar cells. The electrical performance parameters ρc,Rsk , and Lt , which are related to the physical and chemical states of the multiphase materials at the interface, were extracted from the CTLM measurements, and were found to be sensitive to sintering temperature. As the temperature increased from 585 °C to 780 °C, initially the ρc value decreased rapidly, then flattened out and increased slightly. The order of resistivity magnitude was restricted by the SiNx passivation layer in the early sintering stages, and relied on the carrier tunneling probability affected by the precipitated silver crystallites or colloids, emitter doping concentration and molten glass layer. Based on the calculations that the sheet resistance underneath the electrode was reduced form 110 Ω / □ to 0.186 Ω / □ , it could be inferred that there was formation of a highly conductive layer of silver crystallites and colloids contained glass on the emitter. The transfer length Lt exhibited a U-shaped variation along with the temperature, reflecting the variation of the interfacial electrical properties. Overall, this article shows that the CTLM method can become a new powerful tool for researchers to meet the challenges of silver paste metallization innovation for manufacturing high-efficiency silicon solar cells.

Constrained Sintering in Fabrication of Solid Oxide Fuel Cells

PubMed Central

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

2016-01-01

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

Layered Manufacturing: Challenges and Opportunities

DTIC Science & Technology

2003-04-01

quality of the surface finish, eliminating residual stress , controlling local composition and microstructure, achieving fine feature size and...applications. Some methods have achieved commercial status, having graduated from the university level, others are in various stages of research. However...Road * Sintering * Co-firing * Shrinkage * Gas dimensions + Powder or + Resin * Residual stress precursors * Layer wire feeding infiltration * Distortion

A Novel Process for Joining Ti Alloy and Al Alloy using Two-Stage Sintering Powder Metallurgy

NASA Astrophysics Data System (ADS)

Long, Luping; Liu, Wensheng; Ma, Yunzhu; Wu, Lei; Liu, Chao

2018-04-01

The major challenges for conventional diffusion bonding of joining Ti alloy and Al alloy are the undesirable interfacial reaction, low matrixes and joint strength. To avoid the problem in diffusion bonding, a novel two-stage sintering powder metallurgy process is developed. In the present work, the interface characterization and joint performance of the bonds obtained by powder metallurgy bonding are investigated and are compared with the diffusion bonded Ti/Al joints obtained with the same and the optimized process parameters. The results show that no intermetallic compound is visible in the Ti/Al joint obtained by powder metallurgy bonding, while a new layer formed at the joint diffusion bonded with the same parameters. The maximum tensile strength of joint obtained by diffusion bonding is 58 MPa, while a higher tensile strength reaching 111 MPa for a bond made by powder metallurgy bonding. Brittle fractures occur at all the bonds. It is shown that the powder metallurgy bonding of Ti/Al is better than diffusion bonding. The results of this study should benefit the bonding quality.

Examining nanoparticle assemblies using high spatial resolution x-ray microtomography

NASA Astrophysics Data System (ADS)

Jenneson, P. M.; Luggar, R. D.; Morton, E. J.; Gundogdu, O.; Tüzün, U.

2004-09-01

An experimental system has been designed to examine the assembly of nanoparticles in a variety of process engineering applications. These applications include the harvesting from solutions of nanoparticles into green parts, and the subsequent sintering into finished components. The system is based on an x-ray microtomography with a spatial resolution down to 5μm. The theoretical limitations in x-ray imaging are considered to allow experimental optimization. A standard nondestructive evaluation type apparatus with a small focal-spot x-ray tube, high-resolution complementary metal oxide semiconductor flat-panel pixellated detector, and a mechanical rotational stage is used to image the static systems. Dynamic sintering processes are imaged using the same x-ray source and detector but a custom rotational stage which is contained in an environmental chamber where the temperature, atmospheric pressure, and compaction force can be controlled. Three-dimensional tomographic data sets are presented here for samples from the pharmaceutical, nutraceutical, biotechnology, and nanoparticle handling industries and show the microscopic features and defects which can be resolved with the system.

Removal of polychlorinated naphthalenes by desulfurization and emissions of polychlorinated naphthalenes from sintering plant

PubMed Central

Wang, Mengjing; Liu, Wenbin; Hou, Meifang; Li, Qianqian; Han, Ying; Liu, Guorui; Li, Haifeng; Liao, Xiao; Chen, Xuebin; Zheng, Minghui

2016-01-01

The sintering flue gas samples were collected at the inlets and outlets of the desulfurization systems to evaluate the influence of the systems on PCNs emission concentrations, profiles, and emission factors. The PCNs concentrations at the inlets and outlets were 27888–153672 pg m−3 and 11988–42245 pg m−3,respectively. Desulfurization systems showed excellent removal for PCNs, and the removal efficiencies of PCNs increase with increasing chlorination level. Lower chlorinated homologs are more sensitive to the desulfurization process than higher ones. High levels of PCNs were also detected in the gypsum (11600–29720 pg g−1) and fly ash samples (4946–64172 pg g−1). The annual total emissions of PCNs released to flue gas and gypsum from the sintering plants were about 394 kg, 48.5% of which was in gypsum. The surface area of the fly ash samples increased significantly from the first to the fourth stage of the series-connected electrostatic precipitator, accompanying obvious rising of concentration of PCNs in the fly ash samples. PMID:27197591

Microalloying of transition metal silicides by mechanical activation and field-activated reaction

DOEpatents

Munir, Zuhair A [Davis, CA; Woolman, Joseph N [Davis, CA; Petrovic, John J [Los Alamos, NM

2003-09-02

Alloys of transition metal suicides that contain one or more alloying elements are fabricated by a two-stage process involving mechanical activation as the first stage and densification and field-activated reaction as the second stage. Mechanical activation, preferably performed by high-energy planetary milling, results in the incorporation of atoms of the alloying element(s) into the crystal lattice of the transition metal, while the densification and field-activated reaction, preferably performed by spark plasma sintering, result in the formation of the alloyed transition metal silicide. Among the many advantages of the process are its ability to accommodate materials that are incompatible in other alloying methods.

Physico-chemical characteristics and protein adsorption potential of hydroxyapatite particles: influence on in vitro biocompatibility of ceramics after sintering.

PubMed

Rouahi, M; Champion, E; Gallet, O; Jada, A; Anselme, K

2006-01-15

Through the example of two HA ceramics prepared from two HA powders (HAD and HAL), we explored the relation between the physico-chemical qualities of the initial HA powder and the final HA ceramic and their influence on the protein adsorption and cell response to the final HA ceramics. The powders were characterized by XRD, FT-IR, zeta potential, and specific surface area (SSA). Their protein adsorption potential was tested after immersion in culture medium +15% of fetal calf serum. These results were correlated with the protein adsorption potential of the two ceramics (cHAD and cHAL) prepared from the HAD and HAL powders respectively and to the cell attachment after 4, 24 and 72 h on the ceramics. From our results, it appears that a relation can be established between the physico-chemical characteristics of the initial HA powders and the final biological response to the sintered ceramics prepared from these powders. An inverse relation exists between the SSA and the protein adsorption capacity of HA powders and the protein adsorption and cell attachment on HA ceramics. This inverse relation is related to phenomenon occurring during the sintering phase and the formation of inter-granular micro-porosity.

Production of a Powder Metallurgical Hot Work Tool Steel with Harmonic Structure by Mechanical Milling and Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Deirmina, Faraz; Pellizzari, Massimo; Federici, Matteo

2017-04-01

Commercial AISI-H13 gas atomized powders (AT) were mechanically milled (MM) to refine both the particle size and the microstructure. Different volume fractions of coarser grained (CG) AT powders were mixed with the ultra-fine grained (UFG) MM and consolidated by spark plasma sintering to obtain bulks showing a harmonic structure ( i.e. a 3D interconnected network of UFG areas surrounding the CG atomized particles). The low sintering temperature, 1373.15 K (1100 °C) and the short sintering time (30 minutes) made it possible to obtain near full density samples while preserving the refined microstructure induced by MM. A combination of high hardness and significantly improved fracture toughness is achieved by the samples containing 50 to 80 vol pct MM, essentially showing harmonic structure. The design allows to easily achieve specific application oriented properties by varying the MM volume fraction in the initial mixture. Hardness is governed by the fine-grained MM matrix and improved toughening is due to (1) deviatory effect of AT particles and (2) energy dissipation as a result of the decohesion in MM regions or AT and MM interface.

Process and kinetics of bonelike apatite formation on sintered hydroxyapatite in a simulated body fluid.

PubMed

Kim, Hyun-Min; Himeno, Teruyuki; Kokubo, Tadashi; Nakamura, Takashi

2005-07-01

The surfaces of two hydroxyapatites (HA), which have been sintered at different temperatures of 800 and 1200 degrees C, was investigated as a function of soaking time in simulated body fluid (SBF) using transmission electron microscopy (TEM) attached with energy-dispersive spectrometry (EDX) and laser electrophoresis spectroscopy. The TEM-EDX indicated that after soaking in SBF, both the HAs form bonelike apatite by undergoing the same surface structural change, i.e., formations of a Ca-rich amorphous or nano-crystalline calcium phosphate (ACP) and a Ca-poor ACP, which eventually crystallized into bonelike apatite. Zeta potential characterized by the electrophoresis indicated that during exposure to SBF, the HA surfaces reveal negative surface charge, thereby interacting with the positive calcium ions in the fluid to form the Ca-rich ACP, which gains positive surface charge. The Ca-rich ACP on the HAs then interacts with the negative phosphate ions in the fluid to form the Ca-poor ACP, which stabilizes by being crystallized into bonelike apatite with a low solubility in the SBF. The exposure times for formations of these phases of the Ca-rich ACP, the Ca-poor ACP as well as the apatite were, however, all late on HA sintered at 1200 degrees C, compared with the HA sintered at 800 degrees C. This phenomenon was attributed to a lower initial negative surface charge of the HA sintered at 800 degrees C than of that one sintered at 1200 degrees C, owing to poverty in surface hydroxyl and phosphate groups which are responsible for the surface negativity of the HA. These indicate that sintered temperature of HA might influence not in terms of the process but in terms of the rate of formation of biologically active bonelike apatite on its surface, through which the HA integrates with living bone.

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.

3500-hour durability testing of ceramic materials for automotive gas turbine engines

NASA Technical Reports Server (NTRS)

Carruthers, W. D.; Richerson, D. W.; Benn, K. W.

1980-01-01

A two-year durability program was performed by AiResearch Phoenix to evaluate four commercially available ceramic materials under simulated automotive gas turbine combustor discharge conditions. These conditions included extended cyclic thermal exposures up to 2500 F and 3500 hr. The four materials selected for evaluation were Norton NCX-34 hot pressed silicon nitride, AiResearch RBN 101 reaction bonded silicon nitride, Carborundum pressureless sintered alpha-SiC and Pure Carbon Co. (British Nuclear Fuels, Ltd.) Refel reaction sintered silicon carbide. These materials were initially exposed to 350 hr/1750 cycles at 1200 and 1370 C. Subsequent exposures to 1050, 2100 and 3500 hr were performed on those materials maintaining 50% of baseline strength after the initial exposure. Additional evaluations of exposed bars included dimensional and weight changes, dye penetrant, specific damping capacity changes, SEM fractography, and X-ray diffraction.

CALCINATION AND SINTERING MODELS FOR APPLICATION TO HIGH-TEMPERATURE, SHORT-TIME SULFATION OF CALCIUM-BASED SORBENTS

EPA Science Inventory

To simulate the staged availability of transient high surface area CaO observed in high-temperature flow-reactor data, the rate of calcination of CaCO3 or Ca(OH)2 is described by an empirical modification of the shrinking-core model. The physical model depicts particle decomposi...

Needs assessment for nondestructive testing and materials characterization for improved reliability in structural ceramics for heat engines

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

Johnson, D.R.; McClung, R.W.; Janney, M.A.

1987-08-01

A needs assessment was performed for nondestructive testing and materials characterization to achieve improved reliability in ceramic materials for heat engine applications. Raw materials, green state bodies, and sintered ceramics were considered. The overall approach taken to improve reliability of structural ceramics requires key inspections throughout the fabrication flowsheet, including raw materials, greed state, and dense parts. The applications of nondestructive inspection and characterization techniques to ceramic powders and other raw materials, green ceramics, and sintered ceramics are discussed. The current state of inspection technology is reviewed for all identified attributes and stages of a generalized flowsheet for advanced structuralmore » ceramics, and research and development requirements are identified and listed in priority order. 164 refs., 3 figs.« less

Hydrogen Decrepitation Press-Less Process recycling of NdFeB sintered magnets

NASA Astrophysics Data System (ADS)

Xia, Manlong; Abrahamsen, Asger B.; Bahl, Christian R. H.; Veluri, Badrinath; Søegaard, Allan I.; Bøjsøe, Poul

2017-11-01

A Hydrogen Decrepitation Press-Less Process (HD-PLP) recycling method for recycling of anisotropic NdFeB magnets is demonstrated. The method combines hydrogen decrepitation (HD) disintegration of the initial magnet, powder sieving and the Press-Less Process (PLP), where hydride powder is sintered in a graphite mold. Coercivities up to 534 kA/m were obtained in porous samples based on powder size d < 100 μm. Adding a ball milling step resulted in full density isotropic magnets for d > 100 μm. The coercivity reached Hci = 957 kA/m being 86% of the original N48M material without addition of rare earth elements.

Casting of particle-based hollow shapes

DOEpatents

Menchhofer, P.

1997-09-09

A method is disclosed for the production of hollow articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with one aspect of the invention, a thermally settable slurry containing a relatively high concentration of the particles is coated onto a prewarmed continuous surface in a relatively thin layer so that the slurry is substantially uniformly coated on the surface. The heat of the prewarmed surface conducts to the slurry to initiate a reaction which causes the slurry to set or harden in a shape conforming to the surface. The hardened configurations may then be sintered to consolidate the particles and provide a high density product. 9 figs.

Casting of particle-based hollow shapes

DOEpatents

Menchhofer, P.

1995-05-30

A method is disclosed for the production of hollow articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with one aspect of the invention, a thermally settable slurry containing a relatively high concentration of the particles is coated onto a prewarmed continuous surface in a relatively thin layer so that the slurry is substantially uniformly coated on the surface. The heat of the prewarmed surface conducts to the slurry to initiate a reaction which causes the slurry to set or harden in a shape conforming to the surface. The hardened configurations may then be sintered to consolidate the particles and provide a high density product. 9 figs.

Casting of particle-based hollow shapes

DOEpatents

Menchhofer, Paul

1997-01-01

A method for the production of hollow articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with one aspect of the invention, a thermally settable slurry containing a relatively high concentration of the particles is coated onto a prewarmed continuous surface in a relatively thin layer so that the slurry is substantially uniformly coated on the surface. The heat of the prewarmed surface conducts to the slurry to initiate a reaction which causes the slurry to set or harden in a shape conforming to the surface. The hardened configurations may then be sintered to consolidate the particles and provide a high density product.

Casting of particle-based hollow shapes

DOEpatents

Menchhofer, Paul

1995-01-01

A method for the production of hollow articles made of a particle-based material; e.g., ceramics and sintered metals. In accordance with one aspect of the invention, a thermally settable slurry containing a relatively high concentration of the particles is coated onto a prewarmed continuous surface in a relatively thin layer so that the slurry is substantially uniformly coated on the surface. The heat of the prewarmed surface conducts to the slurry to initiate a reaction which causes the slurry to set or harden in a shape conforming to the surface. The hardened configurations may then be sintered to consolidate the particles and provide a high density product.

The investigation of order–disorder transition process of ZSM-5 induced by spark plasma sintering

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

Wang, Liang; Wang, Lianjun, E-mail: wanglj@dhu.edu.cn; Jiang, Wan

2014-04-01

Based on the amorphization of zeolites, an order–disorder transition method was used to prepare silica glass via Spark Plasma Sintering (SPS). In order to get a better understanding about the mechanism of amorphization induced by SPS, the intermediate products in this process were prepared and characterized by different characterization techniques. X-ray diffraction and High-energy synchrotron X-ray scattering show a gradual transformation from ordered crystal to glass. Local structural changes in glass network including Si–O bond length, O–Si–O bond angle, size of rings, coordination were detected by Infrared spectroscopy and {sup 29}Si magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. Topologically ordered,more » amorphous material with a different intermediate-range structure can be obtained by precise control of intermediate process which can be expected to optimize and design material. - Graphical abstract: Low-density, ordered zeolites collapse to the rigid amorphous glass through spark plasma sintering. The intermediate-range structure formed in the process of order–disorder transition may give rise to specific property. - Highlights: • Order–disorder transition process of ZSM-5 induced by spark plasma sintering was investigated using several methods including XRD, High-energy synchrotron X-ray scattering, SAXS, IR, NMR, ect. • Order–disorder transition induced by SPS was compared with TIA and PIA. • Three stages has been divided during the whole process. • The collapse temperature range which may give rise to intermediate-range structure has been located.« less

Wetting Behavior of Calcium Ferrite Slags on Cristobalite Substrates

NASA Astrophysics Data System (ADS)

Yang, Mingrui; Lv, Xuewei; Wei, Ruirui; Xu, Jian; Bai, Chenguang

2018-03-01

Calcium ferrite (CF) is a significant intermediate adhesive phase in high-basicity sinters. The wettability between calcium ferrite (CF) and gangue plays an important role in the assimilation process. The wettability of CF-based slags, in which a constant amount (2 mass pct.) of Al2O3, MgO, SiO2, and TiO2 was added, on solid SiO2 (cristobalite) substrates at 1523 K (1250 °C) was investigated. The interfacial microstructure and spreading mechanisms were discussed for each sample. All the tested slag samples exhibited good wettability on the SiO2 substrate. The initial apparent contact angles were in the range of 20 to 50 deg, while the final apparent contact angles were 5 deg. The wetting process could be divided into three stages on the basis of the change in diameter, namely the "linear spreading" stage, "spreading rate reduction" stage, and "wetting equilibrium" stage. It was found that the CF-SiO2 wetting system exhibits dissolutive wetting and the dissolution of SiO2 into slag influences its spreading process. The spreading rate increases with a decrease in the ratio of viscosity to interfacial tension, which is a result of the addition of Al2O3, MgO, SiO2, and TiO2. After cooling, a deep corrosion pit was formed in the substrate and a diffusion layer was generated in front of the residual slag zone; further, some SiO2 and Fe2O3 solid solutions precipitated in the slag.

Wetting Behavior of Calcium Ferrite Slags on Cristobalite Substrates

NASA Astrophysics Data System (ADS)

Yang, Mingrui; Lv, Xuewei; Wei, Ruirui; Xu, Jian; Bai, Chenguang

2018-06-01

Calcium ferrite (CF) is a significant intermediate adhesive phase in high-basicity sinters. The wettability between calcium ferrite (CF) and gangue plays an important role in the assimilation process. The wettability of CF-based slags, in which a constant amount (2 mass pct.) of Al2O3, MgO, SiO2, and TiO2 was added, on solid SiO2 (cristobalite) substrates at 1523 K (1250 °C) was investigated. The interfacial microstructure and spreading mechanisms were discussed for each sample. All the tested slag samples exhibited good wettability on the SiO2 substrate. The initial apparent contact angles were in the range of 20 to 50 deg, while the final apparent contact angles were 5 deg. The wetting process could be divided into three stages on the basis of the change in diameter, namely the "linear spreading" stage, "spreading rate reduction" stage, and "wetting equilibrium" stage. It was found that the CF-SiO2 wetting system exhibits dissolutive wetting and the dissolution of SiO2 into slag influences its spreading process. The spreading rate increases with a decrease in the ratio of viscosity to interfacial tension, which is a result of the addition of Al2O3, MgO, SiO2, and TiO2. After cooling, a deep corrosion pit was formed in the substrate and a diffusion layer was generated in front of the residual slag zone; further, some SiO2 and Fe2O3 solid solutions precipitated in the slag.

Formation of porous surface layers in reaction bonded silicon nitride during processing

NASA Technical Reports Server (NTRS)

Shaw, N. J.; Glasgow, T. K.

1979-01-01

An effort was undertaken to determine if the formation of the generally observed layer of large porosity adjacent to the as-nitride surfaces of reaction bonded silicon nitrides could be prevented during processing. Isostatically pressed test bars were prepared from wet vibratory milled Si powder. Sintering and nitriding were each done under three different conditions:(1) bars directly exposed to the furnance atmosphere; (2) bars packed in Si powder; (3) bars packed in Si3N4 powder. Packing the bars in either Si of Si3N4 powder during sintering retarded formation of the layer of large porosity. Only packing the bars in Si prevented formation of the layer during nitridation. The strongest bars (316 MPa) were those sintered in Si and nitrided in Si3N4 despite their having a layer of large surface porosity; failure initiated at very large pores and inclusions. The alpha/beta ratio was found to be directly proportional to the oxygen content; a possible explanation for this relationship is discussed.

Osteoblastic cell response to spark plasma-sintered zirconia/titanium cermets.

PubMed

Fernandez-Garcia, Elisa; Guillem-Marti, Jordi; Gutierrez-Gonzalez, Carlos F; Fernandez, Adolfo; Ginebra, Maria-Pau; Lopez-Esteban, Sonia

2015-01-01

Ceramic/metal composites, cermets, arise from the idea to combine the dissimilar properties in the pure materials. This work aims to study the biocompatibility of new micro-nanostructured 3 Y-TZP/Ti materials with 25, 50 and 75 vol.% Ti, which have been successfully obtained by spark slasma sintering technology, as well as to correlate their surface properties (roughness, wettability and chemical composition) with the osteoblastic cell response. All samples had isotropic and slightly waved microstructure, with sub-micrometric average roughness. Composites with 75 vol.% Ti had the highest surface hydrophilicity. Surface chemical composition of the cermets correlated well with the relative amounts used for their fabrication. A cell viability rate over 80% dismissed any cytotoxicity risk due to manufacturing. Cell adhesion and early differentiation were significantly enhanced on materials containing the nanostructured 3 Y-TZP phase. Proliferation and differentiation of SaOS-2 were significantly improved in their late-stage on the composite with 75 vol.% Ti that, from the osseointegration standpoint, is presented as an excellent biomaterial for bone replacement. Thus, spark plasma sintering is consolidated as a suitable technology for manufacturing nanostructured biomaterials with enhanced bioactivity. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

Structural Ceramic Nanocomposites: A Review of Properties and Powders’ Synthesis Methods

PubMed Central

Palmero, Paola

2015-01-01

Ceramic nanocomposites are attracting growing interest, thanks to new processing methods enabling these materials to go from the research laboratory scale to the commercial level. Today, many different types of nanocomposite structures are proposed in the literature; however, to fully exploit their exceptional properties, a deep understanding of the materials’ behavior across length scales is necessary. In fact, knowing how the nanoscale structure influences the bulk properties enables the design of increasingly performing composite materials. A further key point is the ability of tailoring the desired nanostructured features in the sintered composites, a challenging issue requiring a careful control of all stages of manufacturing, from powder synthesis to sintering. This review is divided into four parts. In the first, classification and general issues of nanostructured ceramics are reported. The second provides basic structure–property relations, highlighting the grain-size dependence of the materials properties. The third describes the role of nanocrystalline second-phases on the mechanical properties of ordinary grain sized ceramics. Finally, the fourth part revises the mainly used synthesis routes to produce nanocomposite ceramic powders, underlining when possible the critical role of the synthesis method on the control of microstructure and properties of the sintered ceramics. PMID:28347029

Nanoclay/Polymer Composite Powders for Use in Laser Sintering Applications: Effects of Nanoclay Plasma Treatment

NASA Astrophysics Data System (ADS)

Almansoori, Alaa; Majewski, Candice; Rodenburg, Cornelia

2017-11-01

Plasma-etched nanoclay-reinforced Polyamide 12 (PA12) powder is prepared with its intended use in selective laser sintering (LS) applications. To replicate the LS process we present a downward heat sintering (DHS) process, carried out in a hot press, to fabricate tensile test specimens from the composite powders. The DHS parameters are optimized through hot stage microscopy, which reveal that the etched clay (EC)-based PA12 (EC/PA12) nanocomposite powder melts at a temperature 2°C higher than that of neat PA12, and 1-3°C lower than that of the nonetched clay-based nanocompsite (NEC/PA12 composite). We show that these temperature differences are critical to successful LS. The distribution of EC and NEC onto PA12 is investigated by scanning electron microscopy (SEM). SEM images show clearly that the plasma treatment prevents the micron-scale aggregation of the nanoclay, resulting in an improved elastic modulus of EC/PA12 when compared with neat PA12 and NEC/PA12. Moreover, the reduction in elongation at break for EC/PA12 is less pronounced than for NEC/PA12.

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Microwave processed NiMg ferrite: Studies on structural and magnetic properties

NASA Astrophysics Data System (ADS)

Chandra Babu Naidu, K.; Madhuri, W.

2016-12-01

Ferrites are magnetic semiconductors realizing an important role in electrical and electronic circuits where electrical and magnetic property coupling is required. Though ferrite materials are known for a long time, there is a large scope in the improvement of their properties (vice sintering and frequency dependence of electrical and magnetic properties) with the current technological trends. Forth coming technology is aimed at miniaturization and smart gadgets, electrical components like inductors and transformers cannot be included in integrated circuits. These components are incorporated into the circuit as surface mount devices whose fabrication involves low temperature co-firing of ceramics and microwave monolithic integrated circuits technologies. These technologies demand low temperature sinter-ability of ferrites. This article presents low temperature microwave sintered Ni-Mg ferrites of general chemical formula Ni1-xMgxFe2O4 (x=0, 0.2, 0.4, 0.5, 0.6, 0.8, 1) for potential applications as transformer core materials. The series of ferrites are characterized using X-ray diffractometer, scanning electron microscopy, Fourier transform infrared and vibrating sample magnetometer for investigating structural, morphological and magnetic properties respectively. The initial permeability is studied with magnesium content, temperature and frequency in the temperature range of 308 K-873 K and 42 Hz-5 MHz.

Small angle X-ray scattering analysis of the effect of cold compaction of Al/MoO3 thermite composites.

PubMed

Hammons, Joshua A; Wang, Wei; Ilavsky, Jan; Pantoya, Michelle L; Weeks, Brandon L; Vaughn, Mark W

2008-01-07

Nanothermites composed of aluminum and molybdenum trioxide (MoO(3)) have a high energy density and are attractive energetic materials. To enhance the surface contact between the spherical Al nanoparticles and the sheet-like MoO(3) particles, the mixture can be cold-pressed into a pelleted composite. However, it was found that the burn rate of the pellets decreased as the density of the pellets increased, contrary to expectation. Ultra-small angle X-ray scattering (USAXS) data and scanning electron microscopy (SEM) were used to elucidate the internal structure of the Al nanoparticles, and nanoparticle aggregate in the composite. Results from both SEM imaging and USAXS analysis indicate that as the density of the pellet increased, a fraction of the Al nanoparticles are compressed into sintered aggregates. The sintered Al nanoparticles lost contrast after forming the larger aggregates and no longer scattered X-rays as individual particles. The sintered aggregates hinder the burn rate, since the Al nanoparticles that make them up can no longer diffuse freely as individual particles during combustion. Results suggest a qualitative relationship for the probability that nanoparticles will sinter, based on the particle sizes and the initial structure of their respective agglomerates, as characterized by the mass fractal dimension.

Tritium release from neutron-irradiated Li 2O sintered pellets: porosity dependence

NASA Astrophysics Data System (ADS)

Tanifuji, Takaaki; Yamaki, Daiju; Takahashi, Tadashi; Iwamoto, Akira

2000-12-01

The tritium release behaviour from sintered Li 2O pellets of various densities (71-98.5% theoretical density, T.D.) has been investigated by heating tests at a constant rate. It is shown that the tritium release rate depends on porosity at densities above 87% T.D., while no dependence was observed at densities below 86% T.D. The tritium release process is thought to consist of three stages described as follows: (1) the liberation of tritium trapped at point defects due to their recovery (peak at around 570 K); (2) the advection through interconnected pores via adsorption and desorption on their inner walls and diffusion in the gas phase of interconnected pores (peak at around 620 K); (3) the dissolution and release of tritium trapped in closed pores (peaks at around 700, 830 and 1000 K).

Dental implant customization using numerical optimization design and 3-dimensional printing fabrication of zirconia ceramic.

PubMed

Cheng, Yung-Chang; Lin, Deng-Huei; Jiang, Cho-Pei; Lin, Yuan-Min

2017-05-01

This study proposes a new methodology for dental implant customization consisting of numerical geometric optimization and 3-dimensional printing fabrication of zirconia ceramic. In the numerical modeling, exogenous factors for implant shape include the thread pitch, thread depth, maximal diameter of implant neck, and body size. Endogenous factors are bone density, cortical bone thickness, and non-osseointegration. An integration procedure, including uniform design method, Kriging interpolation and genetic algorithm, is applied to optimize the geometry of dental implants. The threshold of minimal micromotion for optimization evaluation was 100 μm. The optimized model is imported to the 3-dimensional slurry printer to fabricate the zirconia green body (powder is bonded by polymer weakly) of the implant. The sintered implant is obtained using a 2-stage sintering process. Twelve models are constructed according to uniform design method and simulated the micromotion behavior using finite element modeling. The result of uniform design models yields a set of exogenous factors that can provide the minimal micromotion (30.61 μm), as a suitable model. Kriging interpolation and genetic algorithm modified the exogenous factor of the suitable model, resulting in 27.11 μm as an optimization model. Experimental results show that the 3-dimensional slurry printer successfully fabricated the green body of the optimization model, but the accuracy of sintered part still needs to be improved. In addition, the scanning electron microscopy morphology is a stabilized t-phase microstructure, and the average compressive strength of the sintered part is 632.1 MPa. Copyright © 2016 John Wiley & Sons, Ltd.

Evaluation of suitable porosity for sintered porous {beta}-tricalcium phosphate as a bone substitute

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

Park, Jin-Hong; Bae, Ji-Yong; Shim, Jaebum

2012-09-15

Structural and mechanical characterization is performed for sintered porous beta tricalcium phosphate ({beta}-TCP) to determine the appropriate porosity for use as a bone substitute. Four different types of porous {beta}-TCP specimen with different porosities are fabricated through a sintering process. For structural characterization, scanning electron microscopy and a Microfocus X-ray computed tomography system are used to investigate the pore openings on the specimen's surface, pore size, pore distribution, and pore interconnections. Compression tests of the specimens are performed, and mechanical properties such as the elastic modulus and compressive strength are obtained. Also, the geometric shape and volume of the {beta}-TCPmore » around the contact region of two pores, which need to be initially resolved after implantation in order to increase the size of the pore openings, are evaluated through simple calculations. The results show that porous {beta}-TCP with 42.1% porosity may be a suitable bone substitute candidate in terms of sustaining external loads, and inducing and cultivating bone cells. - Highlights: Black-Right-Pointing-Pointer Structural and mechanical characterization was performed for sintered porous {beta}-TCP specimens. Black-Right-Pointing-Pointer For structural characterization, SEM and Microfocus X-ray CT system were used. Black-Right-Pointing-Pointer For mechanical characterization, compression tests were performed. Black-Right-Pointing-Pointer Porous {beta}-TCP with 42.1% porosity may be a suitable bone substitute.« less

40 CFR 63.7824 - What test methods and other procedures must I use to establish and demonstrate initial compliance...

Code of Federal Regulations, 2013 CFR

2013-07-01

... sinter produced (tons/day). (3) Compute the process-weighted mass emissions (Ev) each day using Equation 1 of this section as follows: ER20MY03.002 Where: Ev = Process-weighted mass emissions of volatile...

Thermal Stability of Silver Paste Sintering on Coated Copper and Aluminum Substrates

NASA Astrophysics Data System (ADS)

Pei, Chun; Chen, Chuantong; Suganuma, Katsuaki; Fu, Guicui

2018-01-01

The thermal stability of silver (Ag) paste sintering on coated copper (Cu) and aluminum (Al) substrates has been investigated. Instead of conventional zincating or nickel plating, magnetron sputtering was used to achieve coating with titanium (Ti) and Ag. Silicon (Si) chips were bonded to coated Cu and Al substrates using a mixture of submicron Ag flakes and particles under 250°C and 0.4 MPa for 30 min. The joints were then subject to aging testing at 250°C for duration of 200 h, 500 h, and 1000 h. Two types of joints exhibited satisfactory initial shear strength above 45 MPa. However, the shear strength of the joints on Al substrate decreased to 28 MPa after 1000 h of aging, while no shear strength decline was detected for the joints on Cu substrate. Fracture surface analysis revealed that the vulnerable points of the two types of joints were (1) the Ag layer and (2) the interface between the Ti layer and Cu substrate. Based on the results of scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDS), and simulations, cracks in the Ag layer were identified as the cause of the shear strength degradation in the joints on Al substrate. The interface evolution of the joints on Cu substrate was ascribed to Cu migration and discontinuity points that initialized in the Ti layer. This study reveals that Al exhibited superior thermal stability with sintered Ag paste.

Copper stabilization via spinel formation during the sintering of simulated copper-laden sludge with aluminum-rich ceramic precursors.

PubMed

Tang, Yuanyuan; Chui, Stephen Sin-Yin; Shih, Kaimin; Zhang, Lingru

2011-04-15

The feasibility of incorporating copper-laden sludge into low-cost ceramic products, such as construction ceramics, was investigated by sintering simulated copper-laden sludge with four aluminum-rich ceramic precursors. The results indicated that all of these precursors (γ-Al(2)O(3), corundum, kaolinite, mullite) could crystallochemically stabilize the hazardous copper in the more durable copper aluminate spinel (CuAl(2)O(4)) structure. To simulate the process of copper transformation into a spinel structure, CuO was mixed with the four aluminum-rich precursors, and fired at 650-1150 °C for 3 h. The products were examined using powder X-ray diffraction (XRD) and scanning electron microscopic techniques. The efficiency of copper transformation among crystalline phases was quantitatively determined through Rietveld refinement analysis of the XRD data. The sintering experiment revealed that the optimal sintering temperature for CuAl(2)O(4) formation was around 1000 °C and that the efficiency of copper incorporation into the crystalline CuAl(2)O(4) structure after 3 h of sintering ranged from 40 to 95%, depending on the type of aluminum precursor used. Prolonged leaching tests were carried out by using acetic acid with an initial pH value of 2.9 to leach CuO and CuAl(2)O(4) samples for 22 d. The sample leachability analysis revealed that the CuAl(2)O(4) spinel structure was more superior to stabilize copper, and suggested a promising and reliable technique for incorporating copper-laden sludge or its incineration ash into usable ceramic products. Such results also demonstrated the potential of a waste-to-resource strategy by using waste materials as part of the raw materials with the attainable temperature range used in the production of ceramics.

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

PubMed

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

2013-08-06

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

Role of oxygen on microstructure and thermoelectric properties of silicon nanocomposites

NASA Astrophysics Data System (ADS)

Schierning, G.; Theissmann, R.; Stein, N.; Petermann, N.; Becker, A.; Engenhorst, M.; Kessler, V.; Geller, M.; Beckel, A.; Wiggers, H.; Schmechel, R.

2011-12-01

Phosphorus-doped silicon nanopowder from a gas phase process was compacted by DC-current sintering in order to obtain thermoelectrically active, nanocrystalline bulk silicon. A density between 95% and 96% compared to the density of single crystalline silicon was achieved, while preserving the nanocrystalline character with an average crystallite size of best 25 nm. As a native surface oxidation of the nanopowder usually occurs during nanopowder handling, a focus of this work is on the role of oxygen on microstructure and transport properties of the nanocomposite. A characterization with transmission electron microscopy (TEM) showed that the original core/shell structure of the nanoparticles was not found within the sintered nanocomposites. Two different types of oxide precipitates could be identified by energy filtered imaging technique. For a detailed analysis, 3-dimensional tomography with reconstruction was done using a needle-shaped sample prepared by focused ion beam (FIB). The 3-dimensional distribution of silicon dioxide precipitates confirmed that the initial core/shell structure breaks down and precipitates are formed. It is further found that residual pores are exclusively located within oxide precipitates. Thermoelectric characterization was done on silicon nanocomposites sintered between 960 °C and 1060 °C with varying oxygen content between room temperature and 950 °C. The higher sintering temperature led to a better electrical activation of the phosphorus dopant. The oxidic precipitates support densification and seem to be able to reduce the thermal conductivity therefore enhancing thermoelectric properties. A peak figure of merit, zT, of 0.5 at 950 °C was measured for a sample sintered at 1060 °C with a mean crystallite size of 46 nm.

Strength and fracture mechanism of iron reinforced tricalcium phosphate cermet fabricated by spark plasma sintering.

PubMed

Tkachenko, Serhii; Horynová, Miroslava; Casas-Luna, Mariano; Diaz-de-la-Torre, Sebastian; Dvořák, Karel; Celko, Ladislav; Kaiser, Jozef; Montufar, Edgar B

2018-05-01

The present work studies the microstructure and mechanical performance of tricalcium phosphate (TCP) based cermet toughened by iron particles. A novelty arises by the employment of spark plasma sintering for fabrication of the cermet. Results showed partial transformation of initial alpha TCP matrix to beta phase and the absence of oxidation of iron particles, as well as a lack of chemical reaction between TCP and iron components during sintering. The values of compressive and tensile strength of TCP/Fe cermet were 3.2 and 2.5 times, respectively, greater than those of monolithic TCP. Fracture analysis revealed the simultaneous action of crack-bridging and crack-deflection microstructural toughening mechanisms under compression. In contrast, under tension the reinforcing mechanism was only crack-bridging, being the reason for smaller increment of strength. Elastic properties of the cermet better matched values reported for human cortical bone. Thereby the new TCP/Fe cermet has potential for eventual use as a material for bone fractures fixation under load-bearing conditions. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

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

Plucknett, K.P.; Tiegs, T.N.; Becher, P.F.

Ductile Ni{sub 3}Al alloys have been used as binder phase for fabrication of TiC and WC matrix composites. Ni{sub 3}Al has good corrosion resistance to aqueous acidic environments, and its yield strength increases with temperature to a max at 700-800 C; this combined with high tensile ductilities (up to 50% strain) make Ni{sub 3}Al attractive for replacing Co in cemented carbides. Materials have been fabricated by both hot pressing and vacuum sintering, with Ni{sub 3}Al contents of 15 to 95 vol%. Vacuum sintering cycles, similar to those used for WC/Co and TiC/Ni (1450-1600 C), resulted in sintered densities >95% theoretical.more » WC/Ni{sub 3}Al materials showed an order of magnitude improvement in corrosion resistance over WC/Co, in sulfuric/nitric acid. These materials also had improved high temperature strength retention compared to WC/Co cermets, though initial RT strengths were lower. Fracture toughness varied between 8 and 25 MPa.m{sup 1/2} and depended primarily on Ni{sub 3}Al content and composition.« less

Static capacity model for sealed nickel cadmium cells

NASA Astrophysics Data System (ADS)

Lomaniec, Jacob

1989-04-01

A model was developed for calculating the capacity of nickel cadmium rechargeable sealed cells. The model applies only to the following operating conditions for a cell of capacity C ampere-hours: Temperature of 20 + or - 5 C; charging for 16 hr, at 0.1 C amp; discharging at 0.2 C amp until the terminal voltage falls to 1.0 V. The study considers the dimensional and quantitative relationships among the cell's chemical and mechanical components, and the application of these relationships to optimizing cell design in terms of energy density and electrical performance. The model comprises several components, representing the several stages of the manufacturing process: assembling the electrodes and separator in a cylindrical can; production of porous, sintered nickel plaque on a perforated steel substrate; impregnating the plaque with active material; oxidation of the sintered nickel during impregnation; insertion and concentration of the electrolyte solution. Results from the model were compared with those obtained from cells manufactured during a long period. Good agreement was obtained. The models were used in the plant, to define the operating parameters of various production stages and contributed to a general improvement in product quality. The models were also applied to the optimization of new cell designs, and reduction of development costs by the elimination of much experimental work.

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

Sintering behavior of U 80 at.%Zr powder compacts in a vacuum environment

NASA Astrophysics Data System (ADS)

Kim, Tae-Kyu; Lee, Chong-Tak; Sohn, Dong-Seong

2008-01-01

Sintering behavior of U-80 at.%Zr powder compacts in a temperature range from 1100 to 1500 °C in a vacuum of 1 × 10 -4 Pa was evaluated. The sintered density depended more on the sintering temperature than on the sintering time. The sintered specimens consisted of the δ-UZr 2 matrix with acicular α-Zr precipitates, but it still had un-reacted zirconium when the sintering temperature was 1100 °C. The uranium depletion near the surface of the specimens sintered at temperatures above 1300 °C was detected. Massive Zr(O) grains in the sintered specimen were found, and their formation was restrained when the cooling rate from the sintering temperature was increased.

[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.

[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.

[Influence on microstructure of dental zirconia ceramics prepared by two-step sintering].

PubMed

Jian, Chao; Li, Ning; Wu, Zhikai; Teng, Jing; Yan, Jiazhen

2013-10-01

To investigate the microstructure of dental zirconia ceramics prepared by two-step sintering. Nanostructured zirconia powder was dry compacted, cold isostatic pressed, and pre-sintered. The pre-sintered discs were cut processed into samples. Conventional sintering, single-step sintering, and two-step sintering were carried out, and density and grain size of the samples were measured. Afterward, T1 and/or T2 of two-step sintering ranges were measured. Effects on microstructure of different routes, which consisted of two-step sintering and conventional sintering were discussed. The influence of T1 and/or T2 on density and grain size were analyzed as well. The range of T1 was between 1450 degrees C and 1550 degrees C, and the range of T2 was between 1250 degrees C and 1350 degrees C. Compared with conventional sintering, finer microstructure of higher density and smaller grain could be obtained by two-step sintering. Grain growth was dependent on T1, whereas density was not much related with T1. However, density was dependent on T2, and grain size was minimally influenced. Two-step sintering could ensure a sintering body with high density and small grain, which is good for optimizing the microstructure of dental zirconia ceramics.

A Study on the Mechanical Properties and Impact-Induced Initiation Characteristics of Brittle PTFE/Al/W Reactive Materials.

PubMed

Ge, Chao; Maimaitituersun, Wubuliaisan; Dong, Yongxiang; Tian, Chao

2017-04-26

Polytetrafluoroethylene/aluminum/tungsten (PTFE/Al/W) reactive materials of three different component mass ratios (73.5/26.5/0, 68.8/24.2/7 and 63.6/22.4/14) were studied in this research. Different from the PTFE/Al/W composites published elsewhere, the materials in our research were fabricated under a much lower sintering temperature and for a much shorter duration to achieve a brittle property, which aims to provide more sufficient energy release upon impact. Quasi-static compression tests, dynamic compression tests at room and elevated temperatures, and drop weight tests were conducted to evaluate the mechanical and impact-induced initiation characteristics of the materials. The materials before and after compression tests were observed by a scanning electron microscope to relate the mesoscale structural characteristics to their macro properties. All the three types of materials fail at very low strains during both quasi-static and dynamic compression. The stress-strain curves for quasi-static tests show obvious deviations while that for the dynamic tests consist of only linear-elastic and failure stages typically. The materials were also found to exhibit thermal softening at elevated temperatures and were strain-rate sensitive during dynamic tests, which were compared using dynamic increase factors (DIFs). Drop-weight test results show that the impact-initiation sensitivity increases with the increase of W content due to the brittle mechanical property. The high-speed video sequences and recovered sample residues of the drop-weight tests show that the reaction is initiated at two opposite positions near the edges of the samples, where the shear force concentrates the most intensively, indicating a shear-induced initiation mechanism.

A Study on the Mechanical Properties and Impact-Induced Initiation Characteristics of Brittle PTFE/Al/W Reactive Materials

PubMed Central

Ge, Chao; Maimaitituersun, Wubuliaisan; Dong, Yongxiang; Tian, Chao

2017-01-01

Polytetrafluoroethylene/aluminum/tungsten (PTFE/Al/W) reactive materials of three different component mass ratios (73.5/26.5/0, 68.8/24.2/7 and 63.6/22.4/14) were studied in this research. Different from the PTFE/Al/W composites published elsewhere, the materials in our research were fabricated under a much lower sintering temperature and for a much shorter duration to achieve a brittle property, which aims to provide more sufficient energy release upon impact. Quasi-static compression tests, dynamic compression tests at room and elevated temperatures, and drop weight tests were conducted to evaluate the mechanical and impact-induced initiation characteristics of the materials. The materials before and after compression tests were observed by a scanning electron microscope to relate the mesoscale structural characteristics to their macro properties. All the three types of materials fail at very low strains during both quasi-static and dynamic compression. The stress-strain curves for quasi-static tests show obvious deviations while that for the dynamic tests consist of only linear-elastic and failure stages typically. The materials were also found to exhibit thermal softening at elevated temperatures and were strain-rate sensitive during dynamic tests, which were compared using dynamic increase factors (DIFs). Drop-weight test results show that the impact-initiation sensitivity increases with the increase of W content due to the brittle mechanical property. The high-speed video sequences and recovered sample residues of the drop-weight tests show that the reaction is initiated at two opposite positions near the edges of the samples, where the shear force concentrates the most intensively, indicating a shear-induced initiation mechanism. PMID:28772812

Processing and characterization of boron carbide-hafnium diboride ceramics

NASA Astrophysics Data System (ADS)

Brown-Shaklee, Harlan James

Hafnium diboride based ceramics are promising candidate materials for advanced aerospace and nuclear reactor components. The effectiveness of boron carbide and carbon as HfB2 sintering additives was systematically evaluated. In the first stage of the research, boron carbide and carbon additives were found to improve the densification behavior of milled HfB2 powder in part by removing oxides at the HfB2 surface during processing. Boron carbide additives reduced the hot pressing temperature of HfB2 by 150°C compared to carbon, which reduced the hot pressing temperature by ˜50°C. Reduction of oxide impurities alone could not explain the difference in sintering enhancement, however, and other mechanisms of enhancement were evaluated. Boron carbides throughout the homogeneity range were characterized to understand other mechanisms of sintering enhancement in HfB2. Heavily faulted carbon rich and boron rich boron carbides were synthesized for addition to HfB2. The greatest enhancement to densification was observed in samples containing boron- and carbon-rich compositions whereas B6.5 C provided the least enhancement to densification. It is proposed that carbon rich and boron rich boron carbides create boron and hafnium point defects in HfB2, respectively, which facilitate densification. Evaluation of the thermal conductivity (kth) between room temperature and 2000°C suggested that the stoichiometry of the boron carbide additives did not significantly affect kth of HfB2-BxC composites. The improved sinterability and the high kth (˜110 W/m-K at 300K and ˜90 W/m-K at 1000°C ) of HfB2-BxC ceramics make them excellent candidates for isotopically enriched reactor control materials.

Basaltic maar-diatreme volcanism in the Lower Carboniferous of the Limerick Basin (SW Ireland)

NASA Astrophysics Data System (ADS)

Elliott, H. A. L.; Gernon, T. M.; Roberts, S.; Hewson, C.

2015-05-01

Lead-zinc exploration drilling within the Limerick Basin (SW Ireland) has revealed the deep internal architecture and extra-crater deposits of five alkali-basaltic maar-diatremes. These were emplaced as part of a regional north-east south-west tectonomagmatic trend during the Lower Carboniferous Period. Field relationships and textural observations suggest that the diatremes erupted into a shallow submarine environment. Limerick trace element data indicates a genetic relationship between the diatremes and extra-crater successions of the Knockroe Formation, which records multiple diatreme filling and emptying cycles. Deposition was controlled largely by bathymetry defined by the surrounding Waulsortian carbonate mounds. An initial non-diatreme forming eruption stage occurred at the water-sediment interface, with magma-water interaction prevented by high magma ascent rates. This was followed by seawater incursion and the onset of phreatomagmatic activity. Magma-water interaction generated poorly vesicular blocky clasts, although the co-occurrence of plastically deformed and highly vesicular clasts indicate that phreatomagmatic and magmatic processes were not mutually exclusive. At a later stage, the diatreme filled with a slurry of juvenile lapilli and country rock lithic clasts, homogenised by the action of debris jets. The resulting extra-crater deposits eventually emerged above sea level, so that water ingress significantly declined, and late-stage magmatic processes became dominant. These deposits, largely confined to the deep vents, incorporate high concentrations of partially sintered globular and large `raggy' lapilli showing evidence for heat retention. Our study provides new insights into the dynamics and evolution of basaltic diatremes erupting into a shallow water (20-120 m) submarine environment.

Effects of High-Temperature Preoxidation on the Titanomagnetite Ore Structure and Reduction Behaviors in Fluidized Bed

NASA Astrophysics Data System (ADS)

Sun, Haoyan; Adetoro, Ajala Adewole; Pan, Feng; Wang, Zhen; Zhu, Qingshan

2017-06-01

The oxidation behaviors of South Africa (SA) titanomagnetite (TTM) and its effects on the gas solid reduction in the fluidized bed were investigated on the basis of the two-stage short process of direct reduction-electric arc furnace (DR-EAF) melting separation. The results showed that the oxidation phase transformations in the high-temperature range from 1073 K to 1223 K (800 °C to 950 °C) can be divided into two typical processes: with the fast generation of pseudobrookite and with the maghemite generation at the initial stage. The reduction efficiency for SA TTM was improved by the preoxidation treatment, mainly because of the dissociation of titania-ferrous oxides to the easy reducible hematite. However, at a preoxidation temperature higher than 1173 K (900 °C), the improving effect became weak, due to high-temperature sintering and the larger crystallite size of oxidation products. There is an extreme value of the preoxidation influence, and the optimum preoxidation time is different for various temperatures. The reduction metallization degree of SA TTM can be relatively improved by 14.5 and 4.5 pct for the first and second reduction steps, respectively, by 1173 K (900 °C) preoxidation with an optimum time of 30 minutes. Finally, the equilibrium relationship between the metallization degree and the gas reduction potential for TTM ore with preoxidation treatment was built.

Recent Advances and Research Status in Energy Conservation of Iron Ore Sintering in China

NASA Astrophysics Data System (ADS)

Wang, Yao-Zu; Zhang, Jian-Liang; Liu, Zheng-Jian; Du, Cheng-Bo

2017-11-01

For the ferrous burden of blast furnaces in China, sinter generally accounts for more than 70% and the sintering process accounts for approximately 6-10% of the total energy consumption of the iron and steel enterprise. Therefore, saving energy during the sintering process is important to reduce the energy consumption in the iron and steel industry. This paper aims to illustrate recent advances and the research status of energy conservation of iron ore sintering in China. It focuses on the development and application of energy-saving technologies such as the composite agglomeration process, sintering with high-proportion flue gas recirculation sintering, recovery of sensible heat from the sinter cooling process, homogeneous deep-bed sintering technology, and comprehensive treatment technology of leakage of sintering. Moreover, some suggestions for the future development of energy-saving technologies are put forward.

Sintered bentonite ceramics for the immobilization of cesium- and strontium-bearing radioactive waste

NASA Astrophysics Data System (ADS)

Ortega, Luis Humberto

The Advanced Fuel Cycle Initiative (AFCI) is a Department of Energy (DOE) program, that has been investigating technologies to improve fuel cycle sustainability and proliferation resistance. One of the program's goals is to reduce the amount of radioactive waste requiring repository disposal. Cesium and strontium are two primary heat sources during the first 300 years of spent nuclear fuel's decay, specifically isotopes Cs-137 and Sr-90. Removal of these isotopes from spent nuclear fuel will reduce the activity of the bulk spent fuel, reducing the heat given off by the waste. Once the cesium and strontium are separated from the bulk of the spent nuclear fuel, the isotopes must be immobilized. This study is focused on a method to immobilize a cesium- and strontium-bearing radioactive liquid waste stream. While there are various schemes to remove these isotopes from spent fuel, this study has focused on a nitric acid based liquid waste. The waste liquid was mixed with the bentonite, dried then sintered. To be effective sintering temperatures from 1100 to 1200°C were required, and waste concentrations must be at least 25 wt%. The product is a leach resistant ceramic solid with the waste elements embedded within alumino-silicates and a silicon rich phase. The cesium is primarily incorporated into pollucite and the strontium into a monoclinic feldspar. The simulated waste was prepared from nitrate salts of stable ions. These ions were limited to cesium, strontium, barium and rubidium. Barium and rubidium will be co-extracted during separation due to similar chemical properties to cesium and strontium. The waste liquid was added to the bentonite clay incrementally with drying steps between each addition. The dry powder was pressed and then sintered at various temperatures. The maximum loading tested is 32 wt. percent waste, which refers to 13.9 wt. percent cesium, 12.2 wt. percent barium, 4.1 wt. percent strontium, and 2.0 wt. percent rubidium. Lower loadings of waste were also tested. The final solid product was a hard dense ceramic with a density that varied from 2.12 g/cm3 for a 19% waste loading with a 1200°C sintering temperature to 3.03 g/cm 3 with a 29% waste loading and sintered at 1100°C. Differential Scanning Calorimetry and Thermal Gravimetric Analysis (DSC-TGA) of the loaded bentonite displayed mass loss steps which were consistent with water losses in pure bentonite. Water losses were complete after dehydroxylation at ˜650°C. No mass losses were evident beyond the dehydroxylation. The ceramic melts at temperatures greater than 1300°C. Light flash analysis found heat capacities of the ceramic to be comparable to those of strontium and barium feldspars as well as pollucite. Thermal conductivity improved with higher sintering temperatures, attributed to lower porosity. Porosity was minimized in 1200°C sinterings. Ceramics with waste loadings less than 25 wt% displayed slump, the lowest waste loading, 15 wt% bloated at a 1200°C sintering. Waste loading above 25 wt% produced smooth uniform ceramics when sintered >1100°C. Sintered bentonite may provide a simple alternative to vitrification and other engineered radioactive waste-forms.

Effect of sintering process on the magnetic and mechanical properties of sintered Nd-Fe-B magnets

NASA Astrophysics Data System (ADS)

Hu, Z. H.; Qu, H. J.; Zhao, J. Q.; Yan, C. J.; Liu, X. M.

2014-11-01

The magnetic and mechanical properties of sintered Nd-Fe-B magnets prepared by different sintering processes were investigated. The results showed that the intrinsic coercivity and fracture toughness of sintered Nd-Fe-B magnets first increased, and then declined with increasing annealing temperature. The optimum magnetic properties and fracture toughness of sintered Nd-Fe-B magnets were obtained at the annealing temperature of 540 °C. Sintering temperature increasing from 1047 °C to 1071 °C had hardly effect on the magnetic properties of sintered Nd-Fe-B magnets. The variation of Vickers hardness and fracture toughness was not the same with increasing sintering temperature, and the effect of sintering temperature on the mechanical properties was complex and irregular. The reasons for the variation on magnetic and mechanical properties were analyzed, and we presumed that the effect of microstructure on the mechanical properties was more sensitive than the magnetic properties through analyzing the microstructure of sintered Nd-Fe-B magnets.

New materials through a variety of sintering methods

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

The sintered microsphere matrix for bone tissue engineering: in vitro osteoconductivity studies.

PubMed

Borden, Mark; Attawia, Mohamed; Laurencin, Cato T

2002-09-05

A tissue engineering approach has been used to design three-dimensional synthetic matrices for bone repair. The osteoconductivity and degradation profile of a novel polymeric bone-graft substitute was evaluated in an in vitro setting. Using the copolymer poly(lactide-co-glycolide) [PLAGA], a sintering technique based on microsphere technology was used to fabricate three-dimensional porous scaffolds for bone regeneration. Osteoblasts and fibroblasts were seeded onto a 50:50 PLAGA scaffold. Morphologic evaluation through scanning electron microscopy demonstrated that both cell types attached and spread over the scaffold. Cells migrated through the matrix using cytoplasmic extensions to bridge the structure. Cross-sectional images indicated that cellular proliferation had penetrated into the matrix approximately 700 microm from the surface. Examination of the surfaces of cell/matrix constructs demonstrated that cellular proliferation had encompassed the pores of the matrix by 14 days of cell culture. With the aim of optimizing polymer composition and polymer molecular weight, a degradation study was conducted utilizing the matrix. The results demonstrate that degradation of the sintered matrix is dependent on molecular weight, copolymer ratio, and pore volume. From this data, it was determined that 75:25 PLAGA with an initial molecular weight of 100,000 has an optimal degradation profile. These studies show that the sintered microsphere matrix has an osteoconductive structure capable of functioning as a cellular scaffold with a degradation profile suitable for bone regeneration. Copyright 2002 Wiley Periodicals, Inc.

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

Rager, Matthew S.; Aytug, Tolga; Veith, Gabriel M.

The developing field of printed electronics nanoparticle based inks such as CuO show great promise as a low-cost alternative to other metal-based counterparts (e.g., silver). In particular, CuO inks significantly eliminate the issue of particle oxidation, before and during the sintering process, that is prevalent in Cu-based formulations. We report here the scalable and low-thermal budget photonic fabrication of Cu interconnects employing a roll-to-roll compatible pulse-thermal-processing (PTP) technique that enables phase reduction and subsequent sintering of inkjet-printed CuO patterns onto flexible polymer templates. Detailed investigations of curing and sintering conditions were performed to understand the impact of PTP system conditionsmore » on the electrical performance of the Cu patterns. Specifically, the impact of energy and power of photonic pulses on print conductivity was systematically studied by varying the following key processing parameters: pulse intensity, duration and sequence. Through optimization of such parameters, highly conductive prints in < 1 s with resistivity values as low as 100 n m has been achieved. We also observed that the introduction of an initial ink-drying step in ambient atmosphere, after the printing and before sintering, leads to significant improvements in mechanical integrity and electrical performance of the printed Cu patterns. Moreover, the viability of CuO reactive inks, coupled with the PTP technology and pre ink-drying protocols, has also been demonstrated for the additive integration of a low-cost Cu temperature sensor onto a flexible polymer substrate.« less

Sintering in Ceramics and Solid Oxide Fuel Cells

NASA Astrophysics Data System (ADS)

Hunt, Clay Dale

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

78 FR 42974 - Certain Sintered Rare Earth Magnets, Methods of Making Same and Products Containing Same...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-07-18

... rare earth magnets, methods of making same and products containing same by reason of infringement of..., Methods of Making Same and Products Containing Same; Commission Determination Not to Review an Initial Determination Granting an Unopposed Motion by Complainants; Termination of the Investigation AGENCY: U.S...

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

NASA Astrophysics Data System (ADS)

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

2014-10-01

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

Relation between the microstructure and the electromagnetic properties of BaTiO3/Ni0.5Zn0.5Fe2O4 ceramic composite

NASA Astrophysics Data System (ADS)

Xiao, Bin; Tang, Yu; Ma, Guodong; Ma, Ning; Du, Piyi

2015-06-01

The microstructure-property relation in ferroelectric/ferromagnetic composite is investigated in detail, exemplified by typical sol-gel-derived 0.3BTO/0.7NZFO ceramic composite. The effect of microstructural factors including intergrain connectivity, grain size and interfaces on the dielectric and magnetic properties of the composite prepared by conventional ceramic method and three-step sintering method is discussed both experimentally and theoretically. It reveals that the dielectric behavior of the composite is controlled by a hybrid dielectric process that combines the contribution of Debye-like dipoles and Maxwell-Wagner (M-W or interfacial) polarization. Enhanced dielectric, magnetic and conductive behaviors appear in the composite with better intergrain connectivity and larger grain size derived by sol-gel route and three-step sintering method. The effective permittivity contributed by Debye-like dipoles exhibits a value of ~130,000 in three-step sintered composite, which is almost the same as that in conventionally sintered one, but that contributed by M-W response is much smaller in the former. Compared with conventionally prepared samples, the relaxation time ( τ) is 3.476 × 10-6 s, about one order of magnitude smaller, and the dc electrical conductivity is 3.890 × 10-3 S/m, one order of magnitude higher in three-step sintered composite. The minimum dielectric loss reveals almost the same (~0.2) for all samples, but shows distinguishable difference in low-frequency region. Meanwhile, an initial permeability of 84, twice as large as that of conventionally prepared composite and 56 % the value of single-phased NZFO ferrite (~150), and a saturation magnetization of 63.5 emu/g, 32 % higher than that of conventional one and approximately 84 % the value of single-phased NZFO ferrite (~76 emu/g), appear simultaneously in three-step sintered composite with larger grain size and better intergrain connectivity. It is clear that the discovery is helpful for establishing a more explicit view on the physics of multi-functional composite materials, while the composite with optimized microstructure is beneficial to be used as a high-performance material.

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

NASA Astrophysics Data System (ADS)

Yu, Peng

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

Formation of Aluminum Particles with Shell Morphology during Pressureless Spark Plasma Sintering of Fe–Al Mixtures: Current-Related or Kirkendall Effect?

PubMed Central

Dudina, Dina V.; Bokhonov, Boris B.; Mukherjee, Amiya K.

2016-01-01

A need to deeper understand the influence of electric current on the structure and properties of metallic materials consolidated by Spark Plasma Sintering (SPS) stimulates research on inter-particle interactions, bonding and necking processes in low-pressure or pressureless conditions as favoring technique-specific local effects when electric current passes through the underdeveloped inter-particle contacts. Until now, inter-particle interactions during pressureless SPS have been studied mainly for particles of the same material. In this work, we focused on the interactions between particles of dissimilar materials in mixtures of micrometer-sized Fe and Al powders forming porous compacts during pressureless SPS at 500–650 °C. Due to the chemical interaction between Al and Fe, necks of conventional shape did not form between the dissimilar particles. At the early interaction stages, the Al particles acquired shell morphology. It was shown that this morphology change was not related to the influence of electric current but was due to the Kirkendall effect in the Fe–Al system and particle rearrangement in a porous compact. No experimental evidence of melting or melt ejection during pressureless SPS of the Fe–Al mixtures or Fe and Al powders sintered separately was observed. Porous FeAl-based compacts could be obtained from Fe-40at.%Al mixtures by pressureless SPS at 650 °C. PMID:28773498

Biocompatibility assessment of spark plasma-sintered alumina-titanium cermets.

PubMed

Guzman, Rodrigo; Fernandez-García, Elisa; Gutierrez-Gonzalez, Carlos F; Fernandez, Adolfo; Lopez-Lacomba, Jose Luis; Lopez-Esteban, Sonia

2016-01-01

Alumina-titanium materials (cermets) of enhanced mechanical properties have been lately developed. In this work, physical properties such as electrical conductivity and the crystalline phases in the bulk material are evaluated. As these new cermets manufactured by spark plasma sintering may have potential application for hard tissue replacements, their biocompatibility needs to be evaluated. Thus, this research aims to study the cytocompatibility of a novel alumina-titanium (25 vol. % Ti) cermet compared to its pure counterpart, the spark plasma sintered alumina. The influence of the particular surface properties (chemical composition, roughness and wettability) on the pre-osteoblastic cell response is also analyzed. The material electrical resistance revealed that this cermet may be machined to any shape by electroerosion. The investigated specimens had a slightly undulated topography, with a roughness pattern that had similar morphology in all orientations (isotropic roughness) and a sub-micrometric average roughness. Differences in skewness that implied valley-like structures in the cermet and predominance of peaks in alumina were found. The cermet presented a higher surface hydrophilicity than alumina. Any cytotoxicity risk associated with the new materials or with the innovative manufacturing methodology was rejected. Proliferation and early-differentiation stages of osteoblasts were statistically improved on the composite. Thus, our results suggest that this new multifunctional cermet could improve current alumina-based biomedical devices for applications such as hip joint replacements. © The Author(s) 2015.

Flash sintering of stoichiometric and hyper-stoichiometric urania

DOE PAGES

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

2018-03-29

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

Flash sintering of stoichiometric and hyper-stoichiometric urania

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

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

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

Flash sintering of stoichiometric and hyper-stoichiometric urania

NASA Astrophysics Data System (ADS)

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

2018-07-01

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

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.

Effect of precursor concentration and spray pyrolysis temperature upon hydroxyapatite particle size and density.

PubMed

Cho, Jung Sang; Lee, Jeong-Cheol; Rhee, Sang-Hoon

2016-02-01

In the synthesis of hydroxyapatite powders by spray pyrolysis, control of the particle size was investigated by varying the initial concentration of the precursor solution and the pyrolysis temperature. Calcium phosphate solutions (Ca/P ratio of 1.67) with a range of concentrations from 0.1 to 2.0 mol/L were prepared by dissolving calcium nitrate tetrahydrate and diammonium hydrogen phosphate in deionized water and subsequently adding nitric acid. Hydroxyapatite powders were then synthesized by spray pyrolysis at 900°C and at 1500°C, using these calcium phosphate precursor solutions, under the fixed carrier gas flow rate of 10 L/min. The particle size decreased as the precursor concentration decreased and the spray pyrolysis temperature increased. Sinterability tests conducted at 1100°C for 1 h showed that the smaller and denser the particles were, the higher the relative densities were of sintered hydroxyapatite disks formed from these particles. The practical implication of these results is that highly sinterable small and dense hydroxyapatite particles can be synthesized by means of spray pyrolysis using a low-concentration precursor solution and a high pyrolysis temperature under a fixed carrier gas flow rate. © 2015 Wiley Periodicals, Inc.

Damage Accumulation and Failure of Plasma-Sprayed Thermal Barrier Coatings under Thermal Gradient Cyclic Conditions

NASA Technical Reports Server (NTRS)

Zhu, Dongming; Choi, Sung R.; Ghosn, Louis J.; Miller, rober A.

2005-01-01

Thermal barrier coatings will be more aggressively designed to protect gas turbine engine hot-section components in order to meet future engine higher fuel efficiency and lower emission goals. A fundamental understanding of the sintering and thermal cycling induced delamination of thermal barrier coating systems under engine-like heat flux conditions will potentially help to improve the coating temperature capability. In this study, a test approach is established to emphasize the real-time monitoring and assessment of the coating thermal conductivity, which can initially increase under the steady-state high temperature thermal gradient test due to coating sintering, and later decrease under the thermal gradient cyclic test due to coating cracking and delamination. Thermal conductivity prediction models have been established for a ZrO2-(7- 8wt%)Y2O3 model coating system in terms of heat flux, time, and testing temperatures. The coating delamination accumulation is then assessed based on the observed thermal conductivity response under the combined steady-state and cyclic thermal gradient tests. The coating thermal gradient cycling associated delaminations and failure mechanisms under simulated engine heat-flux conditions will be discussed in conjunction with the coating sintering and fracture testing results.

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

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

Fabrication of Meso-Porous Sintered Metal Thin Films by Selective Etching of Silica Based Sacrificial Template

PubMed Central

Dumée, Ludovic F.; She, Fenghua; Duke, Mikel; Gray, Stephen; Hodgson, Peter; Kong, Lingxue

2014-01-01

Meso-porous metal materials have enhanced surface energies offering unique surface properties with potential applications in chemical catalysis, molecular sensing and selective separation. In this paper, commercial 20 nm diameter metal nano-particles, including silver and copper were blended with 7 nm silica nano-particles by shear mixing. The resulted powders were cold-sintered to form dense, hybrid thin films. The sacrificial silica template was then removed by selective etching in 12 wt% hydrofluoric acid solutions for 15 min to reveal a purely metallic meso-porous thin film material. The impact of the initial silica nano-particle diameter (7–20 nm) as well as the sintering pressure (5–20 ton·m−2) and etching conditions on the morphology and properties of the final nano-porous thin films were investigated by porometry, pyknometery, gas and liquid permeation and electron microscopy. Furthermore, the morphology of the pores and particle aggregation during shear mixing were assessed through cross-sectioning by focus ion beam milling. It is demonstrated that meso-pores ranging between 50 and 320 nm in average diameter and porosities up to 47% can be successfully formed for the range of materials tested. PMID:28344241

Preparation of Ti3Al intermetallic compound by spark plasma sintering

NASA Astrophysics Data System (ADS)

Ito, Tsutomu; Fukui, Takahiro

2018-04-01

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

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

Microstructural changes in NiFe2O4 ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

NASA Astrophysics Data System (ADS)

Chauhan, Lalita; Bokolia, Renuka; Sreenivas, K.

2016-05-01

Structural properties of Nickel ferrite (NiFe2O4) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe2O4 powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe2O4 ceramics with a uniform microstructure and a large grain size.

Laser-Direct Writing of Silver Metal Electrodes on Transparent Flexible Substrates with High-Bonding Strength.

PubMed

Zhou, Weiping; Bai, Shi; Ma, Ying; Ma, Delong; Hou, Tingxiu; Shi, Xiaomin; Hu, Anming

2016-09-21

We demonstrate a novel approach to rapidly fabricate conductive silver electrodes on transparent flexible substrates with high-bonding strength by laser-direct writing. A new type of silver ink composed of silver nitrate, sodium citrate, and polyvinylpyrrolidone (PVP) was prepared in this work. The role of PVP was elucidated for improving the quality of silver electrodes. Silver nanoparticles and sintered microstructures were simultaneously synthesized and patterned on a substrate using a focused 405 nm continuous wave laser. The writing was completed through the transparent flexible substrate with a programmed 2D scanning sample stage. Silver electrodes fabricated by this approach exhibit a remarkable bonding strength, which can withstand an adhesive tape test at least 50 times. After a 1500 time bending test, the resistance only increased 5.2%. With laser-induced in-situ synthesis, sintering, and simultaneous patterning of silver nanoparticles, this technology is promising for the facile fabrication of conducting electronic devices on flexible substrates.

40 CFR 63.1543 - Standards for process and process fugitive sources.

Code of Federal Regulations, 2011 CFR

2011-07-01

... section. (1) Sinter machine; (2) Blast furnace; (3) Dross furnace; (4) Dross furnace charging location; (5) Blast furnace and dross furnace tapping location; (6) Sinter machine charging location; (7) Sinter machine discharge end; (8) Sinter crushing and sizing equipment; and (9) Sinter machine area. (b) The...

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

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.

Fast sintering of silver nanoparticle and flake layers by infrared module assistance in large area roll-to-roll gravure printing system

PubMed Central

Park, Janghoon; Kang, Hyi Jae; Shin, Kee-Hyun; Kang, Hyunkyoo

2016-01-01

We present fast sintering for silver (Ag) nanoparticle (NP) and flake layers printed using roll-to-roll (R2R) gravure printing. An infrared (IR) sintering module was applied to an R2R system to shorten the sintering duration of an R2R gravure-printed Ag layer. IR sintering of the conductive layer was improved by optimising the process condition. After printing of the Ag NP and Ag flake layers, additional IR sintering was performed in the R2R system. The lowest sheet resistance obtained in the Ag NP layer was 0.294 Ω/□, the distance between the substrate and lamp was 50-mm long, the IR lamp power was 500 W, and the sintering time was 5.4 s. The fastest sintering of 0.34 Ω/□ was achieved with 50-mm distance, 1,000-W IR lamp power, and 1.08-s sintering time. In the Ag flake layer, the lowest sheet resistance obtained was 0.288 Ω/□ with a 20-mm distance, 1,000-W IR lamp power, and 10.8-s sintering time. Meanwhile, the fastest sintering was obtained with a 3.83 Ω/□ sheet resistance, 20-mm distance, 1000-W IR lamp, and 1.08-s sintering time. Thus, the IR sintering module can easily be employed in an R2R system to obtain excellent layer sheet resistance. PMID:27713469

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

PubMed

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

2010-09-01

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. 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. 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. 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.

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

Stochastic modeling of filtrate alkalinity in water filtration devices: Transport through micro/nano porous clay based ceramic materials

USDA-ARS?s Scientific Manuscript database

Clay and plant materials such as wood are the raw materials used in manufacture of ceramic water filtration devices around the world. A step by step manufacturing procedure which includes initial mixing, molding and sintering is used. The manufactured ceramic filters have numerous pores which help i...

40 CFR Table 2 to Subpart Fffff of... - Initial Compliance With Emission and Opacity Limits

Code of Federal Regulations, 2013 CFR

2013-07-01

... flow-weighted average concentration of particulate matter from one or more control devices applied to...). 4. Each discharge end at a new sinter plant a. The flow-weighted average concentration of... BOPF at a new or existing BOPF shop a. The average concentration of particulate matter from a primary...

40 CFR Table 2 to Subpart Fffff of... - Initial Compliance With Emission and Opacity Limits

Code of Federal Regulations, 2012 CFR

2012-07-01

... flow-weighted average concentration of particulate matter from one or more control devices applied to...). 4. Each discharge end at a new sinter plant a. The flow-weighted average concentration of... BOPF at a new or existing BOPF shop a. The average concentration of particulate matter from a primary...

40 CFR Table 2 to Subpart Fffff of... - Initial Compliance With Emission and Opacity Limits

Code of Federal Regulations, 2011 CFR

2011-07-01

... flow-weighted average concentration of particulate matter from one or more control devices applied to...). 4. Each discharge end at a new sinter plant a. The flow-weighted average concentration of... BOPF at a new or existing BOPF shop a. The average concentration of particulate matter from a primary...

40 CFR Table 2 to Subpart Fffff of... - Initial Compliance With Emission and Opacity Limits

Code of Federal Regulations, 2014 CFR

2014-07-01

... flow-weighted average concentration of particulate matter from one or more control devices applied to...). 4. Each discharge end at a new sinter plant a. The flow-weighted average concentration of... BOPF at a new or existing BOPF shop a. The average concentration of particulate matter from a primary...

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.

Behavior of New Zealand Ironsand During Iron Ore Sintering

NASA Astrophysics Data System (ADS)

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

2016-02-01

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

High energy electron sintering of icy regoliths: Formation of the PacMan thermal anomalies on the icy Saturnian moons

NASA Astrophysics Data System (ADS)

Schaible, M. J.; Johnson, R. E.; Zhigilei, L. V.; Piqueux, S.

2017-03-01

The so-called 'PacMan' features on the leading hemispheres of the icy Saturnian moons of Mimas, Tethys and Dione were initially identified as anomalous optical discolorations and subsequently shown to have greater thermal inertia than the surrounding regions. The shape of these regions matches calculated deposition contours of high energy plasma electrons moving opposite to the moon's orbital direction, thus suggesting that electron interactions with the grains produce the observed anomalies. Here, descriptions of radiation-induced diffusion processes are given, and various sintering models are considered to calculate the rate of increase in the contact volume between grains in an icy regolith. Estimates of the characteristic sintering timescale, i.e. the time necessary for the thermal inertia to increase from that measured outside the anomalous regions to that within, are given for each of the moons. Since interplanetary dust particle (IDP) impact gardening and E-ring grain infall would be expected to mix the regolith and obscure the effects of high energy electrons, sintering rates are compared to rough estimates of the impact-induced resurfacing rates. Estimates of the sintering timescale determined by extrapolating laboratory measurements are below ∼0.03 Myr, while the regolith renewal timescales are larger than ∼0.1 Myr, thus indicating that irradiation by the high energy electrons should be sufficient to form stable thermal anomalies. More detailed models developed for sintering of spherical grains are able to account for the radiation-induced anomalies on Mimas and Tethys only if the regoliths on those bodies are relatively compact and composed of small (≲ 5 μm) grains or grain aggregates, and/or the grains are highly non-spherical with surface defect densities in the inter-grain contact regions that are much higher than expected for crystalline water ice grains at thermal equilibrium. These results are consistent with regolith thermal conductivity models which can only be reconciled with spacecraft observations if the contacts between grains are assumed to have much lower thermal conductance than predicted for idealized grains. The strength of the anomalies on Tethys and Dione appear to be limited by E-ring grain infall, while on Mimas IDP gardening limits the strength of the anomaly. The smaller flux of more deeply penetrating high energy (>1 MeV) electrons on Dione can account for the small thermal inertia differences measured there. Determining regolith sintering rates and the corresponding effect on thermal conductivity can, in principle, provide an independent constraint on the regolith grain geometries and exposure timescales for icy bodies.

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.

The influence of sintering temperature on the proliferation of fibroblastic cells in contact with HA-bioceramics.

PubMed

Frayssinet, P; Rouquet, N; Fages, J; Durand, M; Vidalain, P O; Bonel, G

1997-06-05

HA-ceramics used in human surgery as osteoconductive surfaces show a great variety of characteristics. Certain characteristics such as grain size, porosity, and surface area, are controlled by the sintering temperature of the slurry. We grew L-929 fibroblast cells on HA-ceramic disks that had been sintered at different temperatures ranging from 850 degrees-1350 degrees C. The cell line growth rate was lower on ceramic disks than on the culture-grade polystyrene used as a negative control. Cell growth correlated with the ceramic sintering temperature although no significant difference in the cell adhesion to the different ceramics was shown. Growth rate on ceramics sintered at low temperatures (850 degrees and 950 degrees C) was negative whereas it was positive on disks sintered at higher temperatures. When the cells were separated from the disks by a polycarbonate membrane, the growth rate was negative on those membranes in contact with low-temperature sintered disks and positive on the high-temperature sintered disks. The calcium and phosphorus concentration in the culture medium in contact with ceramics sintered below 1050 degrees C decreased during the culture period. Ceramics sintered between 1100 degrees and 1250 degrees C brought about an increase in Ca and P concentrations while ceramics sintered at higher temperatures did not induce any changes. SEM examination of the 850 degrees and 1200 degrees C sintered ceramics showed that the 850 degrees C sintered ceramics consisted of small grains with pores between them and the 1200 degrees C sintered ceramics were made of larger grains without any visible pores, thereby decreasing the surface of material in contact with the culture medium. This difference in surface area was confirmed by the fact that the amount of albumin absorbed onto the ceramic was dependent on the sintering temperature. In conclusion, the modification of the culture medium brought about by high-surfaced ceramics could influence the growth of cells with which such ceramics come in contact.

Low thermal budget photonic processing of highly conductive Cu interconnects based on CuO nanoinks. Potential for flexible printed electronics

DOE PAGES

Rager, Matthew S.; Aytug, Tolga; Veith, Gabriel M.; ...

2015-12-31

The developing field of printed electronics nanoparticle based inks such as CuO show great promise as a low-cost alternative to other metal-based counterparts (e.g., silver). In particular, CuO inks significantly eliminate the issue of particle oxidation, before and during the sintering process, that is prevalent in Cu-based formulations. We report here the scalable and low-thermal budget photonic fabrication of Cu interconnects employing a roll-to-roll compatible pulse-thermal-processing (PTP) technique that enables phase reduction and subsequent sintering of inkjet-printed CuO patterns onto flexible polymer templates. Detailed investigations of curing and sintering conditions were performed to understand the impact of PTP system conditionsmore » on the electrical performance of the Cu patterns. Specifically, the impact of energy and power of photonic pulses on print conductivity was systematically studied by varying the following key processing parameters: pulse intensity, duration and sequence. Through optimization of such parameters, highly conductive prints in < 1 s with resistivity values as low as 100 n m has been achieved. We also observed that the introduction of an initial ink-drying step in ambient atmosphere, after the printing and before sintering, leads to significant improvements in mechanical integrity and electrical performance of the printed Cu patterns. Moreover, the viability of CuO reactive inks, coupled with the PTP technology and pre ink-drying protocols, has also been demonstrated for the additive integration of a low-cost Cu temperature sensor onto a flexible polymer substrate.« less

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

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.

[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.

Fuel cell assembly fluid flow plate having conductive fibers and rigidizing material therein

DOEpatents

Walsh, Michael M.

2000-01-01

A fluid flow plate is preferably formed with three initial sections, for instance, two layers of conductive (e.g., metal) fibers and a barrier material (e.g., metal foil) which is interposed between the two layers. For example, sintering of these three sections can provide electrical path(s) between outer faces of the two layers. Then, the sintered sections can be, for instance, placed in a mold for forming of flow channel(s) into one or more of the outer faces. Next, rigidizing material (e.g., resin) can be injected into the mold, for example, to fill and/or seal space(s) about a conductive matrix of the electrical path(s). Preferably, abrading of surface(s) of the outer face(s) serves to expose electrical contact(s) to the electrical path(s).

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 sintering atmosphere on properties of porous stainless steel for biomedical applications.

PubMed

Dudek, Agata; Włodarczyk, Renata

2013-01-01

This study discusses manufacturing of metallic biomaterials by means of powder metallurgy with consideration for their unquestionable advantages, i.e. opportunities of obtaining materials with controllable porosity. The paper focuses on properties of 316 L stainless steel obtained using the method of powder metallurgy with respect to compacting pressure and sintering atmosphere. All the specimens were compacted at 700, 400 and 225 MPa, and sintered at 1250 °C. In order to analyze the sintering atmosphere, three different media were used: dissociated ammonia, hydrogen and vacuum. The study covered sintering density, porosity, microstructure analysis and corrosion resistance. The proposed method of powder metallurgy allowed for obtaining materials with predictable size and distribution of pores, depending on the parameters of sinter preparation (compaction force, sinter atmosphere). High corrosion resistance of the materials (sintering in the atmosphere of hydrogen and in vacuum) and high porosity in the sinters studied offer opportunities for using them for medical purposes. Copyright © 2012 Elsevier B.V. All rights reserved.

[Effect of compaction pressure on the properties of dental machinable zirconia ceramic].

PubMed

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

2010-10-01

To investigate the effect of compaction pressure on the linear shrinkage, sintering property and machinability of the dental zirconia ceramic. The nano-size zirconia powder was compacted at different isostatic pressure and sintered at different temperature. The linear shrinkage of sintered body was measured and the relative density was tested using the Archimedes method. The cylindrical surface of pre-sintering blanks was traversed using a hard metal tool. Surface and edge quality were checked visually using light stereo microscopy. The sintering behaviour depended on the compaction pressure. Increasing compaction pressure led to higher sintering rate and lower sintering temperature. Increasing compaction pressure also led to decreasing linear shrinkage of the sintered bodies, from 24.54% of 50 MPa to 20.9% of 400 MPa. Compaction pressure showed only a weak influence on machinability of zirconia blanks, but the higher compaction pressure resulted in the poor surface quality. The better sintering property and machinability of dental zirconia ceramic is found for 200-300 MPa compaction pressure.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

Characteristics of iron ore sinter with EFB addition

NASA Astrophysics Data System (ADS)

Purwanto, H.; Rozhan, A. N.; Mohamad, A. S.; Zakiyuddin, A.

2018-04-01

Utilization of EFB-derived biochar in sintering of iron ore has been conducted in this work with regards to the porosity of iron sinter. EFB has been heated up in argon atmosphere to 450°C in order to produce biochar. In the present work, the sintering process was conducted at 1150°C with variations of biochar content from 5% to 10%. In this case, the apparent density for iron sinter shows significant decrease as the biochar addition increase. The porosity of iron sinter showed a gradual increment from 5% to 7.5% and escalated at 10% biochar content. The results of porosity and apparent density were in line with the micrograph of iron sinter.

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.

Optimizing Grain Boundary Complexions to Produce Dense Pressure-Less Sintered Boron Carbide (B4C)

DTIC Science & Technology

2008-11-14

discontinuous distribution of the yttria. At this stage it is difficult to determine if the discontinuity is genuine or results from dewetting upon cooling...sample. However, the tendency of the film to form beads indicates a dewetting behavior. The weak interface between the yttria and the boron carbide...conform to the dewetting behavior. There is a possibility of a complexion transition as the sample is cooled down in the furnace. At high temperature the

Sintered Lining for Heat-Pipe Evaporator

NASA Technical Reports Server (NTRS)

Ernst, D. M.; Eastman, G. Y.

1985-01-01

Hotspots eliminated by lining inner wall. Distribution of heat transfer liquid in heat-pipe evaporator improved by lining inner wall with layer of sintered metal. Sintered layer takes place of layer of screen wick formerly sintered or bonded to wall. Since sintered layer always full of liquid, no hotspot of type that previously arose where former screen wick did not fit properly against wall.

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.

[Influence of manufacture technique on translucency and color of dental porcelain].

PubMed

Xiong, Fang; Chao, Yong-Lie; Zhu, Zhi-Min

2007-12-01

To study the influence of manufacture technique on the translucency and color of dental porcelain. Specimens were made of VITA VMK 95 dentin porcelain and enamel porcelain and divided into 3 groups: Sintering times group (1, 2, 4, 6, 8 and 10 times), sintering temperature group (910, 920, 930, 940 and 950 degrees C), sintering vacuum group (95, 65, 35 and 0 kPa). Transmittance, Y, dominant wavelength and saturation were measured by PR-650 spectra scan spectrocolorimeter. Transmittance of dentin porcelain increased after 6 times repeated sintering. Transmittance of enamel porcelain increased first after the second sintering, and then became decreasing when sintering more than 2 times. Transmittance of enamel porcelain deceased when sintering temperature was lower than standard. Decrease of sintering vacuum caused the transmittance of dentin and enamel porcelain decreased. The changing of value was coordinated with transmittance. Dominant wavelength and saturation had negative correlation with sintering times and temperature, and positive correlation with vacuum. Sintering times, temperature and vacuum all had prominent effects on the translucency and color of dental porcelain. Comparing with dentin porcelain, enamel porcelain was more sensitive with the modification of manufacture technique.

Effect of Sintering Temperature on Magnetic Core-Loss Properties of a NiCuZn Ferrite for High-Frequency Power Converters

NASA Astrophysics Data System (ADS)

Yan, Yi; Ngo, Khai D. T.; Hou, Dongbin; Mu, Mingkai; Mei, Yunhui; Lu, Guo-Quan

2015-10-01

In an effort to find a magnetic material for making low-loss magnetic components for high-power-density converters, we investigated the magnetic core-loss characteristics of a commercial NiCuZn ferrite (LSF 50) at 5 MHz as a function of the sintering temperature of the ferrite powder. The ferrite powder was compacted into toroid cores and then sintered at 850°C, 900°C, 950°C, 1000°C, and 1050°C for 2 h. The sintered densities of the cores increased at higher sintering temperatures. The magnetic properties of the sintered cores—complex permeability and core-loss density—were measured. We found that both the real and imaginary parts of the relative permeability increased with sintering temperature. The core-loss results at 5 MHz showed that the cores sintered at 950°C and 1000°C had the lowest core-loss densities, being two to three times lower than that of a commercial NiZn ferrite (4F1) core. Microstructures of the sintered cores were examined by scanning electron microscopy; the grains grew significantly at higher sintering temperatures.

Enhanced thermal conductivity of uranium dioxide-silicon carbide composite fuel pellets prepared by Spark Plasma Sintering (SPS)

NASA Astrophysics Data System (ADS)

Yeo, S.; Mckenna, E.; Baney, R.; Subhash, G.; Tulenko, J.

2013-02-01

Uranium dioxide (UO2)-10 vol% silicon carbide (SiC) composite fuel pellets were produced by oxidative sintering and Spark Plasma Sintering (SPS) at a range of temperatures from 1400 to 1600 °C. Both SiC whiskers and SiC powder particles were utilized. Oxidative sintering was employed over 4 h and the SPS sintering was employed only for 5 min at the highest hold temperature. It was noted that composite pellets sintered by SPS process revealed smaller grain size, reduced formation of chemical products, higher density, and enhanced interfacial contact compared to the pellets made by oxidative sintering. For given volume of SiC, the pellets with powder particles yielded a smaller grain size than pellets with SiC whiskers. Finally thermal conductivity measurements at 100 °C, 500 °C, and 900 °C revealed that SPS sintered UO2-SiC composites exhibited an increase of up to 62% in thermal conductivity compared to UO2 pellets, while the oxidative sintered composite pellets revealed significantly inferior thermal conductivity values. The current study points to the improved processing capabilities of SPS compared to oxidative sintering of UO2-SiC composites.

On the self-damping nature of densification in photonic sintering of nanoparticles

PubMed Central

MacNeill, William; Choi, Chang-Ho; Chang, Chih-Hung; Malhotra, Rajiv

2015-01-01

Sintering of nanoparticle inks over large area-substrates is a key enabler for scalable fabrication of patterned and continuous films, with multiple emerging applications. The high speed and ambient condition operation of photonic sintering has elicited significant interest for this purpose. In this work, we experimentally characterize the temperature evolution and densification in photonic sintering of silver nanoparticle inks, as a function of nanoparticle size. It is shown that smaller nanoparticles result in faster densification, with lower temperatures during sintering, as compared to larger nanoparticles. Further, high densification can be achieved even without nanoparticle melting. Electromagnetic Finite Element Analysis of photonic heating is coupled to an analytical sintering model, to examine the role of interparticle neck growth in photonic sintering. It is shown that photonic sintering is an inherently self-damping process, i.e., the progress of densification reduces the magnitude of subsequent photonic heating even before full density is reached. By accounting for this phenomenon, the developed coupled model better captures the experimentally observed sintering temperature and densification as compared to conventional photonic sintering models. Further, this model is used to uncover the reason behind the experimentally observed increase in densification with increasing weight ratio of smaller to larger nanoparticles. PMID:26443492

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

PubMed

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

2015-09-01

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

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.

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.

Alumina shunt for precooling a cryogen-free 4He or 3He refrigerator

NASA Astrophysics Data System (ADS)

Uhlig, Kurt

2016-10-01

In this technical report a cryogen-free 1 K cryostat is described where the pot of the 4He refrigeration unit is precooled by the 2nd stage of a pulse tube cryocooler (PTC) from room temperature to T ∼ 3 K via a shunt made from sintered alumina (SA); the total mass of the 1 K stage is 3.5 kg. SA has high thermal conductivity at high temperatures; but below ∼50 K the thermal conductivity drops rapidly, almost following a T3-law. This makes SA an interesting candidate for the construction of a thermal shunt, especially as the heat capacity of metals drops by several orders of magnitude in the temperature range from 300 K to 3 K. At the base temperature of the PTC, the heat conduction of the shunt is so small that the heat leak into the 1 K stage is negligible.

Cryogenic cooler apparatus

DOEpatents

Wheatley, J.C.; Paulson, D.N.; Allen, P.C.

1983-01-04

A Malone-type final stage for utilization in a Stirling cycle cryogenic cooler apparatus includes a displacer slidable within a vessel. [sup 4]He, [sup 3]He, or a mixture thereof is made to flow in a pulsating unidirectional manner through a regenerator in the displacer by utilization of check valves in separate fluid channels. Stacked copper screen members extend through the channels and through a second static thermodynamic medium within the displacer to provide efficient lateral heat exchange and enable cooling to temperatures in the range of 3--4 K. Another embodiment utilizes sintered copper particles in the regenerator. Also described is a final stage that has a non-thermally conducting displacer having passages with check valves for directing fluid past a regenerator formed in the surrounding vessel. 10 figs.

Cryogenic cooler apparatus

DOEpatents

Wheatley, John C.; Paulson, Douglas N.; Allen, Paul C.

1983-01-01

A Malone-type final stage for utilization in a Stirling cycle cryogenic cooler apparatus includes a displacer slidable within a vessel. .sup.4 He, .sup.3 He, or a mixture thereof is made to flow in a pulsating unidirectional manner through a regenerator in the displacer by utilization of check valves in separate fluid channels. Stacked copper screen members extend through the channels and through a second static thermodynamic medium within the displacer to provide efficient lateral heat exchange and enable cooling to temperatures in the range of 3-4 K. Another embodiment utilizes sintered copper particles in the regenerator. Also described is a final stage that has a non-thermally conducting displacer having passages with check valves for directing fluid past a regenerator formed in the surrounding vessel.

Al2O3-TiC Composite Prepared by Spark Plasma Sintering Process: Evaluation of Mechanical and Tribological Properties

NASA Astrophysics Data System (ADS)

Kumar, Rohit; Chaubey, A. K.; Bathula, Sivaiah; Prashanth, K. G.; Dhar, Ajay

2018-03-01

Al2O3-10TiC composites were synthesized by spark plasma sintering (SPS) process. Microstructural and mechanical properties of the composite reveal homogeneous distribution of the fine TiC particles in the matrix. The samples were produced with different sintering temperature, and it shows that the hardness and density gradually increases with increasing sintering temperature. Abrasion wear test result reveals that the composite sintered at 1500 °C shows high abrasion resistance (wt. loss 0.016 g) and the lowest abrasion resistance was observed for the composite sample sintered at 1100 °C (wt. loss 1.459 g). The profilometry surface roughness study shows that sample sintered at 1100 °C shows maximum roughness ( R a = 6.53 µm) compared to the sample sintered at 1500 °C ( R a = 0.66 µm) corroborating the abrasion wear test results.

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

NASA Technical Reports Server (NTRS)

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

1985-01-01

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

Gravitational Role in Liquid Phase Sintering

NASA Technical Reports Server (NTRS)

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

1998-01-01

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

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.

Novel Processing of Boron Carbide (B4C): Plasma Synthesized Nano Powders and Pressureless Sintering Forming of Complex Shapes

DTIC Science & Technology

2008-12-01

Figure 4. B4C plates formed via hot pressing with a curved shape. Commercial B4C shows a large number of lenticular graphitic inclusions, Figure 5...materials and they act as crack initiation points in flexure testing. Figure 5. SEM micrograph showing large lenticular graphitic inclusions in commercial

Lightweight Electrode For Nickel/Hydrogen Cell

NASA Technical Reports Server (NTRS)

Britton, Doris L.

1994-01-01

Improved substrate for nickel electrode increases specific energy of nickel/hydrogen cell. Consists of 50 percent by weight nickel fiber, 35 percent nickel powder, and 15 percent cobalt powder. Porosity and thickness of nickel electrodes affect specific energy, initial performance, and cycle life of cell. Substrate easily manufactured with much larger porosities than those of heavy-sintered state-of-art nickel substrate.

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

DTIC Science & Technology

2012-08-01

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

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.

Highly Dispersed and Active ReOx on Alumina-Modified SBA-15 Silica for 2-Butanol Dehydration

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

She, Xiaoyan; Kwak, Ja Hun; Sun, Junming

2012-05-23

SBA-15 silica supported rhenium catalysts were synthesized using solution-based atomic layer deposition method, and their activity and stability were studied in the acid-catalyzed 2-butanol dehydration. We find that ReOx/SBA-15 exhibited an extremely high initial activity but a fast deactivation for 2-butanol dehydration at 90-105 C. Fast deactivation was likely due to the sintering, sublimation, and reduction of rhenia as confirmed by TEM, elemental analysis, and in situ UV vis (DRS) measurements. To overcome these issues, ReOx/AlOx/SBA-15 catalysts with significantly improved stability were prepared by first modifying the surface identity of SBA-15 with alumina followed by dispersion of rhenia using atomicmore » layer deposition. The AlOx phase stabilizes the dispersion of small and uniform rhenia clusters (<2 nm) as as confirmed by TEM, STEM and UV-vis (DRS) characterizations. Additional 27Al MAS NMR characterization revealed that modification of the SBA-15 surface with alumina introduces a strong interaction between rhenia and alumina, which consequently improves the stability of supported rhenia catalysts by suppressing the sintering, sublimation, and reduction of rhenia albeit at a moderately reduced initial catalytic dehydration activity« less

Effect of Particle Morphology on Cold Spray Deposition of Chromium Carbide-Nickel Chromium Cermet Powders

NASA Astrophysics Data System (ADS)

Fernandez, Ruben; Jodoin, Bertrand

2017-08-01

Nickel chromium-chromium carbide coatings provide good corrosion and wear resistance at high temperatures, making them ideal for applications where a harsh environment and high temperatures are expected. Thermal spray processes are preferred as deposition technique of cermets, but the high process temperatures can lead to decarburization and reduction of the coatings properties. Cold spray uses lower temperatures preventing decarburization. Since the metallic phase remains solid, the feedstock powder morphology becomes crucial on the deposition behavior. Six commercially available powders were studied, varying in morphology and metal/ceramic ratios. The powders were categorized into 4 groups depending on their morphology. Spherical powders lead to substrate erosion due to their limited overall ductility. Porous agglomerated and sintered powders lead to severely cracked coatings. For dense agglomerated and sintered powders, the outcome depended on the initial metal/ceramic ratio: powders with 25 wt.% NiCr led to substrate erosion while 35 wt.% NiCr powders led to dense coatings. Finally, blended ceramic-metal mixtures also lead to dense coatings. All coatings obtained had lower ceramic content than the initial feedstock powders. Interrupted spray tests, combined with FEA, helped drawing conclusions on the deposition behavior to explain the obtained results.

Correlation of gold in siliceous sinters with 3He 4He in hot spring waters of Yellowstone National Park

USGS Publications Warehouse

Fournier, R.O.; Kennedy, B.M.; Aoki, M.; Thompson, J.M.

1994-01-01

Opaline sinter samples collected at Yellowstone National Park (YNP) were analyzed for gold by neutron activation and for other trace elements by the inductively coupled plasma optical emission spectroscopy (ICP-OES) method. No correlation was found between Au and As, Sb, or total Fe in the sinters, although the sample containing the highest Au also contains the highest Sb. There also was no correlation of Au in the sinter with the H2S concentration in the discharged hot spring water or with the estimated temperature of last equilibration of the water with the surrounding rock. The Au in rhyolitic tuffs and lavas at YNP found within the Yellowstone caldera show the same range in Au as do those outside the caldera, while thermal waters from within this caldera all have been found to contain relatively low dissolved Au and to deposit sinters that contain relatively little Au. Therefore, it is not likely that variations in Au concentrations among these sinters simply reflect differences in leachable Au in the rocks through which the hydrothermal fluids have passed. Rather, variations in [H2S], the concentration of total dissolved sulfide, that result from different physical and chemical processes that occur in different parts of the hydrothermal system appear to exert the main control on the abundance of Au in these sinters. Hydrothermal fluids at YNP convect upward through a series of successively shallower and cooler reservoirs where water-rock chemical and isotopic reactions occur in response to changing temperature and pressure. In some parts of the system the fluids undergo decompressional boiling, and in other parts they cool conductively without boiling. Mixing of ascending water from deep in the system with shallow groundwaters is common. All three processes generally result in a decrease in [H2S] and destabilize dissolved gold bisulfide complexes in reservoir waters in the YNP system. Thus, different reservoirs in rocks of similar composition and at similar temperatures may contain waters with different [H2S] and [Au]. The [H2S] in a subsurface reservoir water is difficult to assess on the basis of analyses of hot spring waters because of uncertainties about steam loss during fluid ascent. However, the same processes that result in low [H2S] in reservoir waters also tend to result in decreases in the ratio of 3He 4He(R) dissolved in that water. Values of R relative to this ratio in air (Ra) attain values > 15 in YNP thermal waters. To date, all of the thermal waters at YNP that have R Ra values <9 have been found to deposit sinters with relatively low gold concentrations. These include all of the thermal waters that discharge from 180-215??C reservoirs at Upper, Midway, and Lower Geyser Basins within the western part of the Yellowstone caldera, and thermal waters at Norris Geyser Basin, outside the Yellowstone caldera, where some of the waters flow directly to the surface from a reservoir where the temperature is about 300??C. A high 3He 4He ratio in thermal water discharged at the surface does not guarantee high gold concentrations in the sinter deposited by this water. Boiling with loss of steam (the gas phase takes a separate route to the surface) during rapid upflow from the shallowest reservoir to the surface decreases the [H2S] and total He dissolved in the residual liquid without appreciably changing the 3He 4He ratio. This is because the isotopic composition of the He of the initial bulk fluid is unchanged and there is too little time for much radiogenic 4He to build back into the liquid during this rapid ascent from the near-surface reservoir. However, if boiling with phase separation and loss of steam occurs deep in the system, the 3He 4He ratio in the residual liquid, now depleted in H2S and total He, will be susceptible to dilution with radiogenic 4He that is acquired during the longer residence time underground. Some or all of the Au that comes out of solution when an initial gold bisulfide complex breaks

One step sintering of homogenized bauxite raw material and kinetic study

NASA Astrophysics Data System (ADS)

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

2016-10-01

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

[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.

Human endothelial cell growth and phenotypic expression on three dimensional poly(lactide-co-glycolide) sintered microsphere scaffolds for bone tissue engineering.

PubMed

Jabbarzadeh, Ehsan; Jiang, Tao; Deng, Meng; Nair, Lakshmi S; Khan, Yusuf M; Laurencin, Cato T

2007-12-01

Bone tissue engineering offers promising alternatives to repair and restore tissues. Our laboratory has employed poly(lactide-co-glycolide) PLAGA microspheres to develop a three dimensional (3-D) porous bioresorbable scaffold with a biomimetic pore structure. Osseous healing and integration with the surrounding tissue depends in part on new blood vessel formation within the porous structure. Since endothelial cells play a key role in angiogenesis (formation of new blood vessels from pre-existing vasculature), the purpose of this study was to better understand human endothelial cell attachment, viability, growth, and phenotypic expression on sintered PLAGA microsphere scaffold. Scanning electron microscopy (SEM) examination showed cells attaching to the surface of microspheres and bridging the pores between the microspheres. Cell proliferation studies indicated that cell number increased during early stages and reached a plateau between days 10 and 14. Immunofluorescent staining for actin showed that cells were proliferating three dimensionally through the scaffolds while staining for PECAM-1 (platelet endothelial cell adhesion molecule) displayed typical localization at cell-cell contacts. Gene expression analysis showed that endothelial cells grown on PLAGA scaffolds maintained their normal characteristic phenotype. The cell proliferation and phenotypic expression were independent of scaffold pore architecture. These results demonstrate that PLAGA sintered microsphere scaffolds can support the growth and biological functions of human endothelial cells. The insights from this study should aid future studies aimed at enhancing angiogenesis in three dimensional tissue engineered scaffolds.

Effect of SiC Nanowhisker on the Microstructure and Mechanical Properties of WC-Ni Cemented Carbide Prepared by Spark Plasma Sintering

PubMed Central

Fu, Zhiqiang; Wang, Chengbiao

2014-01-01

Ultrafine tungsten carbide-nickel (WC-Ni) cemented carbides with varied fractions of silicon carbide (SiC) nanowhisker (0–3.75 wt.%) were fabricated by spark plasma sintering at 1350°C under a uniaxial pressure of 50 MPa with the assistance of vanadium carbide (VC) and tantalum carbide (TaC) as WC grain growth inhibitors. The effects of SiC nanowhisker on the microstructure and mechanical properties of the as-prepared WC-Ni cemented carbides were investigated. X-ray diffraction analysis revealed that during spark plasma sintering (SPS) Ni may react with the applied SiC nanowhisker, forming Ni2Si and graphite. Scanning electron microscopy examination indicated that, with the addition of SiC nanowhisker, the average WC grain size decreased from 400 to 350 nm. However, with the additional fractions of SiC nanowhisker, more and more Si-rich aggregates appeared. With the increase in the added fraction of SiC nanowhisker, the Vickers hardness of the samples initially increased and then decreased, reaching its maximum of about 24.9 GPa when 0.75 wt.% SiC nanowhisker was added. However, the flexural strength of the sample gradually decreased with increasing addition fraction of SiC nanowhisker. PMID:25003143

Establishing Antibacterial Multilayer Films on the Surface of Direct Metal Laser Sintered Titanium Primed with Phase-Transited Lysozyme

PubMed Central

Guan, Binbin; Wang, Haorong; Xu, Ruiqing; Zheng, Guoying; Yang, Jie; Liu, Zihao; Cao, Man; Wu, Mingyao; Song, Jinhua; Li, Neng; Li, Ting; Cai, Qing; Yang, Xiaoping; Li, Yanqiu; Zhang, Xu

2016-01-01

Direct metal laser sintering is a technology that allows the fabrication of titanium (Ti) implants with a functional gradation of porosity and surface roughness according to three-dimensional (3D) computer data. The surface roughness of direct metal laser sintered titanium (DMLS-Ti) implants may provide abundant binding sites for bacteria. Bacterial colonization and subsequent biofilm formation can cause unsatisfactory cell adhesion and implant-related infections. To prevent such infections, a novel phase-transited lysozyme (PTL) was utilized as an initial functional layer to simply and effectively prime DMLS-Ti surfaces for subsequent coating with antibacterial multilayers. The purpose of the present study was to establish a surface with dual biological functionality. The minocycline-loaded polyelectrolyte multilayers of hyaluronic acid (HA) and chitosan (CS) formed via a layer-by-layer (LbL) self-assembly technique on PTL-functionalized DMLS-Ti were designed to inhibit pathogenic microbial infections while allowing the DMLS-Ti itself and the modified coatings to retain acceptable biocompatibility. The experimental results indicate that the DMLS-Ti and the hydrogel treated surfaces can inhibit early bacterial adhesion while completely preserving osteoblast functions. This design is expected to gain considerable interest in the medical field and to have good potential for applications in multifunctional DMLS-Ti implants. PMID:27821857

Establishing Antibacterial Multilayer Films on the Surface of Direct Metal Laser Sintered Titanium Primed with Phase-Transited Lysozyme.

PubMed

Guan, Binbin; Wang, Haorong; Xu, Ruiqing; Zheng, Guoying; Yang, Jie; Liu, Zihao; Cao, Man; Wu, Mingyao; Song, Jinhua; Li, Neng; Li, Ting; Cai, Qing; Yang, Xiaoping; Li, Yanqiu; Zhang, Xu

2016-11-08

Direct metal laser sintering is a technology that allows the fabrication of titanium (Ti) implants with a functional gradation of porosity and surface roughness according to three-dimensional (3D) computer data. The surface roughness of direct metal laser sintered titanium (DMLS-Ti) implants may provide abundant binding sites for bacteria. Bacterial colonization and subsequent biofilm formation can cause unsatisfactory cell adhesion and implant-related infections. To prevent such infections, a novel phase-transited lysozyme (PTL) was utilized as an initial functional layer to simply and effectively prime DMLS-Ti surfaces for subsequent coating with antibacterial multilayers. The purpose of the present study was to establish a surface with dual biological functionality. The minocycline-loaded polyelectrolyte multilayers of hyaluronic acid (HA) and chitosan (CS) formed via a layer-by-layer (LbL) self-assembly technique on PTL-functionalized DMLS-Ti were designed to inhibit pathogenic microbial infections while allowing the DMLS-Ti itself and the modified coatings to retain acceptable biocompatibility. The experimental results indicate that the DMLS-Ti and the hydrogel treated surfaces can inhibit early bacterial adhesion while completely preserving osteoblast functions. This design is expected to gain considerable interest in the medical field and to have good potential for applications in multifunctional DMLS-Ti implants.

Phase Transformation of Andalusite-Mullite and Its Roles in the Microstructure and Sinterability of Refractory Ceramic

NASA Astrophysics Data System (ADS)

Li, Bowen; He, Mengsheng; Wang, Huaguang

2017-07-01

Andalusite has been realized as a special mineral for the production of refractory ceramics due to its unique property to automatically decompose into mullite and silica during heating at high temperature. The phase transformation from andalusite to mullite plays a critical role for the effective applications of andalusite. This study investigated the microstructural characteristics and sinterability of andalusite powder during high-temperature decomposition. The andalusite powder was bonded with kaolin and prepared as a cylinder green body at 20 MPa; it was then fired at 1423 K to 1723 K (1150 °C to 1450 °C). The microstructures and mechanical strengths of the sintered ceramics were studied by the compressive test, X-ray diffraction, and scanning electron microscopy. The results showed that newly born mullite appeared as rodlike microcrystals and dispersed around the initial andalusite. At 1423 K (1150 °C), the mullitization of andalusite was started, but the complete mullitization was not found until firing at 1723 K (1450 °C). The compressive strength of the ceramics increased from 93.7 to 294.6 MPa while increasing the fire temperature from 1423 K to 1723 K (1150 °C to 1450 °C). Meanwhile, the bulk density of the ceramics was only slightly changed from 2.15 to 2.19 g/cm3.

Establishing Antibacterial Multilayer Films on the Surface of Direct Metal Laser Sintered Titanium Primed with Phase-Transited Lysozyme

NASA Astrophysics Data System (ADS)

Guan, Binbin; Wang, Haorong; Xu, Ruiqing; Zheng, Guoying; Yang, Jie; Liu, Zihao; Cao, Man; Wu, Mingyao; Song, Jinhua; Li, Neng; Li, Ting; Cai, Qing; Yang, Xiaoping; Li, Yanqiu; Zhang, Xu

2016-11-01

Direct metal laser sintering is a technology that allows the fabrication of titanium (Ti) implants with a functional gradation of porosity and surface roughness according to three-dimensional (3D) computer data. The surface roughness of direct metal laser sintered titanium (DMLS-Ti) implants may provide abundant binding sites for bacteria. Bacterial colonization and subsequent biofilm formation can cause unsatisfactory cell adhesion and implant-related infections. To prevent such infections, a novel phase-transited lysozyme (PTL) was utilized as an initial functional layer to simply and effectively prime DMLS-Ti surfaces for subsequent coating with antibacterial multilayers. The purpose of the present study was to establish a surface with dual biological functionality. The minocycline-loaded polyelectrolyte multilayers of hyaluronic acid (HA) and chitosan (CS) formed via a layer-by-layer (LbL) self-assembly technique on PTL-functionalized DMLS-Ti were designed to inhibit pathogenic microbial infections while allowing the DMLS-Ti itself and the modified coatings to retain acceptable biocompatibility. The experimental results indicate that the DMLS-Ti and the hydrogel treated surfaces can inhibit early bacterial adhesion while completely preserving osteoblast functions. This design is expected to gain considerable interest in the medical field and to have good potential for applications in multifunctional DMLS-Ti implants.

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

Plucknett, K.P.; Tiegs, T.N.; Becher, P.F.

Ductile nickel aluminide (Ni{sub 3}Al) alloys have been used as a `binder` phase for the fabrication of both titanium and tungsten carbide (TiC and WC) matrix composites. Ni{sub 3}Al alloys are also unusual in that their yield strength increases with temperature, to a maximum at 700-800{degrees}C. These properties, combined with high tensile ductilities (up to 50% strain), make Ni{sub 3}Al a potentially attractive replacement for Co in cemented carbide fabrication. Materials have been fabricated by both hot-pressing and vacuum-sintering, with Ni{sub 3}Al contents ranging from 15 to 95 vol. %. Vacuum-sintering cycles were generally similar to those used for themore » fabrication of WC/Co and TiC/Ni (i.e. T{sub sint} {approximately}1450-1600{degrees}C), resulting in sintered densities >95 % of theoretical. WC/Ni{sub 3}Al materials exhibited an order of magnitude improvement in corrosion resistance over WC/Co, during immersion tests in either sulfuric or nitric acid. These materials also demonstrated improved high temperature strength retention compared to WC/Co cermets, though the initial room temperature strengths were lower. Fracture toughness varied between 8 and 25 MPa m{sup {1/2}}, and depended primarily upon Ni{sub 3}Al content and composition.« 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.

Sintering Kinetics of Inkjet Printed Conductive Silver Lines on Insulating Plastic Substrate

DOE PAGES

Zhou, Wenchao; List, III, Frederick Alyious; Duty, Chad E; ...

2015-01-24

This paper focuses on sintering kinetics of inkjet printed lines containing silver nanoparticles deposited on a plastic substrate. Upon heat treatment, the change of resistance in the printed lines was measured as a function of time and sintering temperatures from 150 to 200 C. A critical temperature was observed for the sintering process, beyond which there was no further reduction in resistance. Analysis shows the critical temperature correlates to the boiling point of the solvent, which is attributed to a liquid-mediated sintering mechanism. It is demonstrated that the sintering process shuts down after the solvent has completely evaporated.

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.

Lightweight Aluminum/Nano composites for Automotive Drive Train Applications

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

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

2012-12-14

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

Pore Space Connectivity and the Transport Properties of Rocks

DOE PAGES

Bernabé, Yves; Li, Min; Tang, Yan-Bing; ...

2016-06-23

Pore connectivity is likely one of the most important factors affecting the permeability of reservoir rocks. Furthermore, connectivity effects are not restricted to materials approaching a percolation transition but can continuously and gradually occur in rocks undergoing geological processes such as mechanical and chemical diagenesis. Here, we compiled sets of published measurements of porosity, permeability and formation factor, performed in samples of unconsolidated granular aggregates, in which connectivity does not change, and in two other materials, sintered glass beads and Fontainebleau sandstone, in which connectivity does change. We compared these data to the predictions of a Kozeny-Carman model of permeability,more » which does not account for variations in connectivity, and to those of Bernabé et al. (2010, 2011) model, which does [Bernabé Y., Li M., Maineult A. (2010) Permeability and pore connectivity: a new model based on network simulations, J. Geophys. Res. 115, B10203; Bernabé Y., Zamora M., Li M., Maineult A., Tang Y.B. (2011) Pore connectivity, permeability and electrical formation factor: a new model and comparison to experimental data, J. Geophys. Res. 116, B11204]. Both models agreed equally well with experimental data obtained in unconsolidated granular media. But, in the other materials, especially in the low porosity samples that had undergone the greatest amount of sintering or diagenesis, only Bernabé et al. model matched the experimental data satisfactorily. In comparison, predictions of the Kozeny-Carman model differed by orders of magnitude. The advantage of the Bernabé et al. model was its ability to account for a continuous, gradual reduction in pore connectivity during sintering or diagenesis. Though we can only speculate at this juncture about the mechanisms responsible for the connectivity reduction, we propose two possible mechanisms, likely to be active at different stages of sintering and diagenesis, and thus allowing the gradual evolution observed experimentally.« less

Pore Space Connectivity and the Transport Properties of Rocks

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

Bernabé, Yves; Li, Min; Tang, Yan-Bing

Pore connectivity is likely one of the most important factors affecting the permeability of reservoir rocks. Furthermore, connectivity effects are not restricted to materials approaching a percolation transition but can continuously and gradually occur in rocks undergoing geological processes such as mechanical and chemical diagenesis. Here, we compiled sets of published measurements of porosity, permeability and formation factor, performed in samples of unconsolidated granular aggregates, in which connectivity does not change, and in two other materials, sintered glass beads and Fontainebleau sandstone, in which connectivity does change. We compared these data to the predictions of a Kozeny-Carman model of permeability,more » which does not account for variations in connectivity, and to those of Bernabé et al. (2010, 2011) model, which does [Bernabé Y., Li M., Maineult A. (2010) Permeability and pore connectivity: a new model based on network simulations, J. Geophys. Res. 115, B10203; Bernabé Y., Zamora M., Li M., Maineult A., Tang Y.B. (2011) Pore connectivity, permeability and electrical formation factor: a new model and comparison to experimental data, J. Geophys. Res. 116, B11204]. Both models agreed equally well with experimental data obtained in unconsolidated granular media. But, in the other materials, especially in the low porosity samples that had undergone the greatest amount of sintering or diagenesis, only Bernabé et al. model matched the experimental data satisfactorily. In comparison, predictions of the Kozeny-Carman model differed by orders of magnitude. The advantage of the Bernabé et al. model was its ability to account for a continuous, gradual reduction in pore connectivity during sintering or diagenesis. Though we can only speculate at this juncture about the mechanisms responsible for the connectivity reduction, we propose two possible mechanisms, likely to be active at different stages of sintering and diagenesis, and thus allowing the gradual evolution observed experimentally.« less

Development of a double-stage DDIA apparatus and its application to in-situ melting experiments at high pressures

NASA Astrophysics Data System (ADS)

Jing, Z.; Wang, Y.; Tange, Y.; Hilairet, N.; Yu, T.; Sakamaki, T.

2010-12-01

Melting experiments at high pressures are critical to our studies on the chemical evolution and dynamics of Earth and other terrestrial planets. A large volume press can generate a homogeneous and stable high-temperature environment, which is the key to melting experiments. However, previous in-situ melting experiments using a large volume press were often restricted to relatively low pressures. In order to expand the P-T conditions, a double-stage 6-8 configuration (6 first-stage anvils and 8 second stage-anvils) has been developed in a DDIA apparatus (DDIA-30), recently installed at the GSECARS Beamline 13-ID-D at the Advanced Photon Source. 27 mm DIA-type first-stage anvils and 14 mm second-stage anvils with the truncation edge length (TEL) of 1.5 mm are employed. A cell assembly that is suitable for synchrotron X-ray studies developed by Tange et al. (2008) has been adopted for melting experiments. High pressure and temperature conditions are generated up to 27 GPa and 2473 K by using tungsten carbide anvils, and up to 35 GPa and 1773 K by using sintered diamond anvils. Both LaCrO3 and TiB2 heater materials have been successfully applied for high-temperature generation. Although TiB2 shows a decrease of resistance at temperatures higher than 2000 K at 20 GPa, we are able to achieve 2473 K with temperature fluctuations in the range of ±30 K. Using tungsten carbide anvils and TiB2 heaters, we have determined the melting curve of gold up to 20 GPa. We constrain the melting temperature based on the disappearance of the gold peaks in energy dispersive X-ray diffraction patterns and the change of sample shape in the radiographic images. The combination of these two observations can reduce the uncertainties in melting temperatures to within 100 K. The measured melting temperatures of gold at 8, 13, and 20 GPa are consistent with the low-pressure results (up to 6 GPa) such as Mirwald and Kennedy (1979). Melting experiments with sintered diamond anvils are currently under development. This will enable us to conduct melting experiments up to 50 GPa on Fe alloys and silicates.

[Influence of repeated sintering on the color of two brands of porcelain-fused-to-titanium].

PubMed

Shu, Cheng-jun; Luo, Xiao-ping; Wu, Lie

2007-08-01

To investigate the influence of repeated sintering on the color of two porcelain-fused-to-titanium, and the differences between the two porcelains. Thirty samples were prepared and sintered for 9 times. The color of samples were measured following sintering 1, 3, 5, 7, 9 times by ShadeEye NCC colorimeter according to two brands of porcelains with CIE1976L*a*b* color system, and calculated relevant chrome, chromatism and hue, and statistical analysis. When two brands of porcelains were sintered 5 times, the color parameters had no significant change and sintered continuely, the color parameters of L* and a* had obvious changes, but can't be observed by eyes. The color parameters of titanium-porcelains have no significant change after repeated sintering.

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

Processing and Characterization of Porous Ti2AlC with Controlled Porosity and Pore Size

DTIC Science & Technology

2012-09-11

fabricated by spark plasma sintering , were also characterized. The effects of porosity and/or pore size on the room temperature elastic moduli...pressureless- sintered without NaCl pore former, or fabricated by spark plasma sintering , were also characterized. The effects of porosity and/or pore size...as well as several samples sintered using spark plasma sintering (SPS). Furthermore, we demon- strate that the developed methodology can be implemented

Thermal Conductivity and Sintering Behavior of Advanced Thermal Barrier Coatings

NASA Technical Reports Server (NTRS)

Zhu, Dongming; Miller, Robert A.

2002-01-01

Advanced thermal barrier coatings, having significantly reduced long-term thermal conductivities, are being developed using an approach that emphasizes real-time monitoring of thermal conductivity under conditions that are engine-like in terms of temperatures and heat fluxes. This is in contrast to the traditional approach where coatings are initially optimized in terms of furnace and burner rig durability with subsequent measurement in the as-processed or furnace-sintered condition. The present work establishes a laser high-heat-flux test as the basis for evaluating advanced plasma-sprayed and physical vapor-deposited thermal barrier coatings under the NASA Ultra Efficient Engine Technology (UEET) Program. The candidate coating materials for this program are novel thermal barrier coatings that are found to have significantly reduced thermal conductivities due to an oxide-defect-cluster design. Critical issues for designing advanced low conductivity coatings with improved coating durability are also discussed.

[Fractographic analysis of clinically failed anterior all ceramic crowns].

PubMed

DU, Qian; Zhou, Min-bo; Zhang, Xin-ping; Zhao, Ke

2012-04-01

To identify the site of crack initiation and propagation path of clinically failed all ceramic crowns by fractographic analysis. Three clinically failed anterior IPS Empress II crowns and two anterior In-Ceram alumina crowns were retrieved. Fracture surfaces were examined using both optical stereo and scanning electron microscopy. Fractographic theory and fracture mechanics principles were applied to disclose the damage characteristics and fracture mode. All the crowns failed by cohesive failure within the veneer on the labial surface. Critical crack originated at the incisal contact area and propagated gingivally. Porosity was found within the veneer because of slurry preparation and the sintering of veneer powder. Cohesive failure within the veneer is the main failure mode of all ceramic crown. Veneer becomes vulnerable when flaws are present. To reduce the chances of chipping, multi-point occlusal contacts are recommended, and layering and sintering technique of veneering layer should also be improved.

Proportional integral derivative, modeling and ways of stabilization for the spark plasma sintering process

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

Manière, Charles; Lee, Geuntak; Olevsky, Eugene A.

The stability of the proportional–integral–derivative (PID) control of temperature in the spark plasma sintering (SPS) process is investigated. The PID regulations of this process are tested for different SPS tooling dimensions, physical parameters conditions, and areas of temperature control. It is shown that the PID regulation quality strongly depends on the heating time lag between the area of heat generation and the area of the temperature control. Tooling temperature rate maps are studied to reveal potential areas for highly efficient PID control. The convergence of the model and experiment indicates that even with non-optimal initial PID coefficients, it is possiblemore » to reduce the temperature regulation inaccuracy to less than 4 K by positioning the temperature control location in highly responsive areas revealed by the finite-element calculations of the temperature spatial distribution.« less

Metallurgical and Mechanical Evaluation of 4340 Steel Produced by Direct Metal Laser Sintering

NASA Astrophysics Data System (ADS)

Jelis, Elias; Clemente, Matthew; Kerwien, Stacey; Ravindra, Nuggehalli M.; Hespos, Michael R.

2015-03-01

Direct metal laser sintering (DMLS) was used to produce high-strength low-alloy 4340 steel specimens. Mechanical and metallurgical analyses were performed on the specimens to determine the samples with the highest strengths and the least porosity. The optimal process parameters were thus defined based on the corresponding experimental conditions. Additionally, the effects of fabricating specimens with both virgin and recycled powders were studied. Scanning electron microscopy and electron-dispersive spectroscopy were performed on both types of powders to determine the starting morphology and composition. The initial tensile results are promising, suggesting that DMLS can produce specimens equal in strength to wrought materials. However, there is evidence of cracking on several of the heat-treated tensile specimens that is unexplained. Several theories point to disturbances in the build chamber environment that went undetected while the specimens were being fabricated.

Tantalum-tungsten oxide thermite composites prepared by sol-gel synthesis and spark plasma sintering

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

Kuntz, Joshua D.; Gash, Alexander E.; Cervantes, Octavio G.

2010-08-15

Energetic composite powders consisting of sol-gel derived nanostructured tungsten oxide were produced with various amounts of micrometer-scale tantalum fuel metal. Such energetic composite powders were ignition-tested and the results show that the powders are not sensitive to friction, spark and/or impact ignition. Initial consolidation experiments, using the High-Pressure Spark Plasma Sintering (HPSPS) technique, on the sol-gel derived nanostructured tungsten oxide produced samples with higher relative density than can be achieved with commercially available tungsten oxide. The sol-gel derived nanostructured tungsten oxide with immobilized tantalum fuel metal (Ta-WO{sub 3}) energetic composite was consolidated to a density of 9.17 g cm{sup -3}more » or 93% relative density. In addition, those samples were consolidated without significant pre-reaction of the constituents, thus retaining their stored chemical energy. (author)« less

Tantalum-Tungsten Oxide Thermite Composite Prepared by Sol-Gel Synthesis and Spark Plasma Sintering

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

Cervantes, O; Kuntz, J; Gash, A

2009-02-13

Energetic composite powders consisting of sol-gel derived nanostructured tungsten oxide were produced with various amounts of micrometer-scale tantalum fuel metal. Such energetic composite powders were ignition tested and results show that the powders are not sensitive to friction, spark and/or impact ignition. Initial consolidation experiments, using the High Pressure Spark Plasma Sintering (HPSPS) technique, on the sol-gel derived nanostructured tungsten oxide produced samples with higher relative density than can be achieved with commercially available tungsten oxide. The sol-gel derived nanostructured tungsten oxide with immobilized tantalum fuel metal (Ta - WO{sub 3}) energetic composite was consolidated to a density of 9.17more » g.cm{sup -3} or 93% relative density. In addition those parts were consolidated without significant pre-reaction of the constituents, thus the sample retained its stored chemical energy.« less

Proportional integral derivative, modeling and ways of stabilization for the spark plasma sintering process

DOE PAGES

Manière, Charles; Lee, Geuntak; Olevsky, Eugene A.

2017-04-21

The stability of the proportional–integral–derivative (PID) control of temperature in the spark plasma sintering (SPS) process is investigated. The PID regulations of this process are tested for different SPS tooling dimensions, physical parameters conditions, and areas of temperature control. It is shown that the PID regulation quality strongly depends on the heating time lag between the area of heat generation and the area of the temperature control. Tooling temperature rate maps are studied to reveal potential areas for highly efficient PID control. The convergence of the model and experiment indicates that even with non-optimal initial PID coefficients, it is possiblemore » to reduce the temperature regulation inaccuracy to less than 4 K by positioning the temperature control location in highly responsive areas revealed by the finite-element calculations of the temperature spatial distribution.« less

The effect of impurities elements on titanium alloy (Ti-6Al-4V) MIM sintered part properties

NASA Astrophysics Data System (ADS)

Ahmad, M. Azmirruddin; Jabir, M.; Johari, N.; Ibrahim, R.; Hamidi, N.

2017-12-01

The titanium alloys (Ti-6Al-4V) compact were fabricated by Metal Injection Molding (MIM). However, the real challenge of MIM processing for titanium alloy is its affinity to be contaminated by interstitial light elements such as oxygen and carbon which could degrade the mechanical properties of sintered titanium alloy such as its tensile strength and ductility. The sintering temperature effect on carbon and oxygen content that affects its physical and mechanical properties of the sintered titanium alloy was studied. The titanium MIM brown specimen was sintered at four different sintering temperatures which are 1100 °C, 1150 °C, 1200 °C and 1250 °C for 4 hours under furnace control atmosphere. The experimental result indicated that the specimen which has been made from 100% gas atomized powder have a relative density of 92.2 % - 97.6 %, the range of porosity percent around 2.38 %-3.84 %. Ultimate tensile strength of 873.11 MPa - 1007.19 MPa and ductility percent in range of 1.89 %-3.46 %. The titanium alloy MIM specimen which was sintered at 1150 °C contained 0.145 % of carbon and 0.143 % of oxygen possess the highest value of density and tensile strength, with value of 4.344 gcm-3 and 1007.2 MPa respectively. Meanwhile, the titanium alloy MIM specimen which was sintered at 1200 °C contains 0.130 % of carbon and 0.127 % of oxygen, has the highest percentage of ductility with 3.46 %. The carbon content level increased as the sintering temperature increased due to decomposition of high molecule weight of residue binder system which could not be eliminated during solvent extraction debinding process and sintered at low temperature. Contrarily, the oxygen content level indicates a decrease as the sintering temperature increased. Briefly, the sintering temperature could influence the physical and mechanical properties of titanium alloy MIM sintered specimen as it influences the oxygen and carbon content level in the alloys.

Debinding and Sintering of an Injection-Moulded Hypereutectic Al⁻Si Alloy.

PubMed

Ni, Jiaqi; Yu, Muhuo; Han, Keqing

2018-05-16

Hypereutectic Al⁻Si (20 wt.%) alloy parts were fabricated by employing a powder injection moulding (PIM) technique with a developed multi-component binder system composed of high-density polyethylene (35 wt.%), carnauba wax (62 wt.%) and stearic acid (3 wt.%). The feedstocks contained 83 wt.% metal powders. The debinding process was carried out by a combination of solvent extraction and thermal decomposition. The effects of solvent debinding variables such as kind of solvents, debinding temperatures and time, and the bulk surface area to volume ratios on the debinding process were investigated. Thermal debinding and the subsequent sintering process were carried out in a heating sequence under a nitrogen atmosphere. The influences of sintering temperature and sintering time on the mechanical properties and structure were considered. Under the optimal sintering condition, sintering at 550 °C for 3 h, the final sintering parts were free of distortion and exhibited good mechanical properties. Relative sintered density, Brinell hardness, and tensile strength were ~95.5%, 58 HBW and ~154, respectively.

Effect of starting powders on the sintering of nanostructured ZrO2 ceramics by colloidal processing

NASA Astrophysics Data System (ADS)

Suárez, Gustavo; Sakka, Yoshio; Suzuki, Tohru S.; Uchikoshi, Tetsuo; Zhu, Xinwen; Aglietti, Esteban F.

2009-04-01

The effect of starting powders on the sintering of nanostructured tetragonal zirconia was evaluated. Suspensions were prepared with a concentration of 10 vol.% by mixing a bicomponent mixture of commercial powders (97 mol.% monoclinic zirconia with 3 mol.% yttria) and by dispersing commercially available tetragonal zirconia (3YTZ, Tosoh). The preparation of the slurry by bead-milling was optimized. Colloidal processing using 50 μm zirconia beads at 4000 rpm generated a fully deagglomerated suspension leading to the formation of high-density consolidated compacts (62% of the theoretical density (TD) for the bicomponent suspension). Optimum colloidal processing of the bicomponent suspension followed by the sintering of yttria and zirconia allowed us to obtain nanostructured tetragonal zirconia. Three different sintering techniques were investigated: normal sintering, two-step sintering and spark plasma sintering. The inhibition of grain growth in the bicomponent mixed powders in comparison with 3YTZ was demonstrated. The inhibition of the grain growth may have been caused by inter-diffusion of cations during the sintering.

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.

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

Microwave processing of a dental ceramic used in computer-aided design/computer-aided manufacturing.

PubMed

Pendola, Martin; Saha, Subrata

2015-01-01

Because of their favorable mechanical properties and natural esthetics, ceramics are widely used in restorative dentistry. The conventional ceramic sintering process required for their use is usually slow, however, and the equipment has an elevated energy consumption. Sintering processes that use microwaves have several advantages compared to regular sintering: shorter processing times, lower energy consumption, and the capacity for volumetric heating. The objective of this study was to test the mechanical properties of a dental ceramic used in computer-aided design/computer-aided manufacturing (CAD/CAM) after the specimens were processed with microwave hybrid sintering. Density, hardness, and bending strength were measured. When ceramic specimens were sintered with microwaves, the processing times were reduced and protocols were simplified. Hardness was improved almost 20% compared to regular sintering, and flexural strength measurements suggested that specimens were approximately 50% stronger than specimens sintered in a conventional system. Microwave hybrid sintering may preserve or improve the mechanical properties of dental ceramics designed for CAD/CAM processing systems, reducing processing and waiting times.

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 MICROWAVE SINTERING ON THE STRUCTURAL AND ELECTRICAL PROPERTIES OF Li0.51Zn0.2Ti0.2V0.01Fe2.08O4 FERRITE

NASA Astrophysics Data System (ADS)

Maisnam, Mamata; Phanjoubam, Sumitra

2013-07-01

Effect of microwave sintering on the structural and electrical properties of Li+0.51Zn2+0.2Ti4+0.2V5+0.01Fe3+2.08O2-4 is studied in comparison with that of conventionally sintered one. The technique is advantageous in terms of significantly reduced size of microwave kilns and rapid heating compared to the cumbersome and slow heating of conventional sintering technology. Microwave sintering produced enhanced densification and much finer microstructures. The DC resistivity is markedly increased. Microwave sintering reduces chances of evaporation of lithium and oxygen during sintering of lithium based ferrites resulting in formation of lesser ferrous ions. This has profound effect on the electrical properties of microwave sintered ferrites. The dielectric constant is significantly reduced possibly due to reduced space charge polarization and the temperature dependence of the dielectric properties are also studied.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

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.

Enhanced Densification and Hardness of Titanium Bodies Sintered by Advanced Hydrogen Sintering Process

NASA Astrophysics Data System (ADS)

Oh, Jung-Min; Koo, Ja-Geon; Lim, Jae-Won

2018-05-01

A new sintering technique for enhancing a densification and hardness of sintered titanium body by supplying hydrogen was developed (Hydrogen Sintering Process, HSP). The HSP was developed by only injecting hydrogen into an argon atmosphere during the core time. As a result, sound titanium sintered bodies with high density and hardness were obtained by the HSP. In addition, a pore size and number of the HSP specimens were smaller than those of the argon atmosphere specimen. It was found that the injecting hydrogen into the argon atmosphere by HSP can prevent the formation of oxide layers, resulting in enhanced densification and hardness.

Rapid sintering of anisotropic, nanograined Nd-Fe-B by flash-spark plasma sintering

NASA Astrophysics Data System (ADS)

Castle, Elinor; Sheridan, Richard; Grasso, Salvatore; Walton, Allan; Reece, Mike

2016-11-01

A Spark Plasma Sintering (SPS) furnace was used to Flash-Sinter (FS) Nd-Fe-Dy-Co-B-Ga melt spun permanent magnetic material. During the 10 s "Flash" process (heating rate 2660 K min-1), sample sintering (to theoretical density) and deformation (54% height reduction) occurred. This produced texturing and significant magnetic anisotropy, comparable to conventional die-upset magnets; yet with much greater coercivities (>1600 kA m-1) due to the nanoscale characteristics of the plate-like sintered grains. These preliminary results suggest that Flash-SPS could provide a new processing route for the mass production of highly anisotropic, nanocrystalline magnetic materials with high coercivity.

Solvent/non-solvent sintering: a novel route to create porous microsphere scaffolds for tissue regeneration.

PubMed

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

2008-08-01

Solvent/non-solvent sintering creates porous polymeric microsphere scaffolds suitable for tissue engineering purposes with control over the resulting porosity, average pore diameter, and mechanical properties. Five different biodegradable biocompatible polyphosphazenes exhibiting glass transition temperatures from -8 to 41 degrees C and poly (lactide-co-glycolide), (PLAGA) a degradable polymer used in a number of biomedical settings, were examined to study the versatility of the process and benchmark the process to heat sintering. Parameters such as: solvent/non-solvent sintering solution composition and submersion time effect the sintering process. PLAGA microsphere scaffolds fabricated with solvent/non-solvent sintering exhibited an interconnected porosity and pore size of 31.9% and 179.1 mum, respectively which was analogous to that of conventional heat sintered PLAGA microsphere scaffolds. Biodegradable polyphosphazene microsphere scaffolds exhibited a maximum interconnected porosity of 37.6% and a maximum compressive modulus of 94.3 MPa. Solvent/non-solvent sintering is an effective strategy for sintering polymeric microspheres, with a broad spectrum of glass transition temperatures, under ambient conditions making it an excellent fabrication route for developing tissue engineering scaffolds and drug delivery vehicles. (c) 2007 Wiley Periodicals, Inc.

Solvent/Non-Solvent Sintering: A Novel Route to Create Porous Microsphere Scaffolds For Tissue Regeneration

PubMed Central

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

2009-01-01

Solvent/non-solvent sintering creates porous polymeric microsphere scaffolds suitable for tissue engineering purposes with control over the resulting porosity, average pore diameter and mechanical properties. Five different biodegradable biocompatible polyphosphazenes exhibiting glass transition temperatures from −8°C to 41oC and poly(lactide-co-glycolide), (PLAGA) a degradable polymer used in a number of biomedical settings, were examined to study the versatility of the process and benchmark the process to heat sintering. Parameters such as: solvent/non-solvent sintering solution composition and submersion time effect the sintering process. PLAGA microsphere scaffolds fabricated with solvent/non-solvent sintering exhibited an interconnected porosity and pore size of 31.9% and 179.1µm respectively which was analogous to that of conventional heat sintered PLAGA microsphere scaffolds. Biodegradable polyphosphazene microsphere scaffolds exhibited a maximum interconnected porosity of 37.6% and a maximum compressive modulus of 94.3MPa. Solvent/non-solvent sintering is an effective strategy for sintering polymeric microspheres, with a broad spectrum of glass transition temperatures, under ambient conditions making it an excellent fabrication route for developing tissue engineering scaffolds and drug delivery vehicles. PMID:18161819

An Investigation of Sintering Parameters on Titanium Powder for Electron Beam Melting Processing Optimization.

PubMed

Drescher, Philipp; Sarhan, Mohamed; Seitz, Hermann

2016-12-01

Selective electron beam melting (SEBM) is a relatively new additive manufacturing technology for metallic materials. Specific to this technology is the sintering of the metal powder prior to the melting process. The sintering process has disadvantages for post-processing. The post-processing of parts produced by SEBM typically involves the removal of semi-sintered powder through the use of a powder blasting system. Furthermore, the sintering of large areas before melting decreases productivity. Current investigations are aimed at improving the sintering process in order to achieve better productivity, geometric accuracy, and resolution. In this study, the focus lies on the modification of the sintering process. In order to investigate and improve the sintering process, highly porous titanium test specimens with various scan speeds were built. The aim of this study was to decrease build time with comparable mechanical properties of the components and to remove the residual powder more easily after a build. By only sintering the area in which the melt pool for the components is created, an average productivity improvement of approx. 20% was achieved. Tensile tests were carried out, and the measured mechanical properties show comparatively or slightly improved values compared with the reference.

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

NASA Astrophysics Data System (ADS)

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

2015-05-01

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

An Arrhenius-type viscosity function to model sintering using the Skorohod Olevsky viscous sintering model within a finite element code.

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

Ewsuk, Kevin Gregory; Arguello, Jose Guadalupe, Jr.; Reiterer, Markus W.

2006-02-01

The ease and ability to predict sintering shrinkage and densification with the Skorohod-Olevsky viscous sintering (SOVS) model within a finite-element (FE) code have been improved with the use of an Arrhenius-type viscosity function. The need for a better viscosity function was identified by evaluating SOVS model predictions made using a previously published polynomial viscosity function. Predictions made using the original, polynomial viscosity function do not accurately reflect experimentally observed sintering behavior. To more easily and better predict sintering behavior using FE simulations, a thermally activated viscosity function based on creep theory was used with the SOVS model. In comparison withmore » the polynomial viscosity function, SOVS model predictions made using the Arrhenius-type viscosity function are more representative of experimentally observed viscosity and sintering behavior. Additionally, the effects of changes in heating rate on densification can easily be predicted with the Arrhenius-type viscosity function. Another attribute of the Arrhenius-type viscosity function is that it provides the potential to link different sintering models. For example, the apparent activation energy, Q, for densification used in the construction of the master sintering curve for a low-temperature cofire ceramic dielectric has been used as the apparent activation energy for material flow in the Arrhenius-type viscosity function to predict heating rate-dependent sintering behavior using the SOVS model.« less

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

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

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

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

Effect of temperature on porosity of iron ore sinter with biochar derived from EFB

NASA Astrophysics Data System (ADS)

Purwanto, H.; Rozhan, A. N.; Zakiyuddin, A.; Mohamad, A. S.

2018-01-01

In this research, the replacement of fossil fuel energy (coke) with oil palm empty fruit bunch as a potential energy in sintering of iron ore was investigated. Carbon derived biomass has been produced by using oil palm empty fruit bunch by heat treatment process. In the present investigation, sintering process was carried out by heating the mixed iron ore and biochar at various temperatures. The apparent density and porosity for iron sinter show a significant increase and gradual decrement as the temperature increase, respectively. The porosity of iron sinter shows a gradual decrement from 950 °C to 1050 °C but up to 1150 °C it shows a significant decrement about 44%. Inferring to the micrograph, the agglomeration and assimilation of sinter at high temperature is better compared with low sintering temperature.

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

The physical chemistry and materials science behind sinter-resistant catalysts.

PubMed

Dai, Yunqian; Lu, Ping; Cao, Zhenming; Campbell, Charles T; Xia, Younan

2018-06-18

Catalyst sintering, a main cause of the loss of catalytic activity and/or selectivity at high reaction temperatures, is a major concern and grand challenge in the general area of heterogeneous catalysis. Although all heterogeneous catalysts are inevitably subjected to sintering during their operation, the immediate and drastic consequences can be mitigated by carefully engineering the catalytic particles and their interactions with the supports. In this tutorial review, we highlight recent progress in understanding the physical chemistry and materials science involved in sintering, including the discussion of advanced techniques, such as in situ microscopy and spectroscopy, for investigating the sintering process and its rate. We also discuss strategies for the design and rational fabrication of sinter-resistant catalysts. Finally, we showcase recent success in improving the thermal stability and thus sinter resistance of supported catalytic systems.

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.

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

Reaction bonded silicon nitride prepared from wet attrition-milled silicon. [fractography

NASA Technical Reports Server (NTRS)

Herball, T. P.; Glasgow, T. K.; Shaw, N. J.

1980-01-01

Silicon powder wet milled in heptane was dried, compacted into test bar shape, helium-sintered, and then reaction bonded in nitrogen-4 volume percent hydrogen. As-nitrided bend strengths averaged approximately 290 MPa at both room temperature and 1400 C. Fracture initiation appeared to be associated with subsurface flaws in high strength specimens and both subsurface and surface flaws in low strength specimens.

Reaction bonded silicon nitride prepared from wet attrition-milled silicon

NASA Technical Reports Server (NTRS)

Herbell, T. P.; Glasgow, T. K.; Shaw, N. J.

1980-01-01

Silicon powder wet milled in heptane was dried, compacted into test bar shape, helium-sintered, and then reaction bonded in nitrogen-4 vol% hydrogen. As-nitrided bend strengths averaged approximately 290 MPa at both room temperature and 1400 C. Fracture initiation appeared to be associated with subsurface flaws in high-strength specimens and both subsurface and surface flaws in low-strength specimens.

40 CFR 63.7824 - What test methods and other procedures must I use to establish and demonstrate initial compliance...

Code of Federal Regulations, 2010 CFR

2010-07-01

... select sampling port locations and the number of traverse points. Sampling ports must be located at the... Method 25 (40 CFR part 60, appendix A), milligrams per dry standard cubic meters (mg/dscm) for each day... = Conversion factor (mg/lb); and K = Daily production rate of sinter, tons/hr. (4) Continue the sampling and...

40 CFR 63.7824 - What test methods and other procedures must I use to establish and demonstrate initial compliance...

Code of Federal Regulations, 2011 CFR

2011-07-01

... select sampling port locations and the number of traverse points. Sampling ports must be located at the... Method 25 (40 CFR part 60, appendix A), milligrams per dry standard cubic meters (mg/dscm) for each day... = Conversion factor (mg/lb); and K = Daily production rate of sinter, tons/hr. (4) Continue the sampling and...

Zirconium Carbide Produced by Spark Plasma Sintering and Hot Pressing: Densification Kinetics, Grain Growth, and Thermal Properties

PubMed Central

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

2016-01-01

Spark plasma sintering (SPS) has been employed to consolidate a micron-sized zirconium carbide (ZrC) powder. ZrC pellets with a variety of relative densities are obtained under different processing parameters. The densification kinetics of ZrC powders subjected to conventional hot pressing and SPS are comparatively studied by applying similar heating and loading profiles. Due to the lack of electric current assistance, the conventional hot pressing appears to impose lower strain rate sensitivity and higher activation energy values than those which correspond to the SPS processing. A finite element simulation is used to analyze the temperature evolution within the volume of ZrC specimens subjected to SPS. The control mechanism for grain growth during the final SPS stage is studied via a recently modified model, in which the grain growth rate dependence on porosity is incorporated. The constant pressure specific heat and thermal conductivity of the SPS-processed ZrC are determined to be higher than those reported for the hot-pressed ZrC and the benefits of applying SPS are indicated accordingly. PMID:28773697

Zirconium Carbide Produced by Spark Plasma Sintering and Hot Pressing: Densification Kinetics, Grain Growth, and Thermal Properties

DOE PAGES

Wei, Xialu; Back, Christina; Izhvanov, Oleg; ...

2016-07-14

Spark plasma sintering (SPS) has been employed to consolidate a micron-sized zirconium carbide (ZrC) powder. ZrC pellets with a variety of relative densities are obtained under different processing parameters. The densification kinetics of ZrC powders subjected to conventional hot pressing and SPS are comparatively studied by applying similar heating and loading profiles. Due to the lack of electric current assistance, the conventional hot pressing appears to impose lower strain rate sensitivity and higher activation energy values than those which correspond to the SPS processing. A finite element simulation is used to analyze the temperature evolution within the volume of ZrCmore » specimens subjected to SPS. The control mechanism for grain growth during the final SPS stage is studied via a recently modified model, in which the grain growth rate dependence on porosity is incorporated. Finally, the constant pressure specific heat and thermal conductivity of the SPS-processed ZrC are determined to be higher than those reported for the hot-pressed ZrC and the benefits of applying SPS are indicated accordingly.« less

Ce:YAG ceramics: the influence of the synthesis technology features on the luminescent and the optical properties

NASA Astrophysics Data System (ADS)

Lukyashin, K. E.; Shitov, V. A.; Medvedev, A. I.; Ishchenko, A. V.; Shevelev, V. S.; Shulgin, B. V.; Basyrova, L. R.

2018-04-01

In this paper, we report on the dependence of the luminescent and the optical properties on the synthesis conditions of the transparent 0.1 at.% Ce:YAG and 1 at.% Ce:YAG ceramics. The ceramics were produced from the nanopowders with a diameter of about 10–15 nm by means of the laser method. The fundamental difference between the two described methods is in the synthesis of the main phase YAG: directly during the vacuum sintering (1 – the first method) and before the vacuum sintering (2 – the second method). For this purpose, the transparent samples (Ø10×2 mm) with the optical transmittance ranging from 58 to 82% at the wavelength of 600 nm were obtained. The first method was proven to be the most preferable in terms of the exact dosage of the dopant which gives the samples the best scintillation characteristics. In a point of fact atom of cerium can potentially leave the material at any or at a certain stage of the ceramics synthesis, reducing the total concentration of Ce3+ in YAG.

Fabrication of porous silicon nitride ceramics using binder jetting technology

NASA Astrophysics Data System (ADS)

Rabinskiy, L.; Ripetsky, A.; Sitnikov, S.; Solyaev, Y.; Kahramanov, R.

2016-07-01

This paper presents the results of the binder jetting technology application for the processing of the Si3N4-based ceramics. The difference of the developed technology from analogues used for additive manufacturing of silicon nitride ceramics is a method of the separate deposition of the mineral powder and binder without direct injection of suspensions/slurries. It is assumed that such approach allows reducing the technology complexity and simplifying the process of the feedstock preparation, including the simplification of the composite materials production. The binders based on methyl ester of acrylic acid with polyurethane and modified starch were studied. At this stage of the investigations, the technology of green body's fabrication is implemented using a standard HP cartridge mounted on the robotic arm. For the coordinated operation of the cartridge and robot the specially developed software was used. Obtained green bodies of silicon powder were used to produce the ceramic samples via reaction sintering. The results of study of ceramics samples microstructure and composition are presented. Sintered ceramics are characterized by fibrous α-Si3N4 structure and porosity up to 70%.

Microstructural changes in NiFe{sub 2}O{sub 4} ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

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

Chauhan, Lalita, E-mail: chauhan.lalita5@gmail.com; Sreenivas, K.; Bokolia, Renuka

2016-05-23

Structural properties of Nickel ferrite (NiFe{sub 2}O{sub 4}) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe{sub 2}O{submore » 4} powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe{sub 2}O{sub 4} ceramics with a uniform microstructure and a large grain size.« less

Microscopy of Alloy Formation on Arc Plasma Sintered Oxide Dispersion Strengthen (ODS) Steel

NASA Astrophysics Data System (ADS)

Bandriyana, B.; Sujatno, A.; Salam, R.; Dimyati, A.; Untoro, P.

2017-07-01

The oxide dispersed strengthened (ODS) alloys steel developed as structure material for nuclear power plants (NPP) has good resistant against creep due to their unique microstructure. Microscopy investigation on the microstructure formation during alloying process especially at the early stages was carried out to study the correlation between structure and property of ODS alloys. This was possible thanks to the arc plasma sintering (APS) device which can simulate the time dependent alloying processes. The ODS sample with composition of 88 wt.% Fe and 12 wt.% Cr powder dispersed with 1 wt.% ZrO2 nano powder was mixed in a high energy milling, isostatic compressed to form sample coins and then alloyed in APS. The Scanning Electron Microscope (SEM) with X-ray Diffraction Spectroscopy (EDX) line scan and mapping was used to characterize the microstructure and elemental composition distribution of the samples. The alloying process with unification of each Fe and Cr phase continued by the alloying formation of Fe-Cr by inter-diffusion of both Fe and Cr and followed by the improvement of the mechanical properties of hardness.

Bioactive Glasses with Low Ca/P Ratio and Enhanced Bioactivity

PubMed Central

Araújo, Marco; Miola, Marta; Baldi, Giovanni; Perez, Javier; Verné, Enrica

2016-01-01

Three new silica-based glass formulations with low molar Ca/P ratio (2–3) have been synthesized. The thermal properties, the crystalline phases induced by thermal treatments and the sintering ability of each glass formulation have been investigated by simultaneous differential scanning calorimetry-thermogravimetric analysis (DSC-TG), X-ray diffraction (XRD) and hot stage microscopy (HSM). The glasses exhibited a good sintering behavior, with two samples achieving shrinkage of 85%–95% prior to crystallization. The bioactivity of the glasses in simulated body fluid (SBF) has been investigated by performing XRD and Fourier transform infrared spectroscopy (FTIR) on the samples prior and after immersion. The glasses with lower MgO contents were able to form a fully crystallized apatite layer after three days of immersion in simulated body fluid (SBF), while for the glass exhibiting a higher MgO content in its composition, the crystallization of the Ca–P layer was achieved after seven days. The conjugation of these properties opens new insights on the synthesis of highly bioactive and mechanically strong prosthetic materials. PMID:28773350

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

NASA Astrophysics Data System (ADS)

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

2002-02-01

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

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.

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.

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.

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.

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

Preparation and characterization of novel foamed porous glass-ceramics

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

Sasmal, Nibedita; Garai, Mrinmoy; Karmakar, Basudeb, E-mail: basudebk@cgcri.res.in

2015-05-15

Foamed glass-ceramics without using foaming agent have been synthesized in a novel glass system of SrO-CaO-Al{sub 2}O{sub 3}-TiO{sub 2}-B{sub 2}O{sub 3}-SiO{sub 2}-P{sub 2}O{sub 5}-M{sub x}O{sub y} (where M = Ba, Mg, La, Ce and Ni) by a simple process of powder sintering. The glass and glass-ceramics are characterized by dilatometry, differential scanning calorimetry (DSC), heating stage microscopy (HSM), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), optical microscopy and Fourier transformed infrared spectroscopy (FTIR). All the glasses formed are amorphous and the glass transition temperature and dilatometric softening temperature of these glasses are found to be in the rangemore » 673–678 °C and 706–728 °C respectively. The glasses are highly stable as indicated by the DSC evaluated glass stability parameters of the range 195–240 °C. Quantitative sintering study of glass powder compacts revealed swelling in the samples with NiO and CeO{sub 2} corresponding to a geometry change of 75 and 108% around 900 °C respectively. With reference to this finding the glass powder compacts are heated to 900 °C and the foamed glass-ceramics are obtained. Characteristic crystalline silicate phases have been identified in the XRD studies and their microstructures are recorded by FESEM. Optical microscope study of the foamed samples revealed formation of bigger foamed cavity with residual pores in samples with NiO and CeO{sub 2} in comparison to samples with BaO, MgO and La{sub 2}O{sub 3}. The mean pore diameters of the samples with NiO and CeO{sub 2} are determined to be 43 and 32 μm, and their respective porosities are 2.34 and 1.82 cm{sup 3}/g respectively. Thus NiO and CeO{sub 2} are found to be very effective to obtain foamed glass-ceramics without using foaming agent by the viscous flow sintering of fine glass powder compacts along with the reduction of the respective polyvalent ions. - Highlights: • Synthesis of foamed porous glass-ceramics without foaming agent by sintering method • Only powder compact yielded foamed porous glass-ceramics but bulk glass did not. • Glasses containing NiO and CeO{sub 2} exhibited significant foaming efficiency. • Bloating of entrapped gas during viscous flow sintering is the origin of foaming. • Residual void created pores in the sintered glass-ceramics as evidenced in FESEM.« less

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.

40 CFR 63.1543 - Standards for process and process fugitive sources.

Code of Federal Regulations, 2012 CFR

2012-07-01

... paragraphs (a)(1) through (9) of this section. (1) Sinter machine; (2) Blast furnace; (3) Dross furnace; (4... machine charging location; (7) Sinter machine discharge end; (8) Sinter crushing and sizing equipment; and (9) Sinter machine area. (b) No owner or operator of any existing, new, or reconstructed primary lead...

40 CFR 63.1543 - Standards for process and process fugitive sources.

Code of Federal Regulations, 2014 CFR

2014-07-01

... paragraphs (a)(1) through (9) of this section. (1) Sinter machine; (2) Blast furnace; (3) Dross furnace; (4... machine charging location; (7) Sinter machine discharge end; (8) Sinter crushing and sizing equipment; and (9) Sinter machine area. (b) No owner or operator of any existing, new, or reconstructed primary lead...

40 CFR 63.1543 - Standards for process and process fugitive sources.

Code of Federal Regulations, 2013 CFR

2013-07-01

... paragraphs (a)(1) through (9) of this section. (1) Sinter machine; (2) Blast furnace; (3) Dross furnace; (4... machine charging location; (7) Sinter machine discharge end; (8) Sinter crushing and sizing equipment; and (9) Sinter machine area. (b) No owner or operator of any existing, new, or reconstructed primary lead...

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...

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

NASA Astrophysics Data System (ADS)

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

2014-05-01

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

Evaluation of Sintering Behaviors of Saprolitic Nickeliferous Laterite Based on Quaternary Basicity

NASA Astrophysics Data System (ADS)

Luo, Jun; Li, Guanghui; Rao, Mingjun; Zhang, Yuanbo; Peng, Zhiwei; Zhi, Qian; Jiang, Tao

2015-09-01

The sintering behaviors of saprolitic nickeliferous laterite with various quaternary basicities [(CaO + MgO)/(SiO2 + Al2O3) mass ratio] in a reductive atmosphere are investigated by simulative sintering and validated by sintering pot tests. The simulative sintering results show that the generation of diopside (CaMgSi2O6) with low melting point is the key reason for the decrease in characteristic fusion temperatures when the quaternary basicity increases from 0.5 to 0.8-1.0. Continuous increase of basicity leads to transformation of diopside (CaMgSi2O6) into akermanite (Ca2MgSi2O7), which adversely increases the characteristic fusion temperatures. These findings are confirmed by the sinter pot tests, which demonstrate that the sintering indexes including vertical sintering velocity (VSV), yield ( Y), and productivity ( P), can be improved by optimizing quaternary basicity. At basicity of 1.0, the VSV, Y, P, and ISO tumbling index reach 49.2 mm/min, 80.5%, 1.0 t/(h m2), and 66.5%, respectively.

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

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

NASA Astrophysics Data System (ADS)

Zhou, Jian; Tang, Hongbo

2018-05-01

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

Study of sintering behavior of vapor forms of 1-octanethiol coated copper nanoparticles for application to ink-jet printing technology.

PubMed

Kwon, Jinhyeong; Park, Shinyoung; Haque, Md Mominul; Kim, Young-Seok; Lee, Caroline Sunyong

2012-04-01

Sub-50 nm copper nanoparticles coated with sub-5 nm 1-octanethiol layer for oxidation inhibition were examined to confirm the 1-octanethiol removal temperature as the sub-50 nm copper nanoparticles are sintered. As a result, 1-octanethiol Self-Assembled Multi-layers (SAMs) on sub-50 nm copper nanoparticles were successfully removed before sintering of copper nanoparticles so that a high density of copper line could be obtained. Finally, the line resistivity was measured and compared to verify the effect of sintering in different atmospheres. As a result, electrical resistivity of the copper pattern sintered in hydrogen atmosphere was measured at 6.96 x 10(-6) ohm-cm whereas that of the copper pattern sintered in mixed gas atmosphere was measured at 2.62 x 10(-5) ohm-cm. Thus, sintering of copper patterns was successfully done to show low electrical resistivity values. Moreover, removal of 1-octanethiol coating after sintering process was confirmed using X-ray photoelectron spectroscopy (XPS) analysis. By showing no sulfur content, XPS results indicate that 1-octanethiol is completely removed. Therefore, the vapor form of 1-octanethiol coating layers can be safely used as an oxidation inhibition layer for low temperature sintering processes and ink-jet applications.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

Hot-spring sinter deposits in the Alvord-Pueblo Valley, Harney County, Oregon

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

Cummings, M.L.; St. John, A.M.

1993-04-01

Silica sinter deposits occur at Borax Lake, Alvord Hot Springs, and Mickey Springs in the Alvord-Pueblo Valley. Although the sinter deposits occur in areas of active hot springs, sinter is not being deposited. Hot springs are localized along faults that have been active since the Pleistocene. The sinter deposits formed after the drying of glacial Lake Alvord, but before and during extensive wind deflation of glacial-lacustrine sediments. At Mickey Springs, sinter rests directly on unaltered, unconsolidated lithic-rich sand. At Borax Lake, sinter overlies unaltered diatomite, but some armoring, presumably by silica, of the 30 m vent has developed. Field relationsmore » suggest rapid dumping of silica from solution without alteration of the country rock at the vent. Discharge of thermal fluids and cold groundwater along the same structure may have produced colloidal silica carried in a solution stripped of dissolved silica. Sinter is composed of opal-a, traces of detrital feldspar and quartz, and evaporation-related boracite. The concentration of Sb is similar among the three sinter deposits (20 to 70 ppm); however, As, Cs, and Br are highest at Borax Lake (5 to 560 ppm; 26 to 118 ppm; 5 to 1,040 ppm) while Hg is highest at Mickey Springs (1.0 to 5.2 ppm).« less

Pressure-assisted low-temperature sintering for paper-based writing electronics.

PubMed

Xu, L Y; Yang, G Y; Jing, H Y; Wei, J; Han, Y D

2013-09-06

With the aim of preparing paper-based writing electronics, a kind of conductive pen was made with nano-silver ink as the conductive component and a rollerball pen as the writing implement. This was used to direct-write conductive patterns on Epson photo paper. In order to decrease the sintering temperature, pressure was introduced to enhance the driving forces for sintering. Compared with hot sintering without pressure, hot-pressure can effectively improve the conductivity of silver coatings, reduce the sintering time and thus improve productivity. Importantly, pressure can achieve a more uniform and denser microstructure, which increases the connection strength of the silver coating. At the optimum hot-pressure condition (sintering temperature 120 ° C/sintering pressure 25 MPa/sintering time 15 min), a typical measured resistivity value was 1.43 × 10⁻⁷ Ω m, nine greater than that of bulk silver. This heat treatment process is compatible with paper and does not cause any damage to the paper substrates. Even after several thousand bending cycles, the resistivity values of writing tracks by hot-pressure sintering stay almost the same (from 1.43 × 10⁻⁷ to 1.57 × 10⁻⁷ Ω m). The stability and flexibility of the writing circuits are good, which demonstrates the promising future of writing electronics.

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.

Preparation of Porous Stainless Steel Hollow-Fibers through Multi-Modal Particle Size Sintering towards Pore Engineering

PubMed Central

Allioux, Francois-Marie; Etxeberria Benavides, Miren

2017-01-01

The sintering of metal powders is an efficient and versatile technique to fabricate porous metal elements such as filters, diffusers, and membranes. Neck formation between particles is, however, critical to tune the porosity and optimize mass transfer in order to minimize the densification process. In this work, macro-porous stainless steel (SS) hollow-fibers (HFs) were fabricated by the extrusion and sintering of a dope comprised, for the first time, of a bimodal mixture of SS powders. The SS particles of different sizes and shapes were mixed to increase the neck formation between the particles and control the densification process of the structure during sintering. The sintered HFs from particles of two different sizes were shown to be more mechanically stable at lower sintering temperature due to the increased neck area of the small particles sintered to the large ones. In addition, the sintered HFs made from particles of 10 and 44 μm showed a smaller average pore size (<1 μm) as compared to the micron-size pores of sintered HFs made from particles of 10 μm only and those of 10 and 20 μm. The novel HFs could be used in a range of applications, from filtration modules to electrochemical membrane reactors. PMID:28777352

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.

Estimation of Sintering Kinetics of Oxidized Magnetite Pellet Using Optical Dilatometer

NASA Astrophysics Data System (ADS)

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

2015-04-01

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

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 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.

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

Time-resolved in situ XAS study of the preparation of supported gold clusters.

PubMed

Bus, Eveline; Prins, Roel; van Bokhoven, Jeroen A

2007-07-07

Incipient-wetness impregnation of gamma-Al(2)O(3) with HAuCl(4) and subsequent removal of chlorine with NaOH, and deposition-precipitation of HAuCl(4) on TiO(2) at pH 7 resulted in supported Au(3+) species. Time-resolved in situ XAS at the Au L(3) edge showed that the Al(2)O(3)-supported oxidic or hydroxidic species were reduced in hydrogen at 440 K to yield small metallic gold clusters. The Au(3+) precursor decomposed to metallic gold in inert atmosphere at 573 K and in oxidizing atmosphere above 623 K. In all atmospheres, initially small clusters were formed that gradually grew with increasing temperature. The TiO(2)-supported species were considerably less stable. In hydrogen and carbon monoxide, Au(0) clusters of 1 to 1.5 nm were formed at room temperature, which was the lowest temperature studied. In inert and oxidizing atmosphere, the Au(3+) precursor decomposed fully to metallic gold at 530 K, as shown by XAS and temperature-programmed experiments. Large clusters were obtained already in the initial stage of reduction. Residual chlorine inhibited the reduction and led to sintering of the gold clusters. Exposure of the TiO(2)-supported catalyst precursor to light or the X-ray beam led to partial reduction, and STEM showed that storage of the reduced gold clusters under ambient conditions led to agglomeration and bimodal cluster-size distributions.

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.

Energy-Saving Sintering of Electrically Conductive Powders by Modified Pulsed Electric Current Heating Using an Electrically Nonconductive Die

NASA Astrophysics Data System (ADS)

Ito, Mikio; Kawahara, Kenta; Araki, Keita

2014-04-01

Sintering of Cu and thermoelectric Ca3Co4O9 was tried using a modified pulsed electric current sintering (PECS) process, where an electrically nonconductive die was used instead of a conventional graphite die. The pulsed electric current flowed through graphite punches and sample powder, which caused the Joule heating of the powder compact itself, resulting in sintering under smaller power consumption. Especially for the Ca3Co4O9 powder, densification during sintering was also accelerated by this modified PECS process.

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.

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.

Manufacture of high-density ceramic sinters

NASA Technical Reports Server (NTRS)

Hibata, Y.

1986-01-01

High density ceramic sinters are manufactured by coating premolded or presintered porous ceramics with a sealing material of high SiO2 porous glass or nitride glass and then sintering by hot isostatic pressing. The ceramics have excellent abrasion and corrosion resistances. Thus LC-10 (Si3N2 powder) and Y2O3-Al2O3 type sintering were mixed and molded to give a premolded porous ceramic (porosity 37%, relative bulk density 63%). The ceramic was dipped in a slurry containing high SiO2 porous glass and an alcohol solution of cellulose acetate and dried. The coated ceramic was treated in a nitrogen atmosphere and then sintered by hot isostatic pressing to give a dense ceramic sinter.

Improved toughness of silicon carbide

NASA Technical Reports Server (NTRS)

Palm, J. A.

1976-01-01

Impact energy absorbing layers (EALs) comprised of partially densified silicon carbide were formed in situ on fully sinterable silicon carbide substrates. After final sintering, duplex silicon carbide structures resulted which were comprised of a fully sintered, high density silicon carbide substrate or core, overlayed with an EAL of partially sintered silicon carbide integrally bonded to its core member. Thermal cycling tests proved such structures to be moderately resistant to oxidation and highly resistant to thermal shock stresses. The strength of the developed structures in some cases exceeded but essentially it remained the same as the fully sintered silicon carbide without the EAL. Ballistic impact tests indicated that substantial improvements in the toughness of sintered silicon carbide were achieved by the use of the partially densified silicon carbide EALs.

The effect of aging treatment on the fracture toughness and impact strength of injection molded Ni-625 superalloy parts

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

Özgün, Özgür, E-mail: oozgun@bingol.edu.tr; Yılmaz, Ramazan; Özkan Gülsoy, H.

In this study, the effect of aging heat treatment on fracture toughness and impact strength of Ni-625 superalloy fabricated by using powder injection molding (PIM) method was examined. After a feedstock was prepared by mixing the prealloyed Ni-625 superalloy powder, which was fabricated by gas atomisation, with a polymeric binder system and then it was granulated, it was shaped through the use of injection. The molded specimens were sintered at 1300 °C for 3 h after a two-stage debinding process. Once the sintered specimens were treated in the solution at 1150 °C for 2 h, they were quenched. Aging treatmentmore » was performed by keeping specimens at 745 °C for 22 h. Fracture toughness and impact tests were performed on sintered and aged specimens. Microstructure examinations were performed by using optical microscope, scanning electron microscope, and transmission electron microscope. The results revealed that aging heat treatment led to the formation of some carbides and intermetallic phases in the microstructure. While the hardness of the aged specimens increased due to these phases, their fracture toughness and impact strength values decreased. - Highlights: • Ni-625 superalloy components were produced by means of powder injection molding. • The produced components were subjected to aging treatment. • Aging process provided approximately 50% increase in the hardness of components. • Intermetallic precipitates, carbides and TCP phases occurred within the aged parts. • Fracture toughness and impact strength values decreased due to the hard phases.« less

Spark Plasma Sintering for Nanostructured Smart Materials

DTIC Science & Technology

2009-03-02

polyester) with excess isocyanate to form a prepolymer , followed by the addition of a short chain diol that acts as a chain extender to link the... prepolymers together. Due to the thermodynamic imicisibility of segments of PU, phase separation into a flexible soft segment (long chain diol) and a...other reactions of the isocyanate groups with the other functional groups in the chain. [Hepburn, 1992] However, during the initial prepolymer

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.

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

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

Rahman, Md Taibur; McCloy, John; Panat, Rahul, E-mail: rahul.panat@wsu.edu, E-mail: rvchintalapalle@utep.edu

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24–500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasingmore » trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.« less

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

Nenoff, Tina M.; Garino, Terry J.; Croes, Kenneth James

This study encompasses initial scoping tests on the incorporation of a novel iodine loaded getter material into the Sandia developed low temperature sintering glass ceramic material (GCM) waste form. In particular, we studied the PNNL Ag-I-Aerogel. Optical microscopy indicates inhomogenous samples based on particle sizes and variations in color (AgI vs Ag/AgO on silica). TGA/MS data when heated in air indicates loss of iodine and organics (CO2) between 250-450°C a total of ~15wt% loss, with additional / small iodine loss when during 550°C hold for 1 hr. TGA/MS data when heated in N2 indicates less organic and slightly less iodinemore » loss below 550°C, with no loss of iodine in 550°C 1 hour hold. Furthermore, a substantial mass loss of sulfur containing compounds is observed (m/e of 34 and 36) between 150 – 550°C in both air and N2 sintering atmospheres. In an effort to capture iodine lost to volatilization during heating (at temps below glass sintering temperature of 550°C), we added 5 wt% Ag flake to the AgIaerogel. Resulting data indicates the iodine is retained with the addition of the Ag flake, resulting in only a small iodine loss (< 1wt%) at ~350°C. No method of curtailing loss of sulfur containing compounds due to heating was successful in this scoping study.« less

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

NASA Astrophysics Data System (ADS)

Rahman, Md Taibur; McCloy, John; Ramana, C. V.; Panat, Rahul

2016-08-01

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24-500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasing trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.

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.

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

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

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

PubMed

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

2017-11-25

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

Effect of sintering temperature on the electrolysis of TiO2

NASA Astrophysics Data System (ADS)

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

2012-07-01

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

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.

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

PubMed Central

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

2010-01-01

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

Studying hardness, workability and minimum bending radius in selectively laser-sintered Ti–6Al–4V alloy samples

NASA Astrophysics Data System (ADS)

Galkina, N. V.; Nosova, Y. A.; Balyakin, A. V.

2018-03-01

This research is relevant as it tries to improve the mechanical and service performance of the Ti–6Al–4V titanium alloy obtained by selective laser sintering. For that purpose, sintered samples were annealed at 750 and 850°C for an hour. Sintered and annealed samples were tested for hardness, workability and microstructure. It was found that incomplete annealing of selectively laser-sintered Ti–6Al–4V samples results in an insignificant reduction in hardness and ductility. Sintered and incompletely annealed samples had a hardness of 32..33 HRC, which is lower than the value of annealed parts specified in standards. Complete annealing at temperature 850°C reduces the hardness to 25 HRC and ductility by 15...20%. Incomplete annealing lowers the ductility factor from 0.08 to 0.06. Complete annealing lowers that value to 0.025. Complete annealing probably results in the embrittlement of sintered samples, perhaps due to their oxidation and hydrogenation in the air. Optical metallography showed lateral fractures in both sintered and annealed samples, which might be the reason why they had lower hardness and ductility.

Behavior of Oxide Film at Interface between Particles of Al-Mg Alloy Powder Compacts Prepared by Pulse Electric Current Sintering

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Yamaguchi, Norio; Song, Minghui; Mitsuishi, Kazutaka; Furuya, Kazuo; Noda, Tetsuji

2003-07-01

Al-1.0 mass% Mg alloy powders were sintered using the pulse electric current sintering (PECS) process at various temperatures. The microstructure at the interfaces between powder particles and the effect of sintering temperature on interface characteristics were investigated using transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS). The precipitates were observed at the interfaces between powder particles of the compacts. The amounts of the precipitates increased and the compositions changed with an increase in sintering temperature: MgO for the compact sintered at 613 K, MgAl2O4+MgO for those at 663 K and 713 K, and MgAl2O4 for those above 763 K. Comparing the results obtained by the PECS process with those of diffusion bonding experiments and thermodynamic calculation, it was suggested that the temperature at the interfaces between the particles was higher than that of the particles sintered by the PECS process.

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

PubMed

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

2012-08-01

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

Sintered Intermetallic Reinforced 434L Ferritic Stainless Steel Composites

NASA Astrophysics Data System (ADS)

Upadhyaya, A.; Balaji, S.

2009-03-01

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

[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.

Extension of the master sintering curve for constant heating rate modeling

NASA Astrophysics Data System (ADS)

McCoy, Tammy Michelle

The purpose of this work is to extend the functionality of the Master Sintering Curve (MSC) such that it can be used as a practical tool for predicting sintering schemes that combine both a constant heating rate and an isothermal hold. Rather than just being able to predict a final density for the object of interest, the extension to the MSC will actually be able to model a sintering run from start to finish. Because the Johnson model does not incorporate this capability, the work presented is an extension of what has already been shown in literature to be a valuable resource in many sintering situations. A predicted sintering curve that incorporates a combination of constant heating rate and an isothermal hold is more indicative of what is found in real-life sintering operations. This research offers the possibility of predicting the sintering schedule for a material, thereby having advanced information about the extent of sintering, the time schedule for sintering, and the sintering temperature with a high degree of accuracy and repeatability. The research conducted in this thesis focuses on the development of a working model for predicting the sintering schedules of several stabilized zirconia powders having the compositions YSZ (HSY8), 10Sc1CeSZ, 10Sc1YSZ, and 11ScSZ1A. The compositions of the four powders are first verified using x-ray diffraction (XRD) and the particle size and surface area are verified using a particle size analyzer and BET analysis, respectively. The sintering studies were conducted on powder compacts using a double pushrod dilatometer. Density measurements are obtained both geometrically and using the Archimedes method. Each of the four powders is pressed into ¼" diameter pellets using a manual press with no additives, such as a binder or lubricant. Using a double push-rod dilatometer, shrinkage data for the pellets is obtained over several different heating rates. The shrinkage data is then converted to reflect the change in relative density of the pellets based on the green density and the theoretical density of each of the compositions. The Master Sintering Curve (MSC) model is then utilized to generate data that can be utilized to predict the final density of the respective powder over a range of heating rates. The Elton Master Sintering Curve Extension (EMSCE) is developed to extend the functionality of the MSC tool. The parameters generated from the original MSC are used in tandem with the solution to the closed integral, theta ≡ 1cTo T1Texp -QRT dT, over a set range of temperatures. The EMSCE is used to generate a set of sintering curves having both constant heating rate and isothermal hold portions. The EMSCE extends the usefulness of the MSC by allowing this generation of a complete sintering schedule rather than just being able to predict the final relative density of a given material. The EMSCE is verified by generating a set of curves having both constant heating rate and an isothermal hold for the heat-treatment. The modeled curves are verified experimentally and a comparison of the model and experimental results are given for a selected composition. Porosity within the final product can hinder the product from sintering to full density. It is shown that some of the compositions studied did not sinter to full density because of the presence of large porosity that could not be eliminated in a reasonable amount of time. A statistical analysis of the volume fraction of porosity is completed to show the significance of the presence in the final product. The reason this is relevant to the MSC is that the model does not take into account the presence of porosity and assumes that the samples sinter to full density. When this does not happen, the model actually under-predicts the final density of the material.

Densification of LSGM electrolytes using activated microwave sintering

NASA Astrophysics Data System (ADS)

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

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

Hybrid processing and anisotropic sintering shrinkage in textured ZnO ceramics

PubMed Central

Keskinbora, Kahraman; Suzuki, Tohru S; Ozgur Ozer, I; Sakka, Yoshio; Suvaci, Ender

2010-01-01

We have studied the combined effects of the templated grain growth and magnetic alignment processes on sintering, anisotropic sintering shrinkage, microstructure development and texture in ZnO ceramics. Suspensions of 0–10 vol % ZnO template particles were slip cast in a 12 T rotating magnetic field. Sintering and texture characteristics were investigated via thermomechanical analysis and electron backscatter diffraction, respectively. Sintering as well as texture characteristics depend on template concentration. For the studied ZnO system, there is a critical template concentration (2 vol % in this study) above which densification is limited by the templates owing to constrained sintering. Below this limit, the densification is enhanced and the anisotropic shrinkage is reduced, which is attributed to densifying characteristics of the templates. PMID:27877373

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.

Back-side hydrogenation technique for defect passivation in silicon solar cells

DOEpatents

Sopori, Bhushan L.

1994-01-01

A two-step back-side hydrogenation process includes the steps of first bombarding the back side of the silicon substrate with hydrogen ions with intensities and for a time sufficient to implant enough hydrogen atoms into the silicon substrate to potentially passivate substantially all of the defects and impurities in the silicon substrate, and then illuminating the silicon substrate with electromagnetic radiation to activate the implanted hydrogen, so that it can passivate the defects and impurities in the substrate. The illumination step also annihilates the hydrogen-induced defects. The illumination step is carried out according to a two-stage illumination schedule, the first or low-power stage of which subjects the substrate to electromagnetic radiation that has sufficient intensity to activate the implanted hydrogen, yet not drive the hydrogen from the substrate. The second or high-power illumination stage subjects the substrate to higher intensity electromagnetic radiation, which is sufficient to annihilate the hydrogen-induced defects and sinter/alloy the metal contacts.

Back-side hydrogenation technique for defect passivation in silicon solar cells

DOEpatents

Sopori, B.L.

1994-04-19

A two-step back-side hydrogenation process includes the steps of first bombarding the back side of the silicon substrate with hydrogen ions with intensities and for a time sufficient to implant enough hydrogen atoms into the silicon substrate to potentially passivate substantially all of the defects and impurities in the silicon substrate, and then illuminating the silicon substrate with electromagnetic radiation to activate the implanted hydrogen, so that it can passivate the defects and impurities in the substrate. The illumination step also annihilates the hydrogen-induced defects. The illumination step is carried out according to a two-stage illumination schedule, the first or low-power stage of which subjects the substrate to electromagnetic radiation that has sufficient intensity to activate the implanted hydrogen, yet not drive the hydrogen from the substrate. The second or high-power illumination stage subjects the substrate to higher intensity electromagnetic radiation, which is sufficient to annihilate the hydrogen-induced defects and sinter/alloy the metal contacts. 3 figures.

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

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

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

2011-12-12

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

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.

[Effect of sintering gold paste coating on the bonding strength of pure titanium and three low-fusing porcelains].

PubMed

Zhang, Ya-li; Luo, Xiao-ping; Zhou, Li

2012-05-01

To study the effect of sintering gold paste coating of pure titanium on the adhesion of three porcelains following the protocol ISO 9693, and to investigate the titanium-porcelains interfaces. Sixty machined pure titanium samples were prepared in a rectangular shape according to ISO 9693 and divided equally into six groups. Half of the strips were coated with gold paste (Deckgold) and sintered. Three ultra-low-fusing dental porcelains (I: Initial Ti, S: Super porcelain Ti-22, T: TitanKeramik) were fused onto the titanium surfaces. A thin layer of bonding agent was only applied on the surfaces of uncoated gold specimens. The interface of the porcelain and titanium was observed with a field emission scanning electron microscope (FE-SEM) after metallographic preparation and sputtered with a very thin carbon layer of the embedded titanium-porcelain interface. After three-point bending test was performed, optical stereomicroscope was used to characterize the titanium-porcelains adhesion and determine the mode of failure. FE-SEM illustrated intermetallic compounds of Au-Ti formed with some visible microcracks in the gold layer and the interface of gold layer and ceramic. All the uncoated gold titanium-porcelain system showed predominately adhesive fracture at the titanium oxidation, whereas the failure modes in all gold coated systems were cohesive and adhesive, mainly cohesive. The three-point-bending test showed that the bonding strength of GS and GI groups [(37.08 ± 4.32) and (36.20 ± 2.40) MPa] were higher than those in uncoated groups [(31.56 ± 3.74) and (30.88 ± 2.60) MPa, P < 0.05], while no significant difference was found between T group and GT group (P > 0.05). The gold paste intermediate coatings can improve bond strengths of Super porcelain Ti-22 system and Initial Ti system, which have potential applications in clinical fields.

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.

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.

[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.
.

Rapid vacuum sintering: A novel technique for fabricating fluorapatite ceramic scaffolds for bone tissue engineering.

PubMed

Denry, Isabelle; Goudouri, Ourania-Menti; Harless, Jeffrey; Holloway, Julie A

2018-01-01

Macroporous bioceramic scaffolds are often fabricated via the foam replica technique, based on polymeric foam impregnation with a glass slurry, followed by slow heat treatment to allow for drying, polymeric burnout, and sintering of the glass particles. As a consequence, the process is time consuming and complicated by concurrent crystallization of the glass, often leading to incomplete sintering. Our goal was to investigate the effect of heating rate on sintering behavior, architecture, and mechanical properties of fluorapatite-based glass and glass-ceramic scaffolds. Glass scaffolds were prepared and sintered by rapid vacuum sintering (RVS) at 785°C under vacuum at a fast heating rate (55°C/min.) or without vacuum at a slow heating rate (2°C/min.). Two additional groups were further crystallized at 775°C/1 h. XRD confirmed the presence of fluorapatite for crystallized scaffolds. All groups presented interconnected porosity with a pore size in the 500 μm range. Scaffolds produced by RVS exhibited an excellent degree of sintering while scaffolds produced by slow sintering were incompletely sintered. The mean compressive strength was significantly higher for the RVS groups (1.52 ± 0.55 and 1.72 ± 0.61 MPa) compared to the slow-sintered groups (0.54 ± 0.30 and 0.45 ± 0.26 MPa). Meanwhile, the total production time was reduced by more than 12 h by using the RVS technique. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 106B: 291-299, 2018. © 2017 Wiley Periodicals, Inc.

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.

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.

Mechanical Properties and Plasma Erosion Resistance of ZrO2p(3Y)/BN-SiO2 Ceramic Composites under Different Sintering Temperature

NASA Astrophysics Data System (ADS)

Zhou, Yu; Duan1, Xiaoming; Jia, Dechang; Yang, Zhihua; Meng, Qingchang; Yu, Yang; Yu, Daren; Ding, Yongjie

2011-10-01

ZrO2p(3Y)/BN-SiO2 ceramic composites were hot pressed under different sintering temperature. The ceramic composites were composed by BN, m-ZrO2, t-ZrO2 and SiO2. The relative density, bending strength, elastic modulus and fracture toughness increase with the sintering temperature increasing, the maximum value of which at the sintering temperature of 1800°C are 97.5%, 229.9MPa, 60.8GPa and 3.55MPam1/2, respectively. The erosion resistance ability of ZrO2p(3Y)/BN-SiO2 ceramic composites rise gradually with the sintering temperature increasing, and the erosion rate of the ceramic composite sintered at 1800°C is 8.03×10-3mm/h.

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

NASA Astrophysics Data System (ADS)

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

2016-11-01

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

Reactive Spark Plasma Sintering (SPS) of Nitride Reinforced Titanium Alloy Composites (Postprint)

DTIC Science & Technology

2014-08-15

AFRL-RX-WP-JA-2014-0177 REACTIVE SPARK PLASMA SINTERING (SPS) OF NITRIDE REINFORCED TITANIUM ALLOY COMPOSITES (POSTPRINT) Jaimie S...titanium–vanadium alloys, has been achieved by introducing reactive nitrogen gas during the spark plasma sintering (SPS) of blended titanium and...lcomReactive spark plasma sintering (SPS) of nitride reinforced titanium alloy compositeshttp://dx.doi.org/10.1016/j.jallcom.2014.08.049 0925-8388

The thermal stability of hydroxyapatite in biphasic calcium phosphate ceramics.

PubMed

Nilen, R W N; Richter, P W

2008-04-01

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

Electrochemical corrosion and bioactivity of Ti-Nb-Sn-hydroxyapatite composites fabricated by pulse current activated sintering.

PubMed

Xiaopeng, Wang; Fantao, Kong; Biqing, Han; Yuyong, Chen

2017-11-01

Ti-Nb-Sn-hydroxyapatite (HA) composites were prepared by mechanical alloying for different times (unmilled, 4, 8 and 12h), followed by pulse current activated sintering. The effects of the milling time on the electrochemical corrosion resistance and bioactivity of the sintered Ti-35Nb-2.5Sn-15HA composites were investigated. Potentiodynamic polarization test results indicated that the sintered Ti-35Nb-2.5Sn-15HA composites exhibited higher corrosion resistance with increasing milling time. The corrosion potential and current of the Ti-35Nb-2.5Sn-15HA composite sintered by 12h milled powders were - 0.261V and 0.18μA/cm 2 , respectively, and this sintered composite showed a stable and wide passivation region. The hemolysis rate of the sintered Ti-35Nb-2.5Sn-15HA composites reduced with increasing milling time and the lowest hemolytic rate of the composites was 0.87%. In addition, the in vitro cell culture results indicated that the composite sintered by 12h milled powders had good biocompatibility. These results indicate the significant potential of Ti-35Nb-2.5Sn/xHA composites for biomedical implant applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

The interaction of small particles and thin films of metals with gases. I - A brief review of the early stages of oxide formation

NASA Technical Reports Server (NTRS)

Poppa, H.

1976-01-01

Existing work on gas-solid reactions making use of thin film technologies is reviewed. The discussion concentrates on two major areas of gas-metal interactions: chemisorption and the early stages of oxidation of metals (characterized by a non-volatile reaction product) and catalytic surface reactions (featuring volatile reaction products). A brief survey of oxide formation on metals is presented. Here it is of importance to distinguish between reactions on continuous thin film substrates and reactions on particulate deposits. Small particle-gas interactions also affect the nucleation, growth and sintering processes of thin films. It is shown that various combinations of UHV and high resolution electron microscopy techniques, which include in situ experimentation, can provide the appropriate tools for studying angstrom particle chemistry.

Effect of milling and leaching on the structure of sintered silicon

NASA Technical Reports Server (NTRS)

Yeh, H. C.; Glasgow, T. K.; Herbell, T. P.

1980-01-01

The effects of attrition milling and acid leaching on the sintering behavior and the resultant structures of two commercial silicon powders were investigated. Sintering was performed in He for 16 hours at 1200, 1250, and 1300 C. Compacts of as-received Si did not densify during sintering. Milling reduced the average particle size to below 0.5 microns and enhanced densification (1.75 g/cc). Leaching milled Si further enhanced densification (1.90 g/cc max.) and decreased structural coarsening. After sintering, the structure of the milled and leached powder compacts appears favorable for the production of reaction bonded silicon nitride.

Rapid laser sintering of metal nano-particles inks.

PubMed

Ermak, Oleg; Zenou, Michael; Toker, Gil Bernstein; Ankri, Jonathan; Shacham-Diamand, Yosi; Kotler, Zvi

2016-09-23

Fast sintering is of importance in additive metallization processes and especially on sensitive substrates. This work explores the mechanisms which set limits to the laser sintering rate of metal nano-particle inks. A comparison of sintering behavior of three different ink compositions with laser exposure times from micro-seconds to seconds reveals the dominant factor to be the organic content (OC) in the ink. With a low OC silver ink, of 2% only, sintering time falls below 100 μs with resistivity <×4 bulk silver. Still shorter exposure times result in line delamination and deformation with a similar outcome when the OC is increased.

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

NASA Astrophysics Data System (ADS)

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

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

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

NASA Technical Reports Server (NTRS)

Dutta, S.

1977-01-01

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

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.

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.

Defects level evaluation of LiTiZn ferrite ceramics using temperature dependence of initial permeability

NASA Astrophysics Data System (ADS)

Malyshev, A. V.; Petrova, A. B.; Sokolovskiy, A. N.; Surzhikov, A. P.

2018-06-01

The method for evaluating the integral defects level and chemical homogeneity of ferrite ceramics based on temperature dependence analysis of initial permeability is suggested. A phenomenological expression for the description of such dependence was suggested and an interpretation of its main parameters was given. It was shown, that the main criterion of the integral defects level of ferrite ceramics is relation of two parameters correlating with elastic stress value in a material. An indicator of structural perfection can be a maximum value of initial permeability close to Curie point as well. The temperature dependences of initial permeability have analyzed for samples sintered in laboratory conditions and for the ferrite industrial product. The proposed method allows controlling integral defects level of the soft ferrite products and has high sensitivity compare to typical X-ray methods.

KOH concentration effect on the cycle life of nickel-hydrogen cells

NASA Technical Reports Server (NTRS)

Lim, H. S.; Verzwyvelt, S. A.

1985-01-01

Effects of KOH concentration on the cycle life of a sintered-type nickel electrode were studied in a boiler plate nickel-hydrogen cell at 23 C using an accelerated 45-min cycle regime at 80 percent depth of discharge. The cycle life improved greatly as the KOH concentration decreased, although the initial capacity of the cell decreased slightly. The cycle life improved by a factor of two or more when the KOH concentration was reduced from 36 to 31 percent and by a similar factor from reductions of 31 to 26 percent. For many applications, this life improvement may outweigh the initial capacity decrease.

Preparation and Mechanical Behavior of Glass-Ceramics from Feldspathic Frits

NASA Astrophysics Data System (ADS)

da Silva, Fernanda A. N. G.; Barbato, Carla N.; França, Silvia C. A.; Silva, Ana Lúcia N.; de Andrade, Mônica C.

2017-10-01

Glass-ceramics were produced from frits with feldspar (79.09% wt/wt), alumina, sodium carbonate, potassium carbonate, borax and cerium dioxide. Feldspathic frits obtained at 1200 °C were shaped and sintered at various temperatures. Flexural strength results were analyzed by using the Weibull statistical distribution. These materials were also characterized by x-ray diffraction and scanning electron microscopy (SEM). At 600 °C, an initial leucite formation occurred as a crystalline phase, but the amorphous phase still prevailed, with low flexural strength. On the other hand, when the temperature increased to 800 °C, flexural strength also increased to approximately 70 MPa and Weibull modulus, m = 4.4 . This behavior was explained by the formation of leucite crystals dispersed within the glassy matrix, which hinders, in a certain concentration, the propagation of cracks. However, for the sintering temperature of 1000 °C, flexural strength decreased and may be associated with higher levels of this leucite crystal, in spite of the higher reliability m = 6.6.

Tracking the shape-dependent sintering of platinum-rhodium model catalysts under operando conditions

NASA Astrophysics Data System (ADS)

Hejral, Uta; Müller, Patrick; Balmes, Olivier; Pontoni, Diego; Stierle, Andreas

2016-03-01

Nanoparticle sintering during catalytic reactions is a major cause for catalyst deactivation. Understanding its atomic-scale processes and finding strategies to reduce it is of paramount scientific and economic interest. Here, we report on the composition-dependent three-dimensional restructuring of epitaxial platinum-rhodium alloy nanoparticles on alumina during carbon monoxide oxidation at 550 K and near-atmospheric pressures employing in situ high-energy grazing incidence x-ray diffraction, online mass spectrometry and a combinatorial sample design. For platinum-rich particles our results disclose a dramatic reaction-induced height increase, accompanied by a corresponding reduction of the total particle surface coverage. We find this restructuring to be progressively reduced for particles with increasing rhodium composition. We explain our observations by a carbon monoxide oxidation promoted non-classical Ostwald ripening process during which smaller particles are destabilized by the heat of reaction. Its driving force lies in the initial particle shape which features for platinum-rich particles a kinetically stabilized, low aspect ratio.

Stress Intensity of Delamination in a Sintered-Silver Interconnection: Preprint

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

DeVoto, D. J.; Paret, P. P.; Wereszczak, A. A.

2014-08-01

In automotive power electronics packages, conventional thermal interface materials such as greases, gels, and phase-change materials pose bottlenecks to heat removal and are also associated with reliability concerns. The industry trend is toward high thermal performance bonded interfaces for large-area attachments. However, because of coefficient of thermal expansion mismatches between materials/layers and resultant thermomechanical stresses, adhesive and cohesive fractures could occur, posing a reliability problem. These defects manifest themselves in increased thermal resistance. This research aims to investigate and improve the thermal performance and reliability of sintered-silver for power electronics packaging applications. This has been experimentally accomplished by the synthesismore » of large-area bonded interfaces between metalized substrates and copper base plates that have subsequently been subjected to thermal cycles. A finite element model of crack initiation and propagation in these bonded interfaces will allow for the interpretation of degradation rates by a crack-velocity (V)-stress intensity factor (K) analysis. A description of the experiment and the modeling approach are discussed.« less

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

NASA Astrophysics Data System (ADS)

Shikhar

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

Dielectric Properties of Sol-Gel Derived Barium Strontium Titanate and Microwave Sintering of Ceramics

NASA Astrophysics Data System (ADS)

Selmi, Fathi A.

This thesis consists of two areas of research: (1) sol-gel processing of Ba_{rm 1-x}Sr_{rm x} TiO_3 ceramics and their dielectric properties measurement; and (2) microwave versus conventional sintering of ceramics such as Al_2 O_3, Ba_{ rm 1-x}Sr_{rm x}TiO_3, Sb-doped SnO _2 and YBa_2Cu _3O_7. Sol-gel powders of BaTiO_3, SrTiO_3, and their solid solutions were synthesized by the hydrolysis of titanium isopropoxide and Ba and Sr methoxyethoxides. The loss tangent and dielectric constant of both sol-gel and conventionally prepared and sintered Ba_{rm 1-x}Sr _{rm x}TiO _3 ceramics were investigated at high frequencies. The sol-gel prepared ceramics showed higher dielectric constant and lower loss compared to those prepared conventionally. Ba _{rm 1-x}Sr _{rm x}TiO_3 ceramics were tunable with applied bias, indicating the potential use of this material for phase shifter applications. Porous Ba_{0.65}Sr _{0.35}TiO_3 was also investigated to lower the dielectric constant. Microwave sintering of alpha -Al_2O_3 and SrTiO_3 was investigated using an ordinary kitchen microwave oven (2.45 GHz; 600 Watts). The use of microwaves with good insulation of alpha -Al_2O_3 and SrTiO_3 samples resulted in their rapid sintering with good final densities of 96 and 98% of the theoretical density, respectively. A comparison of grain size for conventionally and microwave sintered SrTiO_3 samples did not show a noticeable difference. However, the grain size of microwave sintered alpha-Al_2O _3 was found to be larger than that of conventionally sintered sample. These results show that rapid sintering of ceramics can be achieved by using microwave radiation. The sintering behavior of coprecipitated Sb-doped SnO_2 was investigated using microwave power absorption. With microwave power, samples were sintered at 1450^circC for 20 minutes and showed a density as high as 99.9% of theoretical. However, samples fired in a conventional electric furnace at the same temperature for 4 hours showed only 60% of theoretical density. Microwave sintering also led to improvement in terms of uniform structure and electrical properties. Ba_{0.65}Sr _{0.35}TiO_3 was sintered using the microwave power at 1300 ^circC for 10 minutes. A density of 99% was achieved with small and uniform grain size. Superconducting powders have been successfully prepared by the sol-gel process and sintered and annealed using microwave power. Sintering and densification was achieved in a shorter time with microwave heating than with conventional heating and microwave heating appears to result in refined microstructure.

Sintering and microstructure property relationships of porous hydroxyapatite

NASA Astrophysics Data System (ADS)

Zakaria, Fadzil Ayad

2000-09-01

The use of ceramics inside the body, as implant materials, is a relatively new technology, the first instance having been reported just 20 years ago. The ceramics used for the repair and reconstruction of diseased, damaged or 'worn out' parts of the body are referred to as bioceramics, and such a material is hydroxyapatite. The use of calcium phosphate to repair bone defects has been based on the rationale that calcium phosphate resembles vertebrate tooth and bone mineral, and is biologically compatible with these and surrounding tissues. The concept of preparing porous hydroxyapatite was developed to prevent loosening of implants by enhancing the ingrowth of tissue into the pores (biological fixation). A structural limitation of this type of implant is the requirement to have a minimal pore size between 80- 100 m in diameter to allow bone to grow into the pores. The presence of such porosity would lead to a lower strength of the bioceramic component, but this is offset by the advantages of biocompatibility. It is well known that hydroxyapatite is a brittle material and making it porous would reduce the existing mechanical properties. This study was carried out to optimise the mechanical properties by investigating the processing conditions and methods of preparation. The effect of forming method, pore geometry, pore size, sintering cycle, sintering atmosphere and types of spherical polymers on the microstructure and mechanical properties were studied. As a consequence of the experiments, it was observed that porous hydroxyapatite is formed using an isostatic pressing technique, with 53 vol. % of HMWPVC as the porosifier. Sintering in air, with a heating rate of 50C/h, held for 1h at 600C in the first stage, and a heating rate of 100C/h, held for 4h at between 1200 and 1250C, generated a spherical pore geometry which gave the best combination of properties. This fabrication route resulted in an interconnected porous hydroxyapatite with a pore size ~90 m, the volume fraction of porosity ~35%, relative density of ~60%, a grain size ~1.7-2 m, a compressive strength between 14-18 MPa and a tensile strength of 4-5 MPa.

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

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

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

2016-04-21

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

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.

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

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

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

2015-10-27

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

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.

Reduction behavior and kinetics of vanadium-titanium sinters under high potential oxygen enriched pulverized coal injection

NASA Astrophysics Data System (ADS)

Ma, Jin-fang; Wang, Guang-wei; Zhang, Jian-liang; Li, Xin-yu; Liu, Zheng-jian; Jiao, Ke-xin; Guo, Jian

2017-05-01

In this work, the reduction behavior of vanadium-titanium sinters was studied under five different sets of conditions of pulverized coal injection with oxygen enrichment. The modified random pore model was established to analyze the reduction kinetics. The results show that the reduction rate of sinters was accelerated by an increase of CO and H2 contents. Meanwhile, with the increase in CO and H2 contents, the increasing range of the medium reduction index (MRE) of sinters decreased. The increasing oxygen enrichment ratio played a diminishing role in improving the reduction behavior of the sinters. The reducing process kinetic parameters were solved using the modified random role model. The results indicated that, with increasing oxygen enrichment, the contents of CO and H2 in the reducing gas increased. The reduction activation energy of the sinters decreased to between 20.4 and 23.2 kJ/mol.

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

Effect of sandblasting on surface roughness of zirconia-based ceramics and shear bond strength of veneering porcelain.

PubMed

He, Min; Zhang, Zutai; Zheng, Dongxiang; Ding, Ning; Liu, Yan

2014-01-01

This study aims to investigate the effect of sandblasting on the surface roughness of zirconia and the shear bond strength of the veneering porcelain. Pre-sintered zirconia plates were prepared and divided into four groups. Group A were not treated at all; group B were first sandblasted under 0.2 MPa pressure and then densely sintered; group C and D were sintered first, and then sandblasted under 0.2 MPa and 0.4 MPa pressures respectively. Surface roughness was measured and 3D roughness was reconstructed for the specimens, which were also analyzed with X-ray diffractometry. Finally after veneering porcelain sintering, shear bond tests were conducted. Sandblasting zirconia before sintering significantly increased surface roughness and the shear bond strength between zirconia and veneering porcelain (p<0.05). Sandblasting zirconia before sintering is a useful method to increase surface roughness and could successfully improve the bonding strength of veneering porcelain.

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.

Sintering Behavior of Hypereutectic Aluminum-Silicon Metal Matrix Composites Powder

NASA Astrophysics Data System (ADS)

Rudianto, Haris; Sun, Yang Sang; Jin, Kim Yong; Woo, Nam Ki

Lightweight materials of Aluminum-Silicon P/M alloys offer the advantage of high-wear resistance, high strength, good temperature resistance, and a low coefficient of thermal expansion. An A359 MMC alloy was mixed together with Alumix 231 in this research. Powders were compacted with compaction pressure up to 700 MPa. Particle size and compaction pressure influenced green density. Compacted powders were sintered in a tube furnace under a flowing nitrogen gas. Sintering temperature, heating rate and sintering time were verified to determine best sintering conditions of the alloys. Chemical composition also contributed to gain higher sintered density. Precipitation strengthening method was used to improve mechanical properties of this materials.T6 heat treatment was carried out to produce fine precipitates to impede movement of dislocation. The chemical composition of this materials allow for the potential formation of several strengthening precipitates including θ (Al2Cu) and β (Mg2Si).

Sintering behavior of Lanthana-bearing nanostructured ferritic steel consolidated via spark plasma sintering

DOE PAGES

Pasebani, Somayeh; Charit, Indrajit; Butt, Darryl P.; ...

2015-08-03

Elemental powder mixture of Fe–14Cr–1Ti–0.3Mo–0.5La 2O 3 (wt%) composition is mechanically alloyed for different milling durations (5, 10 and 20 h) and subsequently consolidated via spark plasma sintering under vacuum at 950 °C for 7 min. The effects of milling time on the densification behavior and density/microhardness are studied. The sintering activation energy is found to be close to that of grain boundary diffusion. The bimodal grain structure created in the milled and sintered material is found to be a result of milling and not of sintering alone. The oxide particle diameter varies between 2 and 70 nm. As amore » result, faceted precipitates smaller than 10 nm in diameter are found to be mostly La–Ti–Cr-enriched complex oxides that restrict further recrystallization and related phenomena.« less

Atmospheric Pressure Plasma Jet as a Dry Alternative to Inkjet Printing in Flexible Electronics

NASA Technical Reports Server (NTRS)

Gandhiraman, Ram Prasad; Lopez, Arlene; Koehne, Jessica; Meyyappan, M.

2016-01-01

We have developed an atmospheric pressure plasma jet printing system that works at room temperature to 50 deg C unlike conventional aerosol assisted techniques which require a high temperature sintering step to obtain desired thin films. Multiple jets can be configured to increase throughput or to deposit multiple materials, and the jet(s) can be moved across large areas using a x-y stage. The plasma jet has been used to deposit carbon nanotubes, graphene, silver nanowires, copper nanoparticles and other materials on substrates such as paper, cotton, plastic and thin metal foils.

Measurement of O and Ti atom displacements in TiO 2 during flash sintering experiments

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

Yoon, Bola; Yadav, Devinder; Raj, Rishi

In-situ flash experiments on rutile TiO 2 were performed at the synchrotron at the Brookhaven National Laboratory. Pair distribution function analysis of total X-ray scattering measurements yielded mean-square atomic displacements of oxygen and titanium atoms during the progression of the 3 stages of flash. The displacements are measured to be far greater for oxygen atoms than for titanium atoms. Thus, these large displacements may signal an “elastic softening” of the lattice, which, recently, has been predicted as a precursor to the onset of flash.

Custom-made prefabricated titanium miniplates in Le Fort I osteotomies: principles, procedure and clinical insights.

PubMed

Philippe, B

2013-08-01

This paper describes a new type of miniplate system that is designed and custom made during virtual surgery planning based on an individual patient's osteotomy. These miniplates are prefabricated with commercially pure porous titanium using direct metal laser sintering. The principles that guide the conception and production of this new miniplate are presented. The surgical procedure from the stage of virtual surgery planning until the final Le Fort I osteotomy and bone fixation are described using a case example. Copyright © 2013 International Association of Oral and Maxillofacial Surgeons. Published by Elsevier Ltd. All rights reserved.

Measurement of O and Ti atom displacements in TiO 2 during flash sintering experiments

DOE PAGES

Yoon, Bola; Yadav, Devinder; Raj, Rishi; ...

2017-12-29

In-situ flash experiments on rutile TiO 2 were performed at the synchrotron at the Brookhaven National Laboratory. Pair distribution function analysis of total X-ray scattering measurements yielded mean-square atomic displacements of oxygen and titanium atoms during the progression of the 3 stages of flash. The displacements are measured to be far greater for oxygen atoms than for titanium atoms. Thus, these large displacements may signal an “elastic softening” of the lattice, which, recently, has been predicted as a precursor to the onset of flash.

Efficient sintering of nanocrystalline titanium dioxide films for dye solar cells via raster scanning laser

NASA Astrophysics Data System (ADS)

Mincuzzi, Girolamo; Vesce, Luigi; Reale, Andrea; Di Carlo, Aldo; Brown, Thomas M.

2009-09-01

By identifying the right combination of laser parameters, in particular the integrated laser fluence Φ, we fabricated dye solar cells (DSCs) with UV laser-sintered TiO2 films exhibiting a power conversion efficiency η =5.2%, the highest reported for laser-sintered devices. η is dramatically affected by Φ and a clear trend is reported. Significantly, DSCs fabricated by raster scanning the laser beam to sinter the TiO2 films are made as efficient as those with oven-sintered ones. These results, confirmed on three batches of cells, demonstrate the remarkable potential (noncontact, local, low cost, rapid, selective, and scalable) of scanning laser processing applied to DSC technology.

Thermal barrier coating resistant to sintering

DOEpatents

Subramanian, Ramesh; Seth, Brig B.

2005-08-23

A device (10) is made, having a ceramic thermal barrier coating layer (16) characterized by a microstructure having gaps (18) with a sintering inhibiting material (22) disposed on the columns (20) within the gaps (18). The sintering resistant material (22) is stable over the range of operating temperatures of the device (10), is not soluble with the underlying ceramic layer (16) and is applied by a process that is not an electron beam physical vapor deposition process. The sintering inhibiting material (22) has a morphology adapted to improve the functionality of the sintering inhibiting material (22), characterized as continuous, nodule, rivulet, grain, crack, flake and combinations thereof and being disposed within at least some of the vertical and horizontal gaps.

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.

Fabrication Processes and Mechanical Behavior of CNT/Metal Nanocomposites

DTIC Science & Technology

2013-12-01

process, were investigated and applied for fabrication of CNT/Cu and CNT/Ni nanocomposite powders. The spark plasma sintering process was applied... spark plasma sintering process to fabricate CNT/NiTi and CNT/Al-Cu nanocomposites. It is confirmed that the CNTs were homogeneously dispersed in NiTi...can be seen in Figure 1-1. The CNT/NiTi composite powders were consolidated by spark plasma sintering (SPS, Dr. Sinter Lab., Sumitomo). The CNT/NiTi

A strategy to optimize the thermoelectric performance in a spark plasma sintering process

PubMed Central

Chiu, Wan-Ting; Chen, Cheng-Lung; Chen, Yang-Yuan

2016-01-01

Spark plasma sintering (SPS) is currently widely applied to existing alloys as a means of further enhancing the alloys’ figure of merit. However, the determination of the optimal sintering condition is challenging in the SPS process. This report demonstrates a systematic way to independently optimize the Seebeck coefficient S and the ratio of electrical to thermal conductivity (σ/κ) and thus achieve the maximum figure of merit zT = S2(σ/κ)T. Sb2−xInxTe3 (x = 0–0.2) were chosen as examples to validate the method. Although high sintering temperature and pressure are helpful in enhancing the compactness and electrical conductivity of pressed samples, the resultant deteriorated Seebeck coefficient and increasing thermal conductivity eventually offset the benefit. We found that the optimal sintering temperature coincides with temperatures at which the maximum Seebeck coefficient begins to degrade, whereas the optimal sintering pressure coincided with the pressure at which the σ/κ ratio reaches a maximum. Based on this principle, the optimized sintering conditions were determined, and the zT of Sb1.9In0.1Te3 is raised to 0.92 at 600 K, showing an approximately 84% enhancement. This work develops a facile strategy for selecting the optimal SPS sintering condition to further enhance the zT of bulk specimens. PMID:26975209

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

Embrittling Components in Sintered Steels: Comparison of Phosphorus and Boron

NASA Astrophysics Data System (ADS)

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

2017-12-01

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

Al{sub 2}TiO{sub 5}-Al{sub 2}O{sub 3}-TiO{sub 2} nanocomposite: Structure, mechanical property and bioactivity studies

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

Kalita, Samar Jyoti, E-mail: Samar.Kalita@und.nodak.edu; Somani, Vikas

2010-12-15

Novel biomaterials are of prime importance in tissue engineering. Here, we developed novel nanostructured Al{sub 2}TiO{sub 5}-Al{sub 2}O{sub 3}-TiO{sub 2} composite as a biomaterial for bone repair. Initially, nanocrystalline Al{sub 2}O{sub 3}-TiO{sub 2} composite powder was synthesized by a sol-gel process. The powder was cold compacted and sintered at 1300-1500 {sup o}C to develop nanostructured Al{sub 2}TiO{sub 5}-Al{sub 2}O{sub 3}-TiO{sub 2} composite. Nano features were retained in the sintered structures while the grains showed irregular morphology. The grain-growth and microcracking were prominent at higher sintering temperatures. X-ray diffraction peak intensity of {beta}-Al{sub 2}TiO{sub 5} increased with increasing temperature. {beta}-Al{sub 2}TiO{submore » 5} content increased from 91.67% at 1300 {sup o}C to 98.83% at 1500 {sup o}C, according to Rietveld refinement. The density of {beta}-Al{sub 2}TiO{sub 5} sintered at 1300 {sup o}C, 1400 {sup o}C and 1500 {sup o}C were computed to be 3.668 g cm{sup -3}, 3.685 g cm{sup -3} and 3.664 g cm{sup -3}, respectively. Nanocrystalline grains enhanced the flexural strength. The highest flexural strength of 43.2 MPa was achieved. Bioactivity and biomechanical properties were assessed in simulated body fluid. Electron microscopy confirmed the formation of apatite crystals on the surface of the nanocomposite. Spectroscopic analysis established the presence of Ca and P ions in the crystals. Results throw light on biocompatibility and bioactivity of {beta}-Al{sub 2}TiO{sub 5} phase, which has not been reported previously.« less

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.

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

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

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

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

Silicon 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.

JPRS Report, Science & Technology, Japan

DTIC Science & Technology

1987-12-02

casting nathod —.ntnoshar ic sintering nethod _Reaotion sintering nethod .Btlf-iintering nethod „Recrystallizing sintering nathod -Hot Porning ...was completed by photo- graphically recalling even such things as how bolts were fastened to achieve a complete copy similar to a video replay of

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.

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.

High resolution laser micro sintering / melting using q-switched and high brilliant laser radiation

NASA Astrophysics Data System (ADS)

Exner, H.; Streek, A.

2015-03-01

Since the discovery of selective laser sintering/melting, numerous modifications have been made to upgrade or customize this technology for industrial purposes. Laser micro sintering (LMS) is one of those modifications: Powders with particles in the range of a few micrometers are used to obtain products with highly resolved structures. Pulses of a q-switched laser had been considered necessary in order to generate sinter layers from the micrometer scaled metal powders. LMS has been applied with powders from metals as well as from ceramic and cermet feedstock's to generate micro parts. Recent technological progress and the application of high brilliant continuous laser radiation have now allowed an efficient laser sintering/melting of micrometer scaled metal powders. Thereby it is remarkable that thin sinter layers are generated using high continuous laser power. The principles of the process, the state of the art in LMS concerning its advantages and limitations and furthermore the latest results of the recent development of this technology will be presented. Laser Micro Sintering / Laser Micro Melting (LMM) offer a vision for a new dimension of additive fabrication of miniature and precise parts also with application potential in all engineering fields.

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.

Selective autocatalytic reduction of NO from sintering flue gas by the hot sintered ore in the presence of NH3.

PubMed

Chen, Wangsheng; Luo, Jing; Qin, Linbo; Han, Jun

2015-12-01

In this paper, the selective autocatalytic reduction of NO by NH3 combined with multi-metal oxides in the hot sintered ore was studied, and the catalytic activity of the hot sintered ore was investigated as a function of temperature, NH3/NO ratio, O2 content, H2O and SO2. The experimental results indicated that the hot sintered ore, when combined with NH3, had a maximum denitration efficiency of 37.67% at 450 °C, 3000 h(-1) gas hourly space velocity (GHSV) and a NH3/NO ratio of 0.4/1. Additionally, it was found that O2 played an important role in removing NOx. However, high O2 content had a negative effect on NO reduction. H2O was found to promote the denitration efficiency in the absence of SO2, while SO2 inhibited the catalytic activity of the sintered ore. In the presence of H2O and SO2, the catalytic activity of the sintered ore was dramatically suppressed. Copyright © 2015 Elsevier Ltd. All rights reserved.

Fabrication and study of double sintered TiNi-based porous alloys

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

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

PubMed

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

2009-12-15

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

Microwave sintering of Ag-nanoparticle thin films on a polyimide substrate

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

Fujii, S., E-mail: fujii.s.ap@m.titech.ac.jp; Department of Information and Communication System Engineering, National Institute of Technology, Okinawa College, Nago, Okinawa 905-2192; Kawamura, S.

2015-12-15

Ag-nanoparticle thin films on a polyimide substrate were subjected to microwave sintering by use of a single-mode waveguide applicator. A two-step sintering process was employed. First, at low conductivities of the film, the film sample was placed at the site of the maximum electric field and subjected to microwave irradiation. Second, when the conductivity of the film increased, the film sample was placed at the site of the maximum magnetic field and again subjected to microwave irradiation. The microwave sintering process was completed within 1.5 min, which is significantly lower than the time required for the oven heating process. Themore » resulting conductivity of the film, albeit only 30% of that of the bulk material, was seven times that of a film annealed at the same temperature in a furnace. Scanning electron microscopy images revealed that the nanoparticles underwent both grain necking and grain growth during microwave sintering. In addition, this sintering process was equivalent to the oven heating process performed at a 50 °C higher annealing temperature. An electromagnetic wave simulation and a heat transfer simulation of the microwave sintering process were performed to gain a thorough understanding of the process.« less

Effect of surface chemistry on the rate of osseointegration of sintered porous-surfaced Ti-6Al-4V implants.

PubMed

Taché, Alex; Gan, Lu; Deporter, Douglas; Pilliar, Robert M

2004-01-01

The effect of adding a thin sol-gel-formed calcium phosphate (CaP) coating to sintered porous-surfaced titanium alloy (Ti-6Al-4V) implants on rates of initial bone ingrowth was investigated. Control implants (as manufactured) and similar implants with sol-gel CaP coatings were randomly placed in distal femoral rabbit condyles (1 implant/leg). After healing for 6, 9, 12, and 16 days, 8 of 10 rabbits in each time group were assessed for maximum implant pullout force (N) and interface stiffness (N/mm). Selected extracted implants also were examined by secondary electron imaging to characterize affected surfaces. The implants of the remaining 2 rabbits in each group were examined by backscattered scanning electron microscopy (BSEM). Significantly greater pullout forces and interface stiffness were found for CaP-coated implants at 6 and 9 days. At 6 days, BSEM revealed bone ingrowth on CaP-coated implants but not on control implants. Secondary electron imaging and BSEM observations also suggested greater bone ingrowth with CaP-coated porous implants at 9, 12, and 16 days. Sol-gel-formed CaP surface films significantly enhance rates of bone ingrowth into sintered porous-surfaced implants. This surface treatment may have a number of clinical benefits, including shortening the period prior to functional loading of such implants and improving treatment outcomes in situations of poor bone quality and/or quantity. (More than 50 references).

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

Natural Silica Sand/Alumina Ceramic Composites: Promising Candidates for Fuel-Cell Sealants

NASA Astrophysics Data System (ADS)

Hidayat, N.; Istiqomah; Widianto, M. Y. H.; Taufiq, A.; Sunaryono; Triwikantoro; Zainuri, M.; Baqiya, M. A.; Aristia, G.; Pratapa, S.

2017-05-01

An attempt has been developed to establish the prospect of the useful application of Indonesian natural silica sand, instead of commercially expensive materials, as a future fuel-cell sealant. The sand was initially washed and ball-milled at 150 rpm for 60 minutes and then heated at 1000 °C for the same duration. The resulting powder was then mixed with alumina powder at various amounts and shaped into discs before sintering at 1150 °C and 1250 °C to produce compact ceramics. The diameter shrinkage, porosity, and density of the ceramics were evaluated by Archimedes method. Their crystalline phase composition was quantified by Rietveld refinement analysis on the X-ray diffraction (XRD) data and the phase weight fraction was then used for coefficient of thermal expansion (CTE) evaluation. It was observed that the bulk density increased while the porosity decreased with alumina addition. The XRD data analysis revealed that the prepared silica sand contains a very high purity of quartz-SiO2, i.e. 97.8(18)%. The sintering temperatures of 1150 °C and 1250 °C transformed some quartz-SiO2 to crystobalite-SiO2. All the calcite-CaCO3 exhibited reaction sintering with SiO2 forming wollastonite-CaSiO3. Therefore, the ceramic composites contained SiO2/Al2O3/CaSiO3. Regarding CTE, all of the composites meet the criteria for fuel-cell sealants, in the range of 9-12 ppm/°C.

Y3Fe5O12 nanoparticulate garnet ferrites: Comprehensive study on the synthesis and characterization fabricated by various routes

NASA Astrophysics Data System (ADS)

Niaz Akhtar, Majid; Azhar Khan, Muhammad; Ahmad, Mukhtar; Murtaza, G.; Raza, Rizwan; Shaukat, S. F.; Asif, M. H.; Nasir, Nadeem; Abbas, Ghazanfar; Nazir, M. S.; Raza, M. R.

2014-11-01

The effects of synthesis methods such as sol-gel (SG), self combustion (SC) and modified conventional mixed oxide (MCMO) on the structure, morphology and magnetic properties of the (Y3Fe5O12) garnet ferrites have been studied in the present work. The samples of Y3Fe5O12 were sintered at 950 °C and 1150 °C (by SG and SC methods). For MCMO route the sintering was done at 1350 °C for 6 h. Synthesized samples prepared by various routes were investigated using X-ray diffraction (XRD) analysis, Field emission scanning electron microscopy (FESEM), Impedance network analyzer and transmission electron microscopy (TEM). The structural analysis reveals that the samples are of single phase structure and shows variations in the particle sizes and cells volumes, prepared by various routes. FESEM and TEM images depict that grain size increases with the increase of sintering temperature from 40 nm to 100 nm.Magnetic measurements reveal that garnet ferrite synthesized by sol gel method has high initial permeability (60.22) and low magnetic loss (0.0004) as compared to other garnet ferrite samples, which were synthesized by self combustion and MCMO methods. The M-H loops exhibit very low coercivity which enables the use of these materials in relays and switching devices fabrications. Thus, the garnet nanoferrites with low magnetic loss prepared by different methods may open new horizon for electronic industry for their use in high frequency applications.

Effects of two grading techniques of zirconia material on the fatigue limit of full-contour 3-unit fixed dental prostheses

PubMed Central

Villefort, Regina Furbino; Amaral, Marina; Pereira, Gabriel Kalil Rocha; Campos, Tiago Moreira Bastos; Zhang, Yu; Bottino, Marco Antonio; Valandro, Luiz Felipe; de Melo, Renata Marques

2017-01-01

Objective This study evaluated the effects of two grading zirconia techniques on the fatigue limit of 3-unit fixed dental prostheses (FDPs). Methods Presintered blocks of 3Y-TZP were milled to obtain sixty-nine 3-unit FDPs, which were divided into three groups (n = 23). The control group (CTL) was sintered and glazed following manufacturer’s instructuctions. The two experimental groups presintered FDPs received a surface silica/glass infiltration treatment before the sintering process. Silica sol-gel group (SSG) was graded by the sol-gel processing route, while the glass-zirconia-glass group (GZG) was graded by an enameling technique. Graded groups did not receive a glaze layer after sintering. All FDPs were then luted with a dual-curing resin cement on composite abutments, embedded in polyurethane and stored in water for five days. The initial load of the fatigue test was calculated based on the results of the monotonic testing applied on three specimens of each group. To determine the fatigue limit, 20 samples of each group were subjected to staircase testing (100,000 cycles/5 Hz). Results The fatigue limits (in Newtons) were CTL = 1607.27, SSG = 1824.31, and GZG = 2006.57, and the Dixon and Mood test indicated statistically significant differences among groups (95% confidence interval). Significance The infiltration of silica and glass on bulk zirconia, by two different grading methods, increased the fatigue limits of monolithic zirconia FDPs. PMID:28118929

Alumina polymorphs affect the metal immobilization effect when beneficially using copper-bearing industrial sludge for ceramics.

PubMed

Tang, Yuanyuan; Lu, Xiuqing; Shih, Kaimin

2014-12-01

The feasibility of recycling copper-bearing industrial sludge as a part of ceramic raw materials was evaluated through thermal interaction of sludge with aluminum-rich precursors. To observe copper incorporation mechanism, mixtures of copper-bearing sludge with alumina polymorphs (γ-Al2O3 and α-Al2O3) were fired between 750 and 1250°C. Different copper-hosting phases were identified by X-ray diffraction, and CuAl2O4 was found to be the predominant phase throughout the reactions. The experimental results indicate different CuAl2O4 initiating temperatures for two alumina materials, and the optimal temperature for CuAl2O4 formation is around 1100°C. To monitor the stabilization effect, prolonged leaching tests were carried out to leach sintered products for up to 20d. The results clearly demonstrate a substantial decrease in copper leachability for products with higher CuAl2O4 content formed from both alumina precursors despite their different sintering behavior. Meanwhile, the leachability of aluminum was much lower than that of copper, and it decreased by more than fourfold through the formation of CuAl2O4 spinel in γ-Al2O3 system. This study clearly indicates spinel formation as the most crucial metal stabilization mechanism when sintering multiphase copper-bearing industrial sludge with aluminum-rich ceramic raw materials, and suggests a promising and reliable technique for reusing industrial sludge. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

PubMed

Gunsoy, S; Ulusoy, M

2016-01-01

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

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.

Effect of milling and leaching on the structure of sintered silicon

NASA Technical Reports Server (NTRS)

Yeh, H. C.; Glascow, T. K.; Herbell, T. P.

1980-01-01

Sintering was performed in He for 16 hours at 1200, 1250, and 1300 C. Compacts of as-received Si did not densify during sintering. Milling reduced the average particle size to below 0.5 micrometer and enhanced densification (1.75 g/cc). Leaching milled Si further enhanced densification (1.90 g/cc max.) and decreased structural coarsening. After sintering, the structure of the milled and leached powder compacts appears favorable for the production of reaction bonded silicon nitride.

Structural comparison of sintering products made of "TiC + Ti" composite powders and "Ti + C" powder mixtures

NASA Astrophysics Data System (ADS)

Krinitcyn, Maksim G.; Pribytkov, Gennadii A.; Korosteleva, Elena N.; Firsina, Irina A.; Baranovskii, Anton V.

2017-12-01

In this study, powder composite materials comprised of TiC and Ti with different ratios are processed by sintering of Ti and C powder mixtures and self-propagating high-temperature synthesis (SHS) in "Ti+C" system followed by sintering. The microstructure and porosity of obtained composites are investigated and discussed. The dependence of porosity on sintering time is explained theoretically. Optimal regimes that enable to obtain the most homogeneous structure with the least porosity are described.

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

Ozturk, Fahrettin; Toros, Serkan; Evis, Zafer

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

SINTERED REFRACTORY MASS

DOEpatents

Williams, A.E.

1955-09-01

A method is given for joining sintered masses of refractory compounds. It consists in maintaining the masses in contact with each other by application of a moderate pressure, while they are at sintering temperature. The sintered masses are subjected to am applied pressure of about 1/2 to 1 ton per square inch of the surface in contact for about 10 minutes, and the temperature employed may be fropn about 1400 deg C to 2000 deg C. Refractory oxides to which the invention may be applied are beryllia, alumina, thoria, and magnesia.

Fabrication of turbine components and properties of sintered silicon nitride

NASA Technical Reports Server (NTRS)

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

1982-01-01

This paper presents a status report on the injection molding of sinterable silicon nitride at GTE Laboratories. The effort involves fabrication of single axial turbine blades and monolithic radial turbine rotors. The injection molding process is reviewed and the fabrication of the turbine components discussed. Oxidation resistance and strength results of current injection molded sintered silicon nitride as well as dimensional checks on sintered turbine blades demonstrate that this material is a viable candidate for high temperature structural applications.

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.

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

NASA Astrophysics Data System (ADS)

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

2018-04-01

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

Radiation-Thermal Sintering of Zirconia Powder Compacts Under Conditions of Bilateral Heating Using Beams of Low-Energy Electrons

NASA Astrophysics Data System (ADS)

Ghyngazov, S. A.; Frangulyan, T. S.; Chernyavskii, A. V.; Goreev, A. K.; Naiden, E. P.

2015-06-01

Comparative experiments on sintering zirconia ceramics are performed using colliding beams of low-energy electrons and under conditions of thermal heating. The density and microhardness of ceramic materials manufactured via different processes are determined. The use of a regime of bilateral heating by high-intensity,low-energy electron beams is shown to intensify the sintering process and yield material specimens with improved characteristics compared to those formed by thermal sintering.

Thermal barrier coating resistant to sintering

DOEpatents

Subramanian, Ramesh; Sabol, Stephen M.

2001-01-01

A device (10) having a ceramic thermal barrier coating layer (16) characterized by a microstructure having gaps (18) with a sintering inhibiting material (22) disposed on the columns (20) within the gaps (18). The sintering resistant material (22) is stable over the range of operating temperatures of the device (10) and is not soluble with the underlying ceramic layer (16). For a YSZ ceramic layer (16) the sintering resistant layer (22) may preferably be aluminum oxide or yttrium aluminum oxide, deposited as a continuous layer or as nodules.

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

Tiegs, T.N.

The Cooperative Research and Development Agreement (CRADA) was to develop composites of TiC-Ni{sub 3}Al with refined grain microstructures for application in diesel engine fuel injection devices. Grain refinement is important for improved wear resistance and high strength for the applications of interest. Attrition milling effectively reduces the initial particle size and leads to a reduction of the final grain size. However, an increase in the oxygen content occurs concomitantly with the grinding operation and decreased densification of the compacts occurs during sintering.

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

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.

Magnesia tuned multi-walled carbon nanotubes–reinforced alumina nanocomposites

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

Ahmad, Iftikhar, E-mail: ifahmad@ksu.edu.sa; Islam, Mohammad; Dar, Mushtaq Ahmad

2015-01-15

Magnesia tuned alumina ceramic nanocomposites, reinforced with multi-walled carbon nanotubes, were condensed using pressureless and hot-press sintering processes. Densification, microstructure and mechanical properties of the produced nanocomposites were meticulously investigated. Electron microscopy studies revealed the homogenous carbon nanotube dispersion within the alumina matrix and confirmed the retention of carbon nanotubes' distinctive tubular morphology and nanoscale features during the extreme mixing/sintering processes. Pressureless sintered nanocomposites showed meagre mechanical responses due to the poorly-integrated microstructures with a slight improvement upon magnesia addition. Conversely, both the magnesia addition and application of hot-press sintering technique resulted in the nanocomposite formation with near-theoretical densities (~more » 99%), well-integrated microstructures and superior mechanical properties. Hot-press sintered nanocomposites incorporating 300 and 600 ppm magnesia exhibited an increase in hardness (10 and 11%), flexural strength (5 and 10%) and fracture toughness (15 and 20%) with respect to similar magnesia-free samples. Compared to monolithic alumina, a decent rise in fracture toughness (37%), flexural strength (22%) and hardness (20%) was observed in the hot-press sintered nanocomposites tuned with merely 600 ppm magnesia. Mechanically superior hot-press sintered magnesia tailored nanocomposites are attractive for several load-bearing structural applications. - Highlights: • MgO tailored Al{sub 2}O{sub 3}–2 wt.% CNT nanocomposites are presented. • The role of MgO and sintering on nanocomposite structures and properties was studied. • Well-dispersed CNTs maintained their morphology/structure after harsh sintering. • Hot-pressing and MgO led nanocomposites to higher properties/unified structures. • MgO tuned composites showed higher toughness (37%) and strength (22%) than Al{sub 2}O{sub 3}.« less

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.

Optimization of sintering conditions for cerium-doped yttrium aluminum garnet

NASA Astrophysics Data System (ADS)

Cranston, Robert Wesley McEachern

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

Low temperature sintering of fluorapatite glass-ceramics

PubMed Central

Denry, Isabelle; Holloway, Julie A.

2014-01-01

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. 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. 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. Disc-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. 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. PMID:24252652

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.

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.

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

NASA Astrophysics Data System (ADS)

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

2002-10-01

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

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.

Method of forming a ceramic to ceramic joint

DOEpatents

Cutler, Raymond Ashton; Hutchings, Kent Neal; Kleinlein, Brian Paul; Carolan, Michael Francis

2010-04-13

A method of joining at least two sintered bodies to form a composite structure, includes: providing a joint material between joining surfaces of first and second sintered bodies; applying pressure from 1 kP to less than 5 MPa to provide an assembly; heating the assembly to a conforming temperature sufficient to allow the joint material to conform to the joining surfaces; and further heating the assembly to a joining temperature below a minimum sintering temperature of the first and second sintered bodies. The joint material includes organic component(s) and ceramic particles. The ceramic particles constitute 40-75 vol. % of the joint material, and include at least one element of the first and/or second sintered bodies. Composite structures produced by the method are also disclosed.

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.

Onset conditions for flash sintering of UO 2

DOE PAGES

Raftery, Alicia M.; Pereira da Silva, João Gustavo; Byler, Darrin D.; ...

2017-06-22

In this paper, flash sintering was demonstrated on stoichiometric and non-stoichiometric uranium dioxide pellets at temperatures ranging from room temperature (26°C) up to 600°C. The onset conditions for flash sintering were determined for three stoichiometries (UO 2.00, UO 2.08, and UO 2.16) and analyzed against an established thermal runaway model. The presence of excess oxygen was found to enhance the flash sintering onset behavior of uranium dioxide, lowering the field required to flash and shortening the time required for a flash to occur. Finally, the results from this study highlight the effect of stoichiometry on the flash sintering behavior ofmore » uranium dioxide and will serve as the foundation for future studies on this material.« less

Onset conditions for flash sintering of UO2

NASA Astrophysics Data System (ADS)

Raftery, Alicia M.; Pereira da Silva, João Gustavo; Byler, Darrin D.; Andersson, David A.; Uberuaga, Blas P.; Stanek, Christopher R.; McClellan, Kenneth J.

2017-09-01

In this work, flash sintering was demonstrated on stoichiometric and non-stoichiometric uranium dioxide pellets at temperatures ranging from room temperature (26 °C) up to 600 °C . The onset conditions for flash sintering were determined for three stoichiometries (UO2.00, UO2.08, and UO2.16) and analyzed against an established thermal runaway model. The presence of excess oxygen was found to enhance the flash sintering onset behavior of uranium dioxide, lowering the field required to flash and shortening the time required for a flash to occur. The results from this study highlight the effect of stoichiometry on the flash sintering behavior of uranium dioxide and will serve as the foundation for future studies on this material.

Nanocrystalline Iron-Cobalt Alloys for High Saturation Indutance

DTIC Science & Technology

2016-02-24

toroid. Before fully embarking on the problem of creating the toroid’s from particles sintered by a process known as sparked plasma sintering which...allows the particles to be rapidly sintered without compromising the nano crystalline particle size, it was deemed necessary to anticipate the

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.

SINTERING AND SULFATION OF CALCIUM SILICATE-ALUMINATE

EPA Science Inventory

The effect of sintering on the reactivity of solids at high temperature was studied. The nature of the interaction was studied with calcium silicate-aluminate reacting with SO2 between 665 and 800 C. The kinetics of the sintering and sulfation processes were measured independentl...

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.

Fabrication of low thermal expansion SiC/ZrW2O8 porous ceramics

NASA Astrophysics Data System (ADS)

Poowancum, A.; Matsumaru, K.; Juárez-Ramírez, I.; Torres-Martínez, L. M.; Fu, Z. Y.; Lee, S. W.; Ishizaki, K.

2011-03-01

Low or zero thermal expansion porous ceramics are required for several applications. In this work near zero thermal expansion porous ceramics were fabricated by using SiC and ZrW2O8 as positive and negative thermal expansion materials, respectively, bonded by soda lime glass. The mixture of SiC, ZrW2O8 and soda lime glass was sintered by Pulsed Electric Current Sintering (PECS, or sometimes called Spark Plasma Sintering, SPS) at 700 °C. Sintered samples with ZrW2O8 particle size smaller than 25 μm have high thermal expansion coefficient, because ZrW2O8 has the reaction with soda lime glass to form Na2ZrW3O12 during sintering process. The reaction between soda lime glass and ZrW2O8 is reduced by increasing particle size of ZrW2O8. Sintered sample with ZrW2O8 particle size 45-90 μm shows near zero thermal expansion.

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

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

NASA Astrophysics Data System (ADS)

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

2013-11-01

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

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.

Fabrication of porous titanium implants by three-dimensional printing and sintering at different temperatures.

PubMed

Xiong, Yaoyang; Qian, Chao; Sun, Jian

2012-01-01

This study evaluated the feasibility of using three-dimensional printing (3DP) to fabricate porous titanium implants. Titanium powder was blended with a water-soluble binder material. Green, porous, titanium implants fabricated by 3DP were sintered under protective argon atmosphere at 1,200, 1,300, or 1,400°C. Sintered implant prototypes had uniform shrinkage and no obvious shape distortion after sintering. Evaluation of their mechanical properties revealed that titanium prototypes sintered at different temperatures had elastic modulus of 5.9-34.8 GPa, porosity of 41.06-65.01%, hardness of 115.2-182.8 VHN, and compressive strength of 81.3-218.6 MPa. There were significant differences in each type of these data among the different sintering temperatures (p<0.01). Results of this study confirmed the feasibility of fabricating porous titanium implants by 3DP: pore size and pore interconnectivity were conducive to bone cell ingrowth for implant stabilization, and the mechanical properties matched well with those of the human bone.

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

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.

Development and Investigation of Tungsten Copper Sintered Parts for Using in Medium and High Voltage Switching Devices

NASA Astrophysics Data System (ADS)

Lungu, M. V.; Lucaci, M.; Tsakiris, V.; Brătulescu, A.; Cîrstea, C. D.; Marin, M.; Pătroi, D.; Mitrea, S.; Marinescu, V.; Grigore, F.; Tălpeanu, D.; Stancu, N.; Godeanu, P.; Melnic, C.

2017-06-01

Abstract Tungsten-copper (W-Cu) sintered parts with 75 wt.% W, 24 wt.% Cu and 1 wt.% Ni for using as arcing contacts in medium and high voltage switching devices were developed successfully by powder metallurgy (PM) techniques. Sintered parts with diameter of 50±0.5 mm and height of 6±0.5 mm were manufactured by pressing-sintering-infiltration (P-S-I) and spark plasma sintering (SPS) at sintering temperature of 1150°C, and 1050°C, respectively. Physical, chemical, electrical, thermal and mechanical properties of the samples were investigated. Microstructure was analyzed by optical microscopy and scanning electron microscopy. Material properties were influenced by the consolidation processes. The best results were achieved by SPS process. The relative density was more than 95 %, Vickers hardness HV1/15 was over 227, elastic modulus was over 143 GPa, and homogeneous microstructure was revealed. These good properties can contribute to higher lifetime of arcing contacts under severe working conditions.

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.

Effect of sintering time on the performance of turmeric dye-sensitized solar cells

NASA Astrophysics Data System (ADS)

Basuki, Hidajat, R. Lullus Lambang G.; Suyitno, Kristiawan, Budi; Rachmanto, Rendy Adhi

2017-01-01

This study reports the effect of sintering time on the performance of the dye-sensitized solar cells with turmeric dyes as sensitizers. Sintering TiO2 semiconductors were conducted at a temperature of 450°C for 30, 50, 90, 120, 150, and 180 minutes. The natural dye was extracted from dried turmeric powders with ethanol solvent. The results show that size of grains and the opening area of TiO2 semiconductor depended on the sintering time. The improvement of the properties of TiO2 semiconductor allowed more turmeric dyes were adsorbed by the semiconductors and then improved the performance of solar cells. The sintering time of 150 minutes produced large grains with an average diameter of 68.87 nm, and a porosity area of 26.51% caused the performance of DSSCs was the highest among other sintering time. The Voc, Jsc, and efficiency of DSSCs with turmeric-based natural dyes 0.64 V, 0.47 mA/cm2, and 0.2%, respectively.

The Effects of High Al2O3 on the Metallurgical Properties of Sinter

NASA Astrophysics Data System (ADS)

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

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

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

NASA Astrophysics Data System (ADS)

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

2013-08-01

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

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

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

NASA Astrophysics Data System (ADS)

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

2012-12-01

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

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.

Matrix Structure Evolution and Nanoreinforcement Distribution in Mechanically Milled and Spark Plasma Sintered Al-SiC Nanocomposites.

PubMed

Saheb, Nouari; Aliyu, Ismaila Kayode; Hassan, Syed Fida; Al-Aqeeli, Nasser

2014-09-19

Development of homogenous metal matrix nanocomposites with uniform distribution of nanoreinforcement, preserved matrix nanostructure features, and improved properties, was possible by means of innovative processing techniques. In this work, Al-SiC nanocomposites were synthesized by mechanical milling and consolidated through spark plasma sintering. Field Emission Scanning Electron Microscope (FE-SEM) with Energy Dispersive X-ray Spectroscopy (EDS) facility was used for the characterization of the extent of SiC particles' distribution in the mechanically milled powders and spark plasma sintered samples. The change of the matrix crystallite size and lattice strain during milling and sintering was followed through X-ray diffraction (XRD). The density and hardness of the developed materials were evaluated as function of SiC content at fixed sintering conditions using a densimeter and a digital microhardness tester, respectively. It was found that milling for 24 h led to uniform distribution of SiC nanoreinforcement, reduced particle size and crystallite size of the aluminum matrix, and increased lattice strain. The presence and amount of SiC reinforcement enhanced the milling effect. The uniform distribution of SiC achieved by mechanical milling was maintained in sintered samples. Sintering led to the increase in the crystallite size of the aluminum matrix; however, it remained less than 100 nm in the composite containing 10 wt.% SiC. Density and hardness of sintered nanocomposites were reported and compared with those published in the literature.

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 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.

Bone regeneration in 3D printing bioactive ceramic scaffolds with improved tissue/material interface pore architecture in thin-wall bone defect.

PubMed

Shao, Huifeng; Ke, Xiurong; Liu, An; Sun, Miao; He, Yong; Yang, Xianyan; Fu, Jianzhong; Liu, Yanming; Zhang, Lei; Yang, Guojing; Xu, Sanzhong; Gou, Zhongru

2017-04-12

Three-dimensional (3D) printing bioactive ceramics have demonstrated alternative approaches to bone tissue repair, but an optimized materials system for improving the recruitment of host osteogenic cells into the bone defect and enhancing targeted repair of the thin-wall craniomaxillofacial defects remains elusive. Herein we systematically evaluated the role of side-wall pore architecture in the direct-ink-writing bioceramic scaffolds on mechanical properties and osteogenic capacity in rabbit calvarial defects. The pure calcium silicate (CSi) and dilute Mg-doped CSi (CSi-Mg6) scaffolds with different layer thickness and macropore sizes were prepared by varying the layer deposition mode from single-layer printing (SLP) to double-layer printing (DLP) and then by undergoing one-, or two-step sintering. It was found that the dilute Mg doping and/or two-step sintering schedule was especially beneficial for improving the compressive strength (∼25-104 MPa) and flexural strength (∼6-18 MPa) of the Ca-silicate scaffolds. The histological analysis for the calvarial bone specimens in vivo revealed that the SLP scaffolds had a high osteoconduction at the early stage (4 weeks) but the DLP scaffolds displayed a higher osteogenic capacity for a long time stage (8-12 weeks). Although the DLP CSi scaffolds displayed somewhat higher osteogenic capacity at 8 and 12 weeks, the DLP CSi-Mg6 scaffolds with excellent fracture resistance also showed appreciable new bone tissue ingrowth. These findings demonstrate that the side-wall pore architecture in 3D printed bioceramic scaffolds is required to optimize for bone repair in calvarial bone defects, and especially the Mg doping wollastontie is promising for 3D printing thin-wall porous scaffolds for craniomaxillofacial bone defect treatment.