Consolidation of copper and aluminium powders by spark plasma sintering

Science.gov (United States)

Saiprasad, M.; Atchayakumar, R.; Thiruppathi, K.; Raghuraman, S.

2016-09-01

Processing in the powder metallurgy route has emerged as an economical process for the production of near net shaped components with a wide range of desired mechanical properties suitable for various applications of industrial needs. This research work was conducted with an objective of studying the improvisation of density and hardness of Copper-Aluminium alloy prepared by spark plasma sintering. Cu-Al alloy with a composition of 95% copper and 5% aluminium was prepared by SPS process. SPS is a low voltage, DC pulse current activated, pressure-assisted sintering, which enables sintering at lower temperatures and shorter durations. The combination offered by Cu-Al alloy of high strength and high corrosion resistance results their applications under a wide variety of conditions. The density and hardness of the prepared sample were measured by conducting appropriate tests. Apparently, the values of hardness and density of the specimen prepared by SPS seemed to be better than that of conventional sintering. The experimental procedure, testing methodologies and analysis are presented.

Quartz crystal reinforced quartz glass by spark plasma sintering

International Nuclear Information System (INIS)

Torikai, D.; Barazani, B.; Ono, E.; Santos, M.F.M.; Suzuki, C.K.

2011-01-01

The Spark Plasma Sintering presents fast processing time when compared to conventional sintering techniques. This allows to control the grain growth during sintering as well as the diffusion rate of a multi-material compounds, and make possible obtainment of functionally graded materials and nanostructured compounds. Powders of high purity silica glass and crystalline silica were sintered in a SPS equipment at temperatures around 1350° C, i.e., above the softening temperature of silica glass and below the melting temperature of quartz crystal. As a result, glass ceramics with pure silica glass matrix reinforced with crystalline alpha-quartz grains were fabricated at almost any desired range of composition, as well as controlled size of the crystalline reinforcement. X-ray diffraction and density measurements showed the possibility to manufacture a well controlled density and crystallinity glass-ceramic materials. (author)

Process parameter influence on Electro-sinter-forging (ESF) of titanium discs

DEFF Research Database (Denmark)

Cannella, Emanuele; Nielsen, Chris Valentin; Bay, Niels

Electro-sinter-forging (ESF) is an innovative sintering process based on the principle of electrical Joule heating. The electrical current is flowing through the powder compact, which is under mechanical pressure. As compared to conventional sintering [1] and spark plasma sintering [2], the main...... advantages are the decreased sintering time and high relative density [3]. Near net-shape components can be manufactured and post-removal processing is limited to surface polishing. The present work is focused on analysing the influence of the main process parameters, namely compacting pressure, sintering...... time and electrical current density, on the final density of a disc sample made from commercially pure titanium powder. The maximum achieved relative density was 94% of the bulk density of pure titanium. The density estimation was carried out by using both Archimedes’ and 3D scanning....

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

Science.gov (United States)

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

2016-10-01

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

Spark plasma sintering of tantalum carbide

International Nuclear Information System (INIS)

Khaleghi, Evan; Lin, Yen-Shan; Meyers, Marc A.; Olevsky, Eugene A.

2010-01-01

A tantalum carbide powder was consolidated by spark plasma sintering. The specimens were processed under various temperature and pressure conditions and characterized in terms of relative density, grain size, rupture strength and hardness. The results are compared to hot pressing conducted under similar settings. It is shown that high densification is accompanied by substantial grain growth. Carbon nanotubes were added to mitigate grain growth; however, while increasing specimens' rupture strength and final density, they had little effect on grain growth.

Influence of spark plasma sintering conditions on the sintering and functional properties of an ultra-fine grained 316L stainless steel obtained from ball-milled powder

Energy Technology Data Exchange (ETDEWEB)

Keller, C., E-mail: clement.keller@insa-rouen.fr [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Tabalaiev, K.; Marnier, G. [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Noudem, J. [Laboratoire de Cristallographie des Matériaux, CNRS-UMR 6508, Université de Caen, ENSICAEN, 7 bd du Maréchal Juin, 14050 Caen (France); Sauvage, X. [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Hug, E. [Laboratoire de Cristallographie des Matériaux, CNRS-UMR 6508, Université de Caen, ENSICAEN, 7 bd du Maréchal Juin, 14050 Caen (France)

2016-05-17

In this work, 316L samples with submicrometric grain size were sintered by spark plasma sintering. To this aim, 316L powder was first ball-milled with different conditions to obtain nanostructured powder. The process control agent quantity and milling time were varied to check their influence on the crystallite size of milled powder. Samples were then sintered by spark plasma sintering using different sets of sintering parameters (temperature, dwell time and pressure). For each sample, grain size and density were systematically measured in order to investigate the influence of the sintering process on these two key microstructure parameters. Results show that suitable ball-milling and subsequent sintering can be employed to obtain austenitic stainless steel samples with grain sizes in the nanometer range with porosity lower than 3%. However, ball-milling and subsequent sintering enhance chromium carbides formation at the sample surface in addition to intragranular and intergranular oxides in the sample as revealed by X-ray diffraction and transmission electron microscopy. It has been shown that using Boron nitride together with graphite foils to protect the mold from powder welding prevent such carbide formation. For mechanical properties, results show that the grain size refinement strongly increases the hardness of the samples without deviation from Hall-Petch relationship despite the oxides formation. For corrosion resistance, grain sizes lower than a few micrometers involve a strong decrease in the pitting potential and a strong increase in passivation current. As a consequence, spark plasma sintering can be considered as a promising tool for ultra-fine grained austenitic stainless steel.

Understanding the spark plasma sintering from the view of materials joining

International Nuclear Information System (INIS)

Dong, Peng; Wang, Zhe; Wang, Wenxian; Chen, Shaoping; Zhou, Jun

2016-01-01

Spark plasma sintering (SPS) is an attractive consolidation process. However, the mechanism behind this process is still an open topic for debate. This paper presents the first attempt to understand the SPS mechanism from perspective of materials joining. For this, TiNi_f/Al composites were fabricated by SPS, and the interfacial microstructures were investigated using field emission scanning electron microscopy and transmission electron microscopy. According to the experimental results, several joining processes were reflected well during SPS, involving micro-arc welding, electric resistance welding and diffusion welding. The proposed understanding of SPS will be helpful to the control of sintering quality.

Surface martensitization of Carbon steel using Arc Plasma Sintering

Science.gov (United States)

Wahyudi, Haris; Dimyati, Arbi; Sebayang, Darwin

2018-03-01

In this paper new technology of surface structure modification of steel by short plasma exposure in Arc Plasma Sintering (APS) device is presented. APS is an apparatus working based on plasma generated by DC pulsed current originally used for synthesizing materials via sintering and melting. Plasma exposure in APS was applied into the specimens for 1 and 3 seconds which generate temperature approximately about 1300-1500°C. The SUP9, pearlitic carbon steel samples were used. The hardness, hardening depth and microstructure of the specimens have been investigated by Vickers micro hardness test and Scanning Electron Microscopy (SEM) supported by Energy Dispersive X-Ray Spectroscopy (EDX). The results have showed that the mechanical property was significantly improved due to the formation of single martensitic structures as identified by SEM. The hardness of treated surface evaluated by Vickers hardness test showed significant improvement nearly three time from 190 VHN before to 524 VHN after treatment. Furthermore, EDX confirmed that the formation of martensite layer occurred without altering its composition. The APS also produced uniform hardened layer up to 250 μm. The experiment has demonstrated that arc plasma process was successfully improved the mechanical properties of steel in relatively very short time.

Structural and magnetic properties of γ-Fe{sub 2}O{sub 3} nanostructured compacts processed by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Saravanan, P., E-mail: psdrdo@gmail.com [Department of Physics, National Taiwan University, Taipei 106, Taiwan (China); Defence Metallurgical Research Laboratory, Hyderabad 500058 (India); Hsu, Jen-Hwa, E-mail: jhhsu@phys.ntu.edu.tw [Department of Physics, National Taiwan University, Taipei 106, Taiwan (China); Sivaprahasam, D. [International Advanced Research Centre for Powder Metallurgy and New Materials, Chennai 600113 (India); Kamat, S.V. [Defence Metallurgical Research Laboratory, Hyderabad 500058 (India)

2013-11-15

Gram quantities of γ-Fe{sub 2}O{sub 3} nanopowders having mean particle size of 20±4 nm were synthesized using a hydrothermal method and then consolidated into dense nanostructured compacts by spark plasma sintering (SPS) at relatively low temperatures: 300–350 °C. The cubic spinel structure of the as-synthesized γ-Fe{sub 2}O{sub 3} nanoparticles (NPs) did not get altered by the SPS process; nevertheless, a moderate increase in their grain sizes was evident in the SPSed compacts (80–125 nm). The physical properties such as density (ρ), coercivity (H{sub c}) and magnetization (M{sub s}) values of γ-Fe{sub 2}O{sub 3} NPs were affected by the SPS temperature. Significantly, higher values of ρ (4.45 g/cm{sup 3}), H{sub c} (274 Oe) and M{sub s} (67.2 emu/g) were achieved for the bulk compact SPSed at 350 °C. This work highlights the merits of sintering γ-Fe{sub 2}O{sub 3} NPs by SPS –as a new method of compaction with useful magnetic properties; which cannot be realized with the conventional sintering techniques. Highlights: • γ-Fe{sub 2}O{sub 3} nanoparticles with mean size of 20±4 nm were hydrothermally synthesized. • Spark plasma sintering of γ-Fe{sub 2}O{sub 3} was performed below phase transition temperature. • Sintered compacts were investigated with respect to SPS temperature: 300–350 °C. • Cubic spinel structure of γ-Fe{sub 2}O{sub 3} nanoparticles was retained in sintered compacts. • Maximum values: ρ (4.45 g/cm{sup 3}), H{sub c} (274 Oe) and M{sub s} (67.2 emu/g) obtained at 350 °C.

Sintering of Fine Particles in Suspension Plasma Sprayed Coatings

Directory of Open Access Journals (Sweden)

Leszek Latka

2010-07-01

Full Text Available Suspension plasma spraying is a process that enables the production of finely grained nanometric or submicrometric coatings. The suspensions are formulated with the use of fine powder particles in water or alcohol with some additives. Subsequently, the suspension is injected into plasma jet and the liquid additives evaporate. The remaining fine solids are molten and subsequently agglomerate or remain solid, depending on their trajectory in the plasma jet. The coating’s microstructure results from these two groups of particles arriving on a substrate or previously deposited coating. Previous experimental studies carried out for plasma sprayed titanium oxide and hydroxyapatite coatings enabled us to observe either a finely grained microstructure or, when a different suspension injection mode was used, to distinguish two zones in the microstructure. These two zones correspond to the dense zone formed from well molten particles, and the agglomerated zone formed from fine solid particles that arrive on the substrate in a solid state. The present paper focuses on the experimental and theoretical analysis of the formation process of the agglomerated zone. The experimental section establishes the heat flux supplied to the coating during deposition. In order to achieve this, calorimetric measurements were made by applying experimental conditions simulating the real coatings’ growth. The heat flux was measured to be in the range from 0.08 to 0.5 MW/m2,depending on the experimental conditions. The theoretical section analyzes the sintering during the coating’s growth, which concerns the fine particles arriving on the substrate in the solid state. The models of volume, grain boundary and surface diffusion were analyzed and adapted to the size and chemistry of the grains, temperature and time scales corresponding to the suspension plasma spraying conditions. The model of surface diffusion was found to best describe the sintering during suspension

Preparation of silicon carbide/carbon fiber composites through high-temperature spark plasma sintering

Directory of Open Access Journals (Sweden)

Ehsan Ghasali

2017-12-01

Full Text Available This study discusses the potentials of spark plasma sintering (SPS integrated with high temperature process that can enable sintering of SiC/Cf composites without any sintering aids. The random distribution of carbon fibers was obtained through mixing composite components in ethanol by using a shaker mill for 10 min. The corresponding sintering process was carried out at 1900 and 2200 °C with 50 MPa pressure applied at maximum temperature. The results showed that 89 ± 0.9 and 97 ± 0.8% of the theoretical density can be obtained for sintering temperatures of 1900 and 2200 °C, respectively. The densification curves were plotted to monitor sintering behavior with punch displacement changes. The appropriate bonding between SiC particles and carbon fibers was detected using FE-SEM for sample which was sintered at 2200 °C. The clear maximum in hardness (2992 ± 33 Vickers, bending strength (427 ± 26 MPa and fracture toughness (4.2 ± 0.3 MPa m1/2 were identified for sample sintered at 2200 °C. XRD investigations supposed that SiC and carbon were the only crystalline phases in both sintered samples.

Low temperature spark plasma sintering of YIG powders

International Nuclear Information System (INIS)

Fernandez-Garcia, L.; Suarez, M.; Menendez, J.L.

2010-01-01

A transition from a low to a high spin state in the magnetization saturation between 1000 and 1100 o C calcination temperature is observed in YIG powders prepared by oxides mixture. Spark plasma sintering of these powders between 900 and 950 o C leads to dense samples with minimal formation of YFeO 3 , opening the way to co-sintering of YIG with metals or metallic alloys. The optical properties depend on the sintering stage: low (high) density samples show poor (bulk) optical absorption.

Inversion defects in MgAl2O4 elaborated by pressureless sintering, pressureless sintering plus hot isostatic pressing, and spark plasma sintering

International Nuclear Information System (INIS)

Mussi, A.; Granger, G. Bernard; Addad, A.; Benameur, N.; Beclin, F.; Bataille, A.

2009-01-01

The distribution of inversion defects of Al was investigated in dense magnesium-aluminate spinel elaborated by pressureless sintering, pressureless sintering plus hot isostatic pressing, and spark plasma sintering. This study was conducted by energy electron loss spectroscopy analyses and more particularly by energy loss near edge structure investigations of the Al-L 2,3 edge. Several aspects are discussed with the purpose of understanding why charged defects dispersal reveals a special configuration.

Microstructure and thermoelectric properties of β-FeSi2 ceramics fabricated by hot-pressing and spark plasma sintering

International Nuclear Information System (INIS)

Qu Xiurong; Lue Shuchen; Hu Jianmin; Meng Qingyu

2011-01-01

Highlights: → With increasing hot-pressing (HP) temperature, the thermoelectric figure of merit of β-FeSi 2 ceramics is improved slightly. → The grain size of the sample sintered by the spark plasma sintering (SPS) process is smaller than that by the HP process. → The SPS sample shows excellent thermoelectric performance attributed to low thermal conductivity. - Abstract: The microstructure and thermoelectric properties of β-FeSi 2 ceramics by hot pressing (HP) and spark plasma sintering (SPS) are investigated. With increasing hot-pressing temperature, the density, electronic conductivity and thermal conductivity of the samples increase significantly, the thermoelectric figure of merit is improved slightly. The microstructure study indicates that the sizes of the β-FeSi 2 and ε-FeSi phases in the sample sintered by the SPS process are smaller than that by the HP process. The SPS sample shows excellent thermoelectric performance due to the low thermal conductivity.

Simulated UO{sub 2} fuel containing CsI by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Wangle, T. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, 76125 Karlsruhe (Germany); Czech Technical University in Prague, Faculty of Nuclear Sciences and Physical Engineering, Břehová 7, Praha 1, 115 19 (Czech Republic); Tyrpekl, V. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, 76125 Karlsruhe (Germany); Cologna, M., E-mail: marco.cologna@ec.europa.eu [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, 76125 Karlsruhe (Germany); Somers, J. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, 76125 Karlsruhe (Germany)

2015-11-15

Herein, an innovative preparation procedure has been deployed enabling, for the first time, the incorporation of volatile fission product simulant into highly dense nuclear fuel pellets. Highly volatile fission products were embedded in a dense UO{sub 2} matrix in the form of CsI by simply mixing starting materials and consolidation in a Spark Plasma Sintering step at 1000 °C with a 5 min dwell time. CsI particles were evenly distributed throughout the pellet and were located at the grain boundaries. The sintering rate is dependent on the O/U ratio of the powder. Addition of CsI also acts as a sintering aid, reducing the temperature of maximum densification. - Highlights: • A new method was developed to incorporation of volatile fission products simulants into dense nuclear fuel pellets. • CsI doped UO{sub 2} pellets were synthetized for the first time, by Spark Plasma Sintering. • The sintering rate in Spark Plasma Sintering is dependent on the O/U ratio of UO{sub 2+x}.

Graphene-reinforced aluminum matrix composites prepared by spark plasma sintering

Institute of Scientific and Technical Information of China (English)

Wen-ming Tian; Song-mei Li; Bo Wang; Xin Chen; Jian-hua Liu; Mei Yu

2016-01-01

Graphene-reinforced 7055 aluminum alloy composites with different contents of graphene were prepared by spark plasma sinter-ing (SPS). The structure and mechanical properties of the composites were investigated. Testing results show that the hardness, compressive strength, and yield strength of the composites are improved with the addition of 1wt% graphene. A clean, strong interface is formed between the metal matrix and graphene via metallurgical bonding on atomic scale. Harmful aluminum carbide (Al4C3) is not formed during SPS processing. Further addition of graphene (above 1wt%) results in the deterioration in mechanical properties of the composites. The agglomeration of graphene plates is exacerbated with increasing graphene content, which is the main reason for this deterioration.

Microstructure and properties of TiC-high manganese steel cermet prepared by different sintering processes

Energy Technology Data Exchange (ETDEWEB)

Wang, Zhi; Lin, Tao, E-mail: lintao@ustb.edu.cn; He, Xinbo; Shao, Huiping; Zheng, Jianshu; Qu, Xuanhui

2015-11-25

In the paper, the TiC −50 wt.% high manganese steel cermet was made with different sintering processes including vacuum sintering, hot pressing, microwave sintering and spark plasma sintering (SPS). The microstructure, porosity and fracture morphology of the samples were analyzed with scanning electron microscopy (SEM). Phase analysis was carried out using X-ray diffraction (XRD). The density, hardness, transverse rupture strength (TRS) and wear resistance were investigated for the effect of the sintering processes. The results showed that the core–shell structure was not clearly observed for the TiC particles in microstructures and the high manganese steel matrix is BCC structure. Hot pressing, microwave sintering and SPS are useful processes for densification of the cermet. Nearly full density and higher hardness can be reached by these three processes at a lower sintering temperature and in a shorter sintering time. However, higher TRS can be reached by means of alloying completely in a longer sintering time, for example vacuum sintering. Pre-sintering in a long sintering time at a lower sintering temperature is also useful for improving the TRS. Finally, vacuum sintering is an effective process for producing this composite with the lowest cost in the mass production. - Highlights: • TiC-high manganese steel cermets were prepared by four sintering processes. • The core–shell structure was not clearly observed for the TiC particles in microstructures. • Th high manganese steel matrix is BCC structure instead of FCC structure. • Pre-sintering before microwave sintering is also useful for improving the TRS. • Vacuum sintering can be effective way for prepare this cermet in mass production.

Spark plasma-sintered Sn-based intermetallic alloys and their Li-storage studies

CSIR Research Space (South Africa)

Nithyadharseni, P

2016-06-01

Full Text Available In the present study, SnSb, SnSb/Fe, SnSb/Co, and SnSb/Ni alloy powders processed by co-precipitation were subjected to spark plasma-sintering (SPS) at 400 °C for 5 min. The compacts were structurally and morphologically characterized by X...

Effects of Synthesis and Spark Plasma Sintering Conditions on the Thermoelectric Properties of Ca3Co4O9+δ

DEFF Research Database (Denmark)

Wu, NingYu; Holgate, Tim; Van Nong, Ngo

2013-01-01

Ca3Co4O9+δ samples were synthesized by solid-state (SS) and sol–gel (SG) reactions, followed by spark plasma sintering under different processing conditions. The synthesis process was optimized and the resulting materials characterized with respect to their microstructure, bulk density, and therm......Ca3Co4O9+δ samples were synthesized by solid-state (SS) and sol–gel (SG) reactions, followed by spark plasma sintering under different processing conditions. The synthesis process was optimized and the resulting materials characterized with respect to their microstructure, bulk density...

Spark plasma sintering and microwave electromagnetic properties of MnFe{sub 2}O{sub 4} ceramics

Energy Technology Data Exchange (ETDEWEB)

Penchal Reddy, M., E-mail: drlpenchal@gmail.com [Center for Advanced Materials, Qatar University, Doha 2713 (Qatar); Mohamed, A.M.A. [Center for Advanced Materials, Qatar University, Doha 2713 (Qatar); Department of Metallurgical and Materials Engineering, Faculty of Petroleum and Mining Engineering, Suez University, Suez 4372 (Egypt); Venkata Ramana, M. [Department of Physics, National Taiwan Normal University, Taipei 11677, Taiwan (China); Zhou, X.B.; Huang, Q. [Division of Functional Materials and Nanodevices, Ningbo Institute of Materials Technology and Engineering, Ningbo 315201 (China)

2015-12-01

MnFe{sub 2}O{sub 4} ferrite powder was synthesized by a facile one-pot hydrothermal route and then consolidated into dense nanostructured compacts by the spark plasma sintering (SPS) technique. The effect of sintering temperature, on densification, morphology, magnetic and microwave absorption properties was examined. Spark plasma sintering resulted in uniform microstructure, as well as maximum relative density of 98%. The magnetic analysis indicated that the MnFe{sub 2}O{sub 4} ferrite nanoparticles showed ferrimagnetic behavior. Moreover, the dielectric loss and magnetic loss properties of MnFe{sub 2}O{sub 4} ferrite nanoparticles were both enhanced due to its better dipole polarization, interfacial polarization and shape anisotropy. It is believed that such spark plasma sintered ceramic material will be applied widely in microwave absorbing area. - Highlights: • Successful synthesis of dense MnFe{sub 2}O{sub 4} ceramics using spark plasma sintering. • Lower temperature and shorter sintering time, compared to conventional methods. • Optimal sintering condition was achieved. • The magnetic properties of the sintered samples are sensitive to the density and microstructure.

Constrained sintering of an air-plasma-sprayed thermal barrier coating

International Nuclear Information System (INIS)

Cocks, A.C.F.; Fleck, N.A.

2010-01-01

A micromechanical model is presented for the constrained sintering of an air-plasma-sprayed, thermal barrier coating upon a thick superalloy substrate. The coating comprises random splats with intervening penny-shaped cracks. The crack faces make contact at asperities, which progressively sinter in-service by interfacial diffusion, accommodated by bulk creep. Diffusion is driven by the reduction in interfacial energy at the developing contacts and by the local asperity contact stress. At elevated operating temperature, both sintering and creep strains accumulate within the plane of the coating. The sensitivities of sintering rate and microstructure evolution rate to the kinetic parameters and thermodynamic driving forces are explored. It is demonstrated that the sintering response is governed by three independent timescales, as dictated by the material and geometric properties of the coating. Finally, the role of substrate constraint is assessed by comparing the rate of constrained sintering with that for free sintering.

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

International Nuclear Information System (INIS)

Dash, K.; Chaira, D.; Ray, B.C.

2013-01-01

Graphical abstract: The evolution of microstructure by varying the particle size of reinforcement in the matrix employing spark plasma sintering has been demonstrated here in Al–Al 2 O 3 system. An emphasis has been laid on varying the reinforcement particle size and evaluating the microstructural morphologies and their implications on mechanical performance of the composites. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size 2 O 3 micro- and nano-composites fabricated by spark plasma sintering. • Better matrix-reinforcement integrity in nanocomposites than microcomposites. • Spark plasma sintering method results in higher density and hardness values. • High density and hardness values of nanocomposites than microcomposites. • High dislocation density in spark plasma sintered Al–Al 2 O 3 composites. - Abstract: In the present study, an emphasis has been laid on evaluation of the microstructural morphologies and their implications on mechanical performance of the composites by varying the reinforcement particle size. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size 2 O 3 nancomposites respectively. Spark plasma sintering imparts enhanced densification and matrix-reinforcement proximity which have been corroborated with the experimental results

Microstructural designs of spark-plasma sintered silicon carbide ceramic scaffolds

Energy Technology Data Exchange (ETDEWEB)

Roman-Manso, B.; Pablos, A. de; Belmonte, M.; Osendi, M. I.; Miranzo, P.

2014-04-01

Concentrated ceramic inks based on (SiC) powders, with different amounts of Y{sub 2}O{sub 3} and Al{sub 2}O{sub 3} as sintering aids, are developed for the adequate production of SiC scaffolds, with different patterned morphologies, by the Robocasting technique. The densification of the as-produced 3D structures, previously heat treated in air at 600 degree centigrade for the organics burn-out, is achieved with a Spark Plasma Sintering (SPS) furnace. The effects of the amount of sintering additives (7 - 20 wt. %) and the size of the SiC powders (50 nm and 0.5 {mu}m) on the processing of the inks, microstructure, hardness and elastic modulus of the sintered scaffolds, are studied. The use of nano-sized (SiC) powders significantly restricts the attainable maximum solids volume fraction of the ink (0.32 compared to 0.44 of the submicron-sized powders-based ink), involving a much larger porosity of the green ceramic bodies. Furthermore, reduced amounts of additives improve the mechanical properties of the ceramic skeleton; particularly, the stiffness. The grain size and specific surface area of the starting powders, the ink solids content, green porosity, amount of sintering additives and SPS temperatures are the main parameters to be taken into account for the production of these SiC cellular ceramics. (Author)

Welding of titanium and nickel alloy by combination of explosive welding and spark plasma sintering technologies

Energy Technology Data Exchange (ETDEWEB)

Malyutina, Yu. N., E-mail: iuliiamaliutina@gmail.com; Bataev, A. A., E-mail: bataev@adm.nstu.ru; Shevtsova, L. I., E-mail: edeliya2010@mail.ru [Novosibirsk State Technical University, Novosibirsk, 630073 (Russian Federation); Mali, V. I., E-mail: vmali@mail.ru; Anisimov, A. G., E-mail: anis@hydro.nsc.ru [Lavrentyev Institute of Hydrodynamics SB RAS, Novosibirsk, 630090 (Russian Federation)

2015-10-27

A possibility of titanium and nickel-based alloys composite materials formation using combination of explosive welding and spark plasma sintering technologies was demonstrated in the current research. An employment of interlayer consisting of copper and tantalum thin plates makes possible to eliminate a contact between metallurgical incompatible titanium and nickel that are susceptible to intermetallic compounds formation during their interaction. By the following spark plasma sintering process the bonding has been received between titanium and titanium alloy VT20 through the thin powder layer of pure titanium that is distinguished by low defectiveness and fine dispersive structure.

Preparation of Ni-Ti shape memory alloy by spark plasma sintering method

Czech Academy of Sciences Publication Activity Database

Salvetr, P.; Kubatík, Tomáš František; Novák, P.

2016-01-01

Roč. 16, č. 4 (2016), s. 804-808 ISSN 1213-2489 Institutional support: RVO:61389021 Keywords : Ni-Ti alloy * Powder metallurgy * Reactive sintering * Spark plasma sintering Subject RIV: JK - Corrosion ; Surface Treatment of Materials

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

Science.gov (United States)

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

2017-07-01

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

Thermoelectric property of fine-grained CoSb3 skutterudite compound fabricated by mechanical alloying and spark plasma sintering

International Nuclear Information System (INIS)

Liu Weishu; Zhang Boping; Li Jingfeng; Zhao Lidong

2007-01-01

Skutterudite CoSb 3 polycrystalline materials were prepared using a combined process of mechanical alloying (MA) and spark plasma sintering (SPS). The influence of SPS temperature on the thermoelectric properties was focused in this work with a special emphasis on the analysis of the size effects of grains. The average grain sizes decreased from 300 to 50 nm with decreasing SPS temperatures from 600 to 300 deg. C. The electrical resistivities of samples spark plasma sintered at 300-600 deg. C all decreased with increasing temperature, indicating a classic intrinsic conduction behaviour of semiconductors. The samples spark plasma sintered at 300-500 deg. C showed a positive Seebeck coefficient while the sample spark plasma sintered at 600 deg. C showed a negative Seebeck coefficient. The room-temperature thermal conductivities were reduced from 4.30 to 2.92 W m -1 K -1 as the grain sizes were decreased from 300 to 100 nm corresponding to SPS at 600 and 400 deg. C, respectively. The present work indicates that MA and SPS is a good combination for fabricating fine-grained CoSb 3 thermoelectric materials

Plasma sintering of ferritic steel reinforced with niobium carbide prepared by high energy milling

International Nuclear Information System (INIS)

Silva Junior, J.F. da; Almeida, E.O.; Gomes, U.U.; Alves Junior, C.; Messias, A.P.; Universidade Federal do Rio Grande do Norte

2010-01-01

Plasma is an ionized gas where ions are accelerated from anode to cathode surface, where the sample is placed. There are a lot of collisions on cathode surface by ions heating and sintering the sample. High energy milling (HEM) is often used to produce composite particles to be used on powder metallurgy. These particles can exhibit fine particles and high phase dispersion. This present work aim to study ferritic steels reinforced with 3%NbC prepared by HEM and sintered on plasma furnace. Ferritic steel and NbC powders were milled during 5 hours and characterized by SEM, XRD and laser scattering. Then, these composite powders were compacted in a cylindrical steel die and then sintered in a plasma furnace. Vickers microhardness tests and SEM and XRD analysis were performed on sintered samples. (author)

Fiber-reinforced ceramic matrix composites processed by a hybrid technique based on chemical vapor infiltration, slurry impregnation and spark plasma sintering

International Nuclear Information System (INIS)

Magnant, J.; Pailler, R.; Le Petitcorps, Y.; Maille, L.; Guette, A.; Marthe, J.

2013-01-01

Fabrication of multidirectional continuous carbon and silicon carbide fiber reinforced ceramic matrix composites (CMC) by a new short time hybrid process was studied. This process is based, first, on the deposition of fiber interphase and coating by chemical vapor infiltration, next, on the introduction of silicon nitride powders into the fibrous preform by slurry impregnation and, finally, on the densification of the composite by liquid phase spark plasma sintering (LP-SPS). The homogeneous introduction of the ceramic charges into the multidirectional fiber pre-forms was realized by slurry impregnation from highly concentrated and well-dispersed aqueous colloid suspensions. The chemical degradation of the carbon fibers during the fabrication was prevented by adapting the sintering pressure cycle. The composites manufactured are dense. Microstructural analyses were conducted to explain the mechanical properties achieved. One main important result of this study is that LP-SPS can be used in some hybrid processes to densify fiber reinforced CMC. (authors)

Nanostructured cobalt powders synthesised by polyol process and consolidated by Spark Plasma Sintering: Microstructure and mechanical properties

Energy Technology Data Exchange (ETDEWEB)

Fellah, F.; Schoenstein, F.; Dakhlaoui-Omrani, A.; Cherif, S.M.; Dirras, G.; Jouini, N., E-mail: jouini@univ-paris13.fr

2012-07-15

Bulk nanostructured cobalt was processed using a bottom-up strategy. Nanostructured particle agglomerates of about 50 and 240 nm in diameter were synthesised using a polyol route and subsequently consolidated by Spark Plasma Sintering (SPS). The microstructure of the starting powders and of the processed bulk samples was studied and characterised by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the as-prepared powders showed predominantly a face centred cubic (fcc) crystalline phase, whereas both fcc and hexagonal close packed (hcp) phases were found within the consolidated samples. A sample with the highest relative mass density (94.5%) was obtained from the small powder particles. TEM observations revealed a lamellar substructure with a high density of nanotwins and stacking faults in every grain in the sample with the highest density. Brillouin light scattering (BLS) and quasistatic compression tests were used to investigate the mechanical properties of the consolidated samples. The two techniques yielded Young modulus values of 168 GPa and 130 GPa, respectively, in the sample with the highest density. This sample also exhibited a yield stress higher than 1 GPa after the compression test, which is mainly attributed to the lamellar-like structure occurring in almost every grain of the polycrystalline aggregate. - Highlights: Black-Right-Pointing-Pointer Cobalt nanoparticles produced by the polyol process present mainly the fcc metastable phase. Black-Right-Pointing-Pointer Bulk nanostructured cobalt is obtained from the nano-particles by Spark Plasma Sintering consolidation. Black-Right-Pointing-Pointer Nanotwins and stacking faults are present in every grain of the more dense sample. Black-Right-Pointing-Pointer Yield strength and plastic domain may be varied depending on the nanoparticle size and the porosity of the consolidated material.

Sintering unalloyed titanium in DC electrical abnormal glow discharge

Directory of Open Access Journals (Sweden)

Allan Seeber

2010-03-01

Full Text Available Powder metallurgy is widely used in the manufacture of components that have complex geometry. The good dimensional control, reduction in manufacturing steps and operating costs which has favored the use of this technique for manufacturing of titanium alloys components. However, the high affinity of this material with oxygen hinders strongly the sintering process. For this, the sintering associated with plasma technology can be considered an alternative technique for the processing of this material. The strict control of sintering atmosphere performed at low pressures and the reactive species present in the plasma environment can help to improve the sintering of this material. The results presented in this paper show a good correlation between the parameters used for the compaction of the samples and the microstructure develop during the plasma sintering of samples. The microstructure of the plasma assisted samples is also affected by the particular configuration used in the plasma reactor.

Graphene-induced strengthening in spark plasma sintered tantalum carbide–nanotube composite

International Nuclear Information System (INIS)

Lahiri, Debrupa; Khaleghi, Evan; Bakshi, Srinivasa Rao; Li, Wei; Olevsky, Eugene A.; Agarwal, Arvind

2013-01-01

Transverse rupture strength of spark plasma sintered tantalum carbide (TaC) composites reinforced with long and short carbon nanotubes (CNTs) is reported. The rupture strength depends on the transformation behavior of the CNTs during spark plasma sintering, which is dependent on their length. The TaC composite with short nanotubes shows the highest specific rupture strength. Shorter CNTs transform into multi-layered graphene sheets between TaC grains, whereas long ones retain the tubular structure. Two-dimensionsal graphene platelets offer higher resistance to pull-out, resulting in delayed fracture and higher strength.

Preparation of Ti3Al intermetallic compound by spark plasma sintering

Science.gov (United States)

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.

Full densification of inkjet-printed copper conductive tracks on a flexible substrate utilizing a hydrogen plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Kwon, Young-Tae [Department of Fusion Chemical Engineering, Hanyang University, Ansan 15588 (Korea, Republic of); Lee, Young-In [Department of Materials Science and Engineering, Seoul National University of Science and Technology, Seoul 01811 (Korea, Republic of); Kim, Seil [Department of Fusion Chemical Engineering, Hanyang University, Ansan 15588 (Korea, Republic of); Lee, Kun-Jae [Department of Energy Engineering, Dankook University, Cheonan 31116 (Korea, Republic of); Choa, Yong-Ho, E-mail: choa15@hanyang.ac.kr [Department of Fusion Chemical Engineering, Hanyang University, Ansan 15588 (Korea, Republic of)

2017-02-28

Highlights: • Hydrogen thermally- and plasma- treatments are applied to reduce and sinter the inkjet-printed copper patterns at low temperature. • Plasma sintered Cu patterns have fully densified microstructure with the resistivity of 3.23 μW cm. • Cu conductive track with dense microstructure remains its electrical resistivity after 1 month. • Thermal sintered Cu patterns show a relatively poor microstructure and high resistivity. - Abstract: Low temperature sintering techniques are crucial in developing flexible printed electronics. In this work, we demonstrate a novel hydrogen plasma sintering method that achieves a full reduction and densification of inkjet-printed patterns using a copper complex ion ink. After inkjet printing on polyethylene terephthalate (PET) substrates, both hydrogen plasma and conventional hydrogen thermal treatment were employed to compare the resulting microstructures, electrical properties and anti-oxidation behavior. The plasma treated pattern shows a fully densified microstructure with a resistivity of 3.23 μΩ cm, while the thermally treated pattern shows a relatively poor microstructure and high resistivity. In addition, the hydrogen plasma-treated copper pattern retains its electrical resistivity for one month without any significant decrease. This novel hydrogen plasma sintering technique could be used to produce conductive patterns with excellent electrical properties, allowing for highly reliable flexible printed electronics.

Sintering, consolidation, reaction and crystal growth by the spark plasma system (SPS)

Energy Technology Data Exchange (ETDEWEB)

Omori, M. [Tohoku Univ., Sendai (Japan). Inst. for Materials Research

2000-08-15

The graphite die set in spark plasma system (SPS) is heated by a pulse direct current. Weak plasma, discharge impact, electric field and electric current, which are based on this current, induce good effects on materials in the die. The surface films of aluminum and pure WC powders are ruptured by the spark plasma. Pure AlN powder is sintered without sintering additives in the electric field. The spark plasma leaves discharge patterns on insulators. Organic fibers are etched by the spark plasma. Thermosetting polyimide is consolidated by the spark plasma. Insoluble polymonomethylsilane is rearranged into the soluble one by the spark plasma. A single crystal of CoSb{sub 3} is grown from the compound powders in the electric field by slow heating. Coupled crystals of eutectic powder are connected with each other in the electric field. (orig.)

Properties of sintered glass-ceramics prepared from plasma vitrified air pollution control residues

International Nuclear Information System (INIS)

Roether, J.A.; Daniel, D.J.; Amutha Rani, D.; Deegan, D.E.; Cheeseman, C.R.; Boccaccini, A.R.

2010-01-01

Air pollution control (APC) residues, obtained from a major UK energy from waste (EfW) plant, processing municipal solid waste, have been blended with silica and alumina and melted using DC plasma arc technology. The glass produced was crushed, milled, uni-axially pressed and sintered at temperatures between 750 and 1150 deg. C, and the glass-ceramics formed were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Mechanical properties assessed included Vickers's hardness, flexural strength, Young's modulus and thermal shock resistance. The optimum sintering temperature was found to be 950 deg. C. This produced a glass-ceramic with high density (∼2.58 g/cm 3 ), minimum water absorption (∼2%) and relatively high mechanical strength (∼81 ± 4 MPa). Thermal shock testing showed that 950 deg. C sintered samples could withstand a 700 deg. C quench in water without micro-cracking. The research demonstrates that glass-ceramics can be readily formed from DC plasma treated APC residues and that these have comparable properties to marble and porcelain. This novel approach represents a technically and commercially viable treatment option for APC residues that allow the beneficial reuse of this problematic waste.

Recycling of mill scale in sintering process

Directory of Open Access Journals (Sweden)

El-Hussiny N.A.

2011-01-01

Full Text Available This investigation deals with the effect of replacing some amount of Baharia high barite iron ore concentrate by mill scale waste which was characterized by high iron oxide content on the parameters of the sintering process., and investigation the effect of different amount of coke breeze added on sintering process parameters when using 5% mill scale waste with 95% iron ore concentrate. The results of this work show that, replacement of iron ore concentrate with mill scale increases the amount of ready made sinter, sinter strength and productivity of the sinter machine and productivity at blast furnace yard. Also, the increase of coke breeze leads to an increase the ready made sinter and productivity of the sintering machine at blast furnace yard. The productivity of the sintering machine after 5% decreased slightly due to the decrease of vertical velocity.

The effect of spark plasma sintering on lithium disilicate glass-ceramics.

Science.gov (United States)

Al Mansour, Fatima; Karpukhina, Natalia; Grasso, Salvatore; Wilson, Rory M; Reece, Mike J; Cattell, Michael J

2015-10-01

To evaluate the effects of spark plasma sintering (SPS) on the microstructure of lithium disilicate glass-ceramics. IPS e.max CAD glass-ceramic samples were processed using spark plasma sintering (SPS) and conventionally sintered (CS) as a comparison. Specimens were sintered at varying temperatures (T1: 840°C, T2: 820°C, T3: 800°C), heating rates (HR1: 150°C/min, HR2: 300°C/min, HR3: 500°C/min) and pressures (P1: 15MPa, P2: 50MPa, P3: 70MPa). IPS e.max Press glass powder samples were densified at 750 and 800°C (50 or 200MPa pressure). Samples were characterized using XRD, HTXRD, and SEM and quantitative image analysis. There was a significant increase in median crystal size (MCS) between the CS and the SPS T1 groups. A statistical difference (p>0.05) in MCS between SPS T1 and SPS T2 groups was observed. The SPS HR3 sample produced a smaller MCS than the CS, SPS HR1 and HR2 groups (pglass samples resulted in fine fibrils or graduated lithium disilicate crystals. The effects of SPS were used to refine the microstructure of IPS e.max CAD lithium disilicate glass-ceramics. Densification by SPS of IPS e.max Press glass resulted in textured and fine nano-crystalline microstructures. SPS generated glass-ceramic microstructures may have unique properties and could be useful in the production of CAD/CAM materials for dentistry. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Sintering-alkaline processing of borosilicate ores of Tajikistan

International Nuclear Information System (INIS)

Nazarov, F.A.

2018-01-01

The aim of the work is to study the processes of decomposition of boron-containing ore by sintering with NaOH, finding the optimal parameters of the decomposition process, studying the kinetics of processes and developing the technological foundations for ore processing. The processes of borosilicate ore processing were studied by sintering with NaOH. Possible mechanisms of chemical reactions of the process of sintering-alkaline decomposition of boron-containing ore are established, the results of which are substantiated by physicochemical methods of analysis. A principal technological scheme for processing of borosilicate ores by a sintering-alkaline method has been developed. In the first chapter, data on alkaline and caking processes for processing boron-containing and aluminium comprising raw materials are available in the literature. Based on this, the directions of our own research are outlined. The second chapter is devoted to the study of the chemical and mineralogical compositions of borosilicate ores and their concentrates with the help of X-ray phase and chemical analysis methods, the stoichiometric calculation of the formation of aluminum, iron, and boron salts has been carried out, and a thermodynamic analysis of the processes of sintering borosilicate ores with alkali has been considered. The third chapter presents the results of a study of sintering-alkaline method of processing of initial borosilicate ore of the Ak-Arkhar Deposit and its concentrate without calcination and after calcination. The kinetics of sintering of borosilicate ores with sodium hydroxide was studied. The optimal conditions of borosilicate ore sintering before and after the preliminary calcination with alkali were determined. Optimal parameters of the sintering process have been found: sintering temperature 800-8500 deg C, duration of the process - 60 minutes, mass ratio of NaOH to raw materials 2: 1. The conditions for sintering of borosilicate concentrate with alkali have been

Interface evolution and shear strength of Al/Ti bi-metals processed by a spark plasma sintering (SPS) apparatus

Energy Technology Data Exchange (ETDEWEB)

Miriyev, Aslan, E-mail: aslan.miriyev@columbia.edu [Department of Mechanical Engineering, Columbia University in the City of New York, 500 W. 120th St., Mudd 220, New York, NY 10027 (United States); Levy, Asaf; Kalabukhov, Sergey; Frage, Nachum [Department of Materials Engineering, Ben-Gurion University of the Negev, P.O.B. 653, Beer Sheva 8410501 (Israel)

2016-09-05

Microstructural evolution of the Al/Ti bi-metal interface during heat treatment in a spark plasma sintering (SPS) apparatus was investigated under various conditions for the first time. A mechanism of interfacial layer growth was suggested based on the results of SEM, TEM and X-ray diffraction analysis. A continuous TiAl{sub 3} intermetallic layer was formed at the Al/Ti interface even after a processing time as short as about a minute. The TiAl{sub 3} layer grew mainly into the Ti part, while only a few individual grains grew into the Al part. Evolution of the interlayer was determined by Al diffusion through the (TiAl{sub 3}/TiAl{sub 3}) grain boundary. The activation energy of the process was 140 kJ/mol. The shear strength of the interface in the Al/Ti bi-metal was determined after various heat treatments. The shear strength of the bi-metal was limited by the properties of aluminum, with no effect of interlayer thickness or current mode and pulse pattern of the SPS treatment being detected. - Highlights: • Spark plasma sintering apparatus was used for heat treatment of Al/Ti bi-metals. • Microstructural evolution of Al/Ti interface during SPS treatment was investigated. • A continuous TiAl{sub 3} intermetallic layer was formed at the Al/Ti interface. • The bi-metal shear strength was limited by the properties of pure aluminum. • No effect of TiAl{sub 3} thickness or SPS current mode and pulse pattern was detected.

Composites of amorphous and nanocrystalline Zr–Cu–Al–Nb bulk materials synthesized by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Drescher, P., E-mail: philipp.drescher@uni-rostock.de [Fluidic Technology and Microfluidics, Faculty of Mechanical Engineering and Marine Technology, University of Rostock, 18059 Rostock (Germany); Witte, K. [Physics of New Materials, Institute of Physics, University of Rostock, 18051 Rostock (Germany); Yang, B. [Polymer Physics, Institute of Physics, University of Rostock, 18051 Rostock (Germany); Steuer, R.; Kessler, O. [Chair of Materials Science, Faculty of Mechanical Engineering and Marine Technology, University of Rostock, 18059 Rostock (Germany); Burkel, E. [Physics of New Materials, Institute of Physics, University of Rostock, 18051 Rostock (Germany); Schick, C. [Polymer Physics, Institute of Physics, University of Rostock, 18051 Rostock (Germany); Seitz, H. [Fluidic Technology and Microfluidics, Faculty of Mechanical Engineering and Marine Technology, University of Rostock, 18059 Rostock (Germany)

2016-05-15

The fabrication of Zr{sub 70}Cu{sub 24}Al{sub 4}Nb{sub 2} bulk metallic glass composite samples by spark plasma sintering (SPS) process has been successfully realized. The unique characteristics of bulk metallic glasses could lead to the possibility of future applications as new structural and functional materials. The densification of an amorphous Zr{sub 70}Cu{sub 24}Al{sub 4}Nb{sub 2} powder was realized in a systematic study changing the sintering temperature in the SPS process leading to stable composites characteristic of amorphous and nanocrystalline structures. X-ray diffractometry (XRD) and differential scanning calorimetry (DSC) analysis, transmission electron microscopy (TEM) as well as hardness tests were applied to determine the structural and mechanical properties of the sintered materials. A stable amorphous bulk metallic glass based on Zr{sub 70}Cu{sub 24}Al{sub 4}Nb{sub 2} with a low fraction of crystallites could be fabricated applying a nominal sintering temperature of 400 °C. Higher sintering temperatures lead to composites with high fractions of nanocrystalline material with porosities below 0.5%.

A Modified Porous Titanium Sheet Prepared by Plasma-Activated Sintering for Biomedical Applications

Directory of Open Access Journals (Sweden)

Yukimichi Tamaki

2010-01-01

Full Text Available This study aimed to develop a contamination-free porous titanium scaffold by a plasma-activated sintering within an originally developed TiN-coated graphite mold. The surface of porous titanium sheet with or without a coated graphite mold was characterized. The cell adhesion property of porous titanium sheet was also evaluated in this study. The peak of TiC was detected on the titanium sheet processed with the graphite mold without a TiN coating. Since the titanium fiber elements were directly in contact with the carbon graphite mold during processing, surface contamination was unavoidable event in this condition. The TiC peak was not detectable on the titanium sheet processed within the TiN-coated carbon graphite mold. This modified plasma-activated sintering with the TiN-coated graphite mold would be useful to fabricate a contamination-free titanium sheet. The number of adherent cells on the modified titanium sheet was greater than that of the bare titanium plate. Stress fiber formation and the extension of the cells were observed on the titanium sheets. This modified titanium sheet is expected to be a new tissue engineering material in orthopedic bone repair.

Characterization of plasma nitrided layers produced on sintered iron

Directory of Open Access Journals (Sweden)

Marcos Alves Fontes

2014-07-01

Full Text Available Plasma nitriding is a thermo-physical-chemical treatment process, which promotes surface hardening, caused by interstitial diffusion of atomic nitrogen into metallic alloys. In this work, this process was employed in the surface modification of a sintered ferrous alloy. Scanning electron microscopy (SEM, X-ray diffraction (XRD analyses, and wear and microhardness tests were performed on the samples submitted to ferrox treatment and plasma nitriding carried out under different conditions of time and temperature. The results showed that the nitride layer thickness is higher for all nitrided samples than for ferrox treated samples, and this layer thickness increases with nitriding time and temperature, and temperature is a more significant variable. The XRD analysis showed that the nitrided layer, for all samples, near the surface consists in a mixture of γ′-Fe4N and ɛ-Fe3N phases. Both wear resistance and microhardness increase with nitriding time and temperature, and temperature influences both the characteristics the most.

Lanthana-bearing nanostructured ferritic steels via spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Pasebani, Somayeh [Department of Chemical and Materials Engineering, University of Idaho, Moscow, ID 83844 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States); Charit, Indrajit, E-mail: icharit@uidaho.edu [Department of Chemical and Materials Engineering, University of Idaho, Moscow, ID 83844 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States); Wu, Yaqiao; Burns, Jatuporn; Allahar, Kerry N.; Butt, Darryl P. [Department of Materials Science and Engineering, Boise State University, Boise, ID 83725 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States); Cole, James I. [Idaho National Laboratory, Idaho Falls, ID 83401 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States); Alsagabi, Sultan F. [Department of Chemical and Materials Engineering, University of Idaho, Moscow, ID 83844 (United States); Center for Advanced Energy Studies, Idaho Falls, ID 83401 (United States)

2016-03-15

A lanthana-containing nanostructured ferritic steel (NFS) was processed via mechanical alloying (MA) of Fe-14Cr-1Ti-0.3Mo-0.5La{sub 2}O{sub 3} (wt.%) and consolidated via spark plasma sintering (SPS). In order to study the consolidation behavior via SPS, sintering temperature and dwell time were correlated with microstructure, density, microhardness and shear yield strength of the sintered specimens. A bimodal grain size distribution including both micron-sized and nano-sized grains was observed in the microstructure of specimens sintered at 850, 950 and1050 °C for 45 min. Significant densification occurred at temperatures greater than 950 °C with a relative density higher than 98%. A variety of nanoparticles, some enriched in Fe and Cr oxides and copious nanoparticles smaller than 10 nm with faceted morphology and enriched in La and Ti oxides were observed. After SPS at 950 °C, the number density of Cr–Ti–La–O-enriched nanoclusters with an average radius of 1.5 nm was estimated to be 1.2 × 10{sup 24} m{sup −3}. The La + Ti:O ratio was close to 1 after SPS at 950 and 1050 °C; however, the number density of nanoclusters decreased at 1050 °C. With SPS above 950 °C, the density improved but the microhardness and shear yield strength decreased due to partial coarsening of the grains and nanoparticles.

Ferritic oxide dispersion strengthened alloys by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Allahar, Kerry N., E-mail: KerryAllahar@boisestate.edu [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Burns, Jatuporn [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Jaques, Brian [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Wu, Y.Q. [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Charit, Indrajit [Department of Chemical and Materials Engineering, University of Idaho, McClure Hall Room 405D, Moscow, ID 83844 (United States); Cole, James [Idaho National Laboratory, Idaho Falls, ID 83401 (United States); Butt, Darryl P. [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States)

2013-11-15

Spark plasma sintering (SPS) was used to consolidate a Fe–16Cr–3Al (wt.%) powder that was mechanically alloyed with Y{sub 2}O{sub 3} and Ti powders to produce 0.5 Y{sub 2}O{sub 3} and 0.5 Y{sub 2}O{sub 3}–1Ti powders. The effects of mechanical alloying and sintering conditions on the microstructure, relative density and hardness of the sintered oxide dispersion strengthened (ODS) alloys are presented. Scanning electron microscopy indicated a mixed fine-grain and coarse-grain microstructure that was attributed to recrystallization and grain growth during sintering. Analysis of the transmission electron microscopy (TEM) and atom probe tomography (APT) data identified Y–O and Y–O–Ti nanoclusters. Elemental ratios of these nanoclusters were consistent with that observed in hot-extruded ODS alloys. The influence of Ti was to refine the grains as well as the nanoclusters with there being greater number density and smaller sizes of the Y–O–Ti nanoclusters as compared to the Y–O nanoclusters. This resulted in the Ti-containing samples being harder than the Ti-free alloys. The hardness of the alloys with the Y–O–Ti nanoclusters was insensitive to sintering time while smaller hardness values were associated with longer sintering times for the alloys with the Y–O nanoclusters. Pressures greater than 80 MPa are recommended for improved densification as higher sintering temperatures and longer sintering times at 80 MPa did not improve the relative density beyond 97.5%.

Matrix Structure Evolution and Nanoreinforcement Distribution in Mechanically Milled and Spark Plasma Sintered Al-SiC Nanocomposites.

Science.gov (United States)

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.

Properties of sintered glass-ceramics prepared from plasma vitrified air pollution control residues

Energy Technology Data Exchange (ETDEWEB)

Roether, J.A.; Daniel, D.J. [Department of Materials, Imperial College London, London SW7 2AZ (United Kingdom); Amutha Rani, D. [Department of Materials, Imperial College London, London SW7 2AZ (United Kingdom); Department of Civil and Environmental Engineering, Imperial College London, London SW7 2AZ (United Kingdom); Deegan, D.E. [Tetronics Ltd., Swindon, Wiltshire SN3 4DE (United Kingdom); Cheeseman, C.R., E-mail: c.cheeseman@imperial.ac.uk [Department of Civil and Environmental Engineering, Imperial College London, London SW7 2AZ (United Kingdom); Boccaccini, A.R., E-mail: a.boccaccini@imperial.ac.uk [Department of Materials, Imperial College London, London SW7 2AZ (United Kingdom)

2010-01-15

Air pollution control (APC) residues, obtained from a major UK energy from waste (EfW) plant, processing municipal solid waste, have been blended with silica and alumina and melted using DC plasma arc technology. The glass produced was crushed, milled, uni-axially pressed and sintered at temperatures between 750 and 1150 deg. C, and the glass-ceramics formed were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Mechanical properties assessed included Vickers's hardness, flexural strength, Young's modulus and thermal shock resistance. The optimum sintering temperature was found to be 950 deg. C. This produced a glass-ceramic with high density ({approx}2.58 g/cm{sup 3}), minimum water absorption ({approx}2%) and relatively high mechanical strength ({approx}81 {+-} 4 MPa). Thermal shock testing showed that 950 deg. C sintered samples could withstand a 700 deg. C quench in water without micro-cracking. The research demonstrates that glass-ceramics can be readily formed from DC plasma treated APC residues and that these have comparable properties to marble and porcelain. This novel approach represents a technically and commercially viable treatment option for APC residues that allow the beneficial reuse of this problematic waste.

Two-dimensional simulation of sintering process

International Nuclear Information System (INIS)

Vasconcelos, Vanderley de; Pinto, Lucio Carlos Martins; Vasconcelos, Wander L.

1996-01-01

The results of two-dimensional simulations are directly applied to systems in which one of the dimensions is much smaller than the others, and to sections of three dimensional models. Moreover, these simulations are the first step of the analysis of more complex three-dimensional systems. In this work, two basic features of the sintering process are studied: the types of particle size distributions related to the powder production processes and the evolution of geometric parameters of the resultant microstructures during the solid-state sintering. Random packing of equal spheres is considered in the sintering simulation. The packing algorithm does not take into account the interactive forces between the particles. The used sintering algorithm causes the densification of the particle set. (author)

Development of a TiAl Alloy by Spark Plasma Sintering

Science.gov (United States)

Couret, Alain; Voisin, Thomas; Thomas, Marc; Monchoux, Jean-Philippe

2017-12-01

Spark plasma sintering (SPS) is a consolidated powder metallurgy process for which the powder sintering is achieved through an applied electric current. The present article aims to describe the method we employed to develop a TiAl-based alloy adjusted for this SPS process. Owing to its enhanced mechanical properties, this alloy was found to fully match the industrial specifications for the aeronautic and automotive industries, which require a high strength at high temperature and a reasonably good ductility at room temperature. A step-by-step method was followed for this alloy development. Starting from a basic study on the as-SPSed GE alloy (Ti-48Al-2Cr-2Nb) in which the influence of the microstructure was studied, the microstructure-alloy composition relationships were then investigated to increase the mechanical properties. As a result of this study, we concluded that tungsten had to be the major alloying element to improve the resistance at high temperature and a careful addition of boron would serve the properties at room temperature. Thus, we developed the IRIS alloy (Ti-48Al-2W-0.08B). Its microstructure and mechanical properties are described here.

Preparation and soft magnetic properties of spark plasma sintered compacts based on Fe–Si–B glassy powder

Energy Technology Data Exchange (ETDEWEB)

Neamţu, B.V., E-mail: bogdan.neamtu@stm.utcluj.ro [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 400614 Cluj-Napoca (Romania); Marinca, T.F.; Chicinaş, I. [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 400614 Cluj-Napoca (Romania); Isnard, O. [Institut Néel, CNRS/University Joseph Fourier, BP 166, 38042 Grenoble Cédex 9 (France); Popa, F. [Materials Science and Engineering Department, Technical University of Cluj-Napoca, 400614 Cluj-Napoca (Romania); Păşcuţă, P. [Physics and Chemistry Department Technical University of Cluj-Napoca, 400614 Cluj-Napoca (Romania)

2014-07-05

Highlights: • Amorphous powder of Fe{sub 75}Si{sub 20}B{sub 5} (at.%) was prepared by wet mechanical alloying. • Spark plasma sintering was used for compaction of amorphous Fe{sub 75}Si{sub 20}B{sub 5} powder. • Increasing SPS time/temperature leads to improvement of AC/DC compacts properties. - Abstract: Amorphous powder of Fe{sub 75}Si{sub 20}B{sub 5} (at.%) was prepared by wet mechanical alloying route using benzene as surfactant. The amorphous phase is obtained after 60 h of milling. Structural, morphological, and thermal characteristics were investigated. The as-milled powder consists in micrometric particles with a mean diameter of 10.4 μm which are formed by the agglomeration of smaller particles. The amorphous powder is thermally stable up to the temperature of 490 °C. Spark plasma sintered compacts were prepared from the amorphous powders at sintering temperatures of 800, 850 and 900 °C. The phases formation and their evolution was investigated by X-ray diffraction technique showing that Fe{sub 3}Si and Fe{sub 2}B are the main phases formed during the spark plasma sintering process. Fe{sub 75}Si{sub 20}B{sub 5} (at.%) samples in the form of a ring were investigated in DC and AC magnetization regime. It was found that the boride phase formation (during sintering) and the low density of the compacts affect the magnetic properties of the compacts. In addition, a superficial contamination of the compacts with carbon (a layer of 2–3 μm) was evidenced, contributing thus to their soft magnetic deterioration. Increasing of the saturation induction, maximum relative permeability and initial relative permeability was observed by increasing both sintering temperature and time. It was generally observed that the compacts with high density have higher total core losses at high frequency.

Microstructure and property evolution of isotropic and anisotropic NdFeB magnets fabricated from nanocrystalline ribbons by spark plasma sintering and hot deformation

Energy Technology Data Exchange (ETDEWEB)

Liu, Z W; Huang, H Y; Yu, H Y; Zhong, X C; Zeng, D C [School of Materials Science and Engineering, South China University of Technology, Guangzhou 510640 (China); Gao, X X; Zhu, J, E-mail: zwliu@scut.edu.cn [State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083 (China)

2011-01-19

Isotropic and anisotropic NdFeB magnets were synthesized by spark plasma sintering (SPS) and SPS+HD (hot deformation), respectively, using melt-spun ribbons as the starting materials. Spark plasma sintered magnets sintered at low temperatures (<700 {sup 0}C) almost maintained the uniform fine grain structure inherited from rapid quenching. At higher temperatures, due to the local high-temperature field caused by the spark plasma discharge, the grain growth occurred at the initial particle surfaces and the coarse grain zones formed in the vicinity of the particle boundaries. Since the interior of the particles maintained the fine grain structure, a distinct two-zone structure was formed in the spark plasma sintered magnets. The SPS temperature and pressure have important effects on the widths of coarse and fine grain zones, as well as the grain sizes in two zones. The changes in grain structure led to variations in the magnetic properties. By employing low SPS temperature and high pressure, high-density magnets with negligible coarse grain zone and an excellent combination of magnetic properties can be obtained. An anisotropic magnet with a maximum energy product of {approx}30 MG Oe was produced by the SPS+HD process. HD at 750 {sup 0}C did not lead to obvious grain growth and the two-zone structure still existed in the hot deformed magnets. Intergranular exchange coupling was demonstrated in the spark plasma sintered magnets and was enhanced by the HD process, which reduced the coercivity. Good temperature stability was manifested by low temperature coefficients of remanence and coercivity. The results indicated that nanocrystalline NdFeB magnets without significant grain growth and with excellent properties could be obtained by SPS and HD processes.

Mechanochemical synthesis and spark plasma sintering of the cerium silicides

Energy Technology Data Exchange (ETDEWEB)

Alanko, Gordon A.; Jaques, Brian; Bateman, Allyssa [Department of Materials Science and Engineering, College of Engineering, Boise State University, 1910 University Drive, Boise, ID 83725 (United States); Butt, Darryl P., E-mail: darrylbutt@boisestate.edu [Department of Materials Science and Engineering, College of Engineering, Boise State University, 1910 University Drive, Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Boulevard, Idaho Falls, ID 83401 (United States)

2014-12-15

Highlights: • Ce{sub 5}Si{sub 3}, Ce{sub 3}Si{sub 2}, CeSi, CeSi{sub 2−x} and CeSi{sub 2} were mechanochemically synthesized. • Temperature and pressure were monitored to investigate reaction progress. • All syntheses proceeded through a MSR event followed by rapid solid-state diffusion. • Milling time before MSR correlates well with effective heat of formation. • Some synthesized material was densified by spark plasma sintering. - Abstract: The cerium silicides, Ce{sub 5}Si{sub 3}, Ce{sub 3}Si{sub 2}, CeSi, CeSi{sub 2−y}, and CeSi{sub 2−x}, have been prepared from the elements by mechanochemical processing in a planetary ball mill. Preparation of the cerium silicide Ce{sub 5}Si{sub 4} was unsuccessfully attempted and potential reasons for this are discussed. Temperature and pressure of the milling vial were monitored in situ to gain insight into the mechanochemical reaction kinetics, which include a mechanically-induced self-propagating reaction (MSR). Some prepared powders were consolidated by spark plasma sintering to high density. Starting materials, as-milled powders, and consolidated samples were characterized by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy. The results obtained help elucidate key questions in mechanochemical processing of intermetallics, showing first phase formation similar to thin films, MSR ignition times that are composition- and milling speed-dependent, and sensitivity of stable compound formation on the impact pressure. The results demonstrate mechanochemical synthesis as a viable technique for rare earth silicides.

New materials through a variety of sintering methods

Science.gov (United States)

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.

Study of effective utilization of iron ore sinter through arc plasma

Science.gov (United States)

Swain, Biswajit; Samal, S. K.; Mohanty, M. K.; Behera, A.; Mishra, S. C.

2018-03-01

Generation of fines is common in mining, sizing, and beneficiation and also in high-temperature metallurgical processes as the disintegration of agglomerate/compact occurs. Extraction of metallic iron from ore fines is one of the challenging aspects of iron making industries as the liberation of fines blocks, the charge burden porosity and hence hinders the reduction rate. Along with size factor, mineral composition plays a vital role in the extraction process; particularly silica. As silica has the very high tendency towards iron oxide, at comparatively low temperature, the activity of silica should be suppressed to prevent silicate phases. Adjustment of such conditions is controlled by addition of lime, but sometimes excessive slag generation increases the cost of production. In the present work, carbothermic reduction of partially reduced iron bearing pellets has been melted through 20 KW DC arc plasma furnace, and a comparative study has been made for considering different slag chemistry approaches. Pellets as aforementioned are made available from Patnaik Steel and Alloys Ltd, Odisha, having high silica content ore fines (of about 8.6%) as obtained from the chemical analysis. X-Ray analysis and optical image analyzer result of sinter thus obtained reveal that fayalite phase has major fractional value. Smelting works were done for sinter with/without adjustment of slag chemistry, where argon and nitrogen were used as plasma forming gases. A range of recovery rates (between 87-94%) is achieved by charge composition, ionizing gases, and smelting duration. It is observed that use of nitrogen as plasma forming gas increases the recovery rate than that of using only argon plasma; due to high energy flux of nitrogen which increases the enthalpy due to its diatomicity. A maximum recovery rate of about 94% is achieved for process duration of 13minutes utilizing nitrogen plasma. Smelting of charge with the addition of hydrated lime targeting melilite as final slag

A finite difference model of the iron ore sinter process

OpenAIRE

Muller, J.; de Vries, T.L.; Dippenaar, B.A.; Vreugdenburg, J.C.

2015-01-01

Iron ore fines are agglomerated to produce sinter, which is an important feed material for blast furnaces worldwide. A model of the iron ore sintering process has been developed with the objective of being representative of the sinter pot test, the standard laboratory process in which the behaviour of specific sinter feed mixtures is evaluated. The model aims to predict sinter quality, including chemical quality and physical strength, as well as key sinter process performance parameters such ...

Spark plasma sintering of titanium aluminide intermetallics and its composites

Science.gov (United States)

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.

Full densification of inkjet-printed copper conductive tracks on a flexible substrate utilizing a hydrogen plasma sintering

Science.gov (United States)

Kwon, Young-Tae; Lee, Young-In; Kim, Seil; Lee, Kun-Jae; Choa, Yong-Ho

2017-02-01

Low temperature sintering techniques are crucial in developing flexible printed electronics. In this work, we demonstrate a novel hydrogen plasma sintering method that achieves a full reduction and densification of inkjet-printed patterns using a copper complex ion ink. After inkjet printing on polyethylene terephthalate (PET) substrates, both hydrogen plasma and conventional hydrogen thermal treatment were employed to compare the resulting microstructures, electrical properties and anti-oxidation behavior. The plasma treated pattern shows a fully densified microstructure with a resistivity of 3.23 μΩ cm, while the thermally treated pattern shows a relatively poor microstructure and high resistivity. In addition, the hydrogen plasma-treated copper pattern retains its electrical resistivity for one month without any significant decrease. This novel hydrogen plasma sintering technique could be used to produce conductive patterns with excellent electrical properties, allowing for highly reliable flexible printed electronics.

Design of experiment approach for sintering study of nanocrystalline SiC fabricated using plasma pressure compaction

Directory of Open Access Journals (Sweden)

Bothara M.G.

2009-01-01

Full Text Available Plasma pressure compaction (P2C is a novel sintering technique that enables the consolidation of silicon carbide with a nanoscale microstructure at a relatively low temperature. To achieve a high final density with optimized mechanical properties, the effects of various sintering factors pertaining to the temperature-time profile and pressure were characterized. This paper reports a design of experiment approach used to optimize the processing for a 100 nm SiC powder focused on four sintering factors: temperature, time, pressure, and heating rate. Response variables included the density and mechanical properties. A L9 orthogonal array approach that includes the signal-to-noise (S/N ratio and analysis of variance (ANOVA was employed to optimize the processing factors. All of the sintering factors have significant effect on the density and mechanical properties. A final density of 98.1% was achieved with a temperature of 1600°C, hold time of 30 min, pressure of 50 MPa, and heating rate of 100°C/min. The hardness reached 18.4 GPa with a fracture toughness of 4.6 MPa√m, and these are comparable to reports from prior studies using higher consolidation temperatures.

COMPACTION OF LITHIUM-SILICATE CERAMICS USING SPARK PLASMA SINTERING

Directory of Open Access Journals (Sweden)

Tomas Frantisek Kubatik

2016-12-01

Full Text Available This paper deals with the compaction of ceramics based on lithium-silicate by spark plasma sintering (SPS. The initial powder was prepared by calcination in a resistance furnace at a temperature of 1300 °C with the ratio of Li/Si = 1. Compacting by SPS was carried out at temperatures of 800 - 1000 °C with a maximum pressure of 80 MPa. Samples with open porosity of less than 1 % were prepared at the temperature of 1000 °C. According to the quantitative Rietveld refinement of x-ray diffraction data, the dominant phases in all samples were Li₂Si₂O₅ and Li₂SiO₃, together representing over 80 wt. % of the sintered material.

Uranium migration in spark plasma sintered W/UO2 CERMETS

Science.gov (United States)

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

2018-03-01

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

Spark Plasma Sintering and Densification Mechanisms of Antimony-Doped Tin Oxide Nanoceramics

Directory of Open Access Journals (Sweden)

Junyan Wu

2013-01-01

Full Text Available Densification of antimony-doped tin oxide (ATO ceramics without sintering aids is very difficult, due to the volatilization of SnO2, formation of deleterious phases above 1000°C, and poor sintering ability of ATO particles. In this paper, monodispersed ATO nanoparticles were synthesized via sol-gel method, and then ATO nanoceramics with high density were prepared by spark plasma sintering (SPS technology using the as-synthesized ATO nanoparticles without the addition of sintering aids. The effect of Sb doping content on the densification was investigated, and the densification mechanisms were explored. The results suggest that ATO nanoparticles derived from sol-gel method show good crystallinity with a crystal size of 5–20 nm and Sb is incorporated into the SnO2 crystal structure. When the SPS sintering temperature is 1000°C and the Sb doping content is 5 at.%, the density of ATO nanoceramics reaches a maximum value of 99.2%. Densification mechanisms are explored in detail.

Preparing Magnetocaloric LaFeSi Uniform Microstructures by Spark Plasma Sintering

DEFF Research Database (Denmark)

Vicente, N.; Ocanã, J.; Neves Bez, Henrique

2014-01-01

Spark Plasma Sintering (SPS) of LaFeSi alloy powders was conducted to prepare magnetocaloric La-Fe-Si-based uniform microstructures. Two electrically insulating discs made of alumina were interposed between the punches and powder sample inhibiting the flow of electric current across the powder...... from hydrogenated and decrypted casting ingot. The characterizations of sintered samples were performed by Scanning Electron Microscopy (SEM), Archimedes principle, Vicker’s hardness and microhardness. The uniformity of the microstructure was evaluated by checking the evidence of position on the Vicker...

Mechanical characterization of cemented carbide WC-6Co (%wt) manufactured by SPS (Spark Plasma Sintering; Caracterizacao mecanica de metal duro WC-6Co (%massa) sinterizado via SPS (Spark Plasma Sintering)

Energy Technology Data Exchange (ETDEWEB)

Boidi, G.; Tertuliano, A.J.; Machado, I.F., E-mail: guido.boidi@usp.br [Universidade de Sao Paulo (USP), SP (Brazil). Departamento de Engenharia Mecatronica e Sistemas Mecanicos; Rodrigues, D. [BRATS- Filtros Sinterizados e Pos Metalicos, Cajamar, SP (Brazil)

2016-07-01

This work aimed to manufacture cemented carbide (WC-6%wtCo) obtained by SPS (Spark Plasma Sintering) process and to carry out the mechanical characterization by hardness and fracture toughness. The material was consolidated at 1100 deg C for different holding times (1 min, 5 min, 10 min), in order to evaluate the densification. A reference sample was also used to be compared to SPS. Optical and scanning electron microscopy were carried out to characterize the microstructural features of the samples and mechanical properties were obtained by hardness measurements (micro and macro) and instrumented indentation. The fracture toughness was calculated with the method of Palmqvist. Best results were found in the material sintered by SPS for 10 minutes of holding time, in which 97% of relative density and about 1600 HV{sub 10} was reached. (author)

Post-treatment of Plasma-Sprayed Amorphous Ceramic Coatings by Spark Plasma Sintering

Science.gov (United States)

Chraska, T.; Pala, Z.; Mušálek, R.; Medřický, J.; Vilémová, M.

2015-04-01

Alumina-zirconia ceramic material has been plasma sprayed using a water-stabilized plasma torch to produce free standing coatings. The as-sprayed coatings have very low porosity and are mostly amorphous. The amorphous material crystallizes at temperatures above 900 °C. A spark plasma sintering apparatus has been used to heat the as-sprayed samples to temperatures above 900 °C to induce crystallization, while at the same time, a uniaxial pressure of 80 MPa has been applied to their surface. After such post-treatment, the ceramic samples are crystalline and have very low open porosity. The post-treated material exhibits high hardness and significantly increased flexural strength. The post-treated samples have a microstructure that is best described as nanocomposite with the very small crystallites embedded in an amorphous matrix.

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

Science.gov (United States)

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.

Flash sintering of ceramic materials

Science.gov (United States)

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.

Real-time operation guide system for sintering process with artificial intelligence

Institute of Scientific and Technical Information of China (English)

FAN Xiao-hui; CHEN Xu-ling; JIANG Tao; LI Tao

2005-01-01

In order to optimize the sintering process, a real-time operation guide system with artificial intelligence was developed, mainly including the data acquisition online subsystem, the sinter chemical composition controller, the sintering process state controller, and the abnormal conditions diagnosis subsystem. Knowledge base of the sintering process controlling was constructed, and inference engine of the system was established. Sinter chemical compositions were controlled by the strategies of self-adaptive prediction, internal optimization and center on basicity. And the state of sintering was stabilized centering on permeability. In order to meet the needs of process change and make the system clear, the system has learning ability and explanation function. The software of the system was developed in Visual C++ programming language. The application of the system shows that the hitting accuracy of sinter compositions and burning through point prediction are more than 85%; the first-grade rate of sinter chemical composition, stability rate of burning through point and stability rate of sintering process are increased by 3%, 9% and 4%, respectively.

W/Cu composites produced by low temperature Pulse Plasma Sintering

International Nuclear Information System (INIS)

Rosinski, M.S.; Fortuna, E.; Michalski, A.J.; Kurzydlowski, K.J.

2006-01-01

The plasma facing components (PFCs) must withstand the thermal, mechanical and neutron loads under cyclic mode of operation and vacuum. Despite that PFCs of ITER and demonstration reactors must assure reliability and long in service lifetime. For that reason PFCs are designed to be made of beryllium, tungsten or carbon fibre composites armours and copper based heat sink material. Such design concepts can only be used if joining methods of these dissimilar materials are resolved. Several techniques have been developed for joining W and Cu e. g. casting of pure Cu onto W, high temperature brazing, direct diffusion bonding or CVDs of W onto Cu. The main problem in the development of such joints is the large difference in the coefficients of thermal expansion, CTE (alpha Cu > 4 alpha W) and elastic modula (ECu > 0.2 EW). These differences result in large stresses at the W/Cu interfaces during manufacturing and/or during operation, which may lead to cracking or delamination reducing lifetime of the components. Possible solution to this problem is the use of W-Cu composites (FGM). W-Cu composites are widely used for spark erosion electrodes, in heavy duty circuit breakers and as heat sinks of microelectronic devices. They are commonly produced by infiltration of a porous sintered tungsten by liquid copper. Other technological route is powder metallurgy. Coatings can be produced by low pressure plasma spraying. All these methods, however, are known to have some disadvantages. For infiltration there is a 30 wt.% limit of Cu content while for powder metallurgy and plasma spraying techniques porosity is of concern. In our work the W-Cu composites of different composition were produced by pulse plasma sintering (PPS). This new method utilizes pulsed high electric discharges to heat the powders under uniaxial load. The arc discharges clean surface of powder particles and intensify diffusion. The total sintering time is reduced to several minutes. In our investigations various

Spark plasma sintering of tungsten-yttrium oxide composites from chemically synthesized nanopowders and microstructural characterization

International Nuclear Information System (INIS)

Yar, M.A.; Wahlberg, Sverker; Bergqvist, Hans; Salem, H.G.; Johnsson, Mats; Muhammed, Mamoun

2011-01-01

Nano-crystalline W-1%Y 2 O 3 (wt.%) powder was produced by a modified solution chemical reaction of ammonium paratungstate (APT) and yttrium nitrate. The precursor powder was found to consist of particles of bimodal morphology i.e. large APT-like particles up to 20 μm and rectangular yttrium containing ultrafine plates. After thermal processing tungsten crystals were evolved from W-O-Y plate like particles. spark plasma sintering (SPS) was used to consolidate the powder at 1100 and 1200 deg. C for different holding times in order to optimize the sintering conditions to yield high density but with reduced grain growth. Dispersion of yttrium oxide enhanced the sinterability of W powder with respect to lanthanum oxide. W-1%Y 2 O 3 composites with sub-micron grain size showed improved density and mechanical properties as compared to W-La 2 O 3 composites. Sample sintered in two steps showed improved density, due to longer holding time at lower temperature (900 deg. C) and less grain growth due to shorter holding time at higher temperature i.e. 1 min at 1100 deg. C.

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

Directory of Open Access Journals (Sweden)

Guy-Daniel Dutel

2017-04-01

Full Text Available 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.

The influence of green microstructure and sintering parameters on precipitation process during copper-nickel-zinc ferrites sintering

International Nuclear Information System (INIS)

Barba, A.; Clausell, C.; Jarque, J. C.; Monzo, M.

2014-01-01

Microstructural changes that occur during heat treatment of copper-nickel-zinc ferrites have been studied. The process of precipitation of the two types of crystals that occur during the sintering process has been analyzed. It is found that this process depends on dry relative density of the press specimens and on the following sintering parameters: sintering temperature, sintering time and cooling rate of the thermal cycle. Crystal precipitates characterization have been done by scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) analysis, X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). These techniques have allowed to determine the nature of these crystals, which in this case correspond to zinc and copper oxides. It has been used two chemical reactions to explain the bulk precipitation and subsequent re-dissolution of these crystal precipitates during sintering. (Author)

Spark plasma sintering of TiNi nano-powders for biological application

International Nuclear Information System (INIS)

Fu, Y Q; Gu, Y W; Shearwood, C; Luo, J K; Flewitt, A J; Milne, W I

2006-01-01

Nano-sized TiNi powder with an average size of 50 nm was consolidated using spark plasma sintering (SPS) at 800 deg. C for 5 min. A layer of anatase TiO 2 coating was formed on the sintered TiNi by chemical reaction with a hydrogen peroxide (H 2 O 2 ) solution at 60 deg. C followed by heat treatment at 400 deg. C to enhance the bioactivity of the metal surface. Cell culture using osteoblast cells and a biomimetic test in simulated body fluid proved the biocompatibility of the chemically treated SPS TiNi

Argon plasma sintering of inkjet printed silver tracks on polymer substrates

NARCIS (Netherlands)

Reinhold, I.; Hendriks, C.E.; Eckardt, R.; Kranenburg, J.M.; Perelaer, J.; Baumann, R.; Schubert, U.S.

2009-01-01

An alternative and selective sintering method for the fabrication of conductive silver tracks on common polymer substrates is presented, by exposure to low-pressure argon plasma. Inkjet printing has been used to pattern a silver nanoparticle ink. This resulted in conductive features with a

Techniques for ceramic sintering using microwave energy

International Nuclear Information System (INIS)

Kimrey, H.D.; Janney, M.A.; Becher, P.F.

1987-01-01

The use of microwave energy for ceramic sintering offers exciting new possibilities for materials processing. Based on experience gathered in microwave processing associated with the heating of fusion plasmas, we have developed hardware and methods for uniformly heating ceramic parts of large volume and irregular shape to temperatures in excess of 1600 0 C, in vacuum or pressurized atmosphere. Microwave processing at 28 GHz yields enhanced densification rates with a corresponding reduction in sintering temperatures. 6 refs

Removable partial denture alloys processed by laser-sintering technique.

Science.gov (United States)

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 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.

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

International Nuclear Information System (INIS)

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

2014-01-01

Graphical abstract: Densification of HfO 2 –Y 2 O 3 micro-beads by Spark Plasma Sintering High density pellets with homogenous distribution of Hf and Y serve as neutron absorbers. - Abstract: Dense yttrium–stabilised hafnia pellets (91.35 wt.% HfO 2 and 8.65 wt.% Y 2 O 3 ) were prepared by spark plasma sintering consolidation of micro-beads synthesised by the “external gelation” sol–gel technique. This technique allows a preparation of HfO 2 –Y 2 O 3 beads with homogenous yttria–hafnia solid solution. A sintering time of 5 min at 1600 °C was sufficient to produce high density pellets (over 90% of the theoretical density) with significant reproducibility. The pellets have been machined in a lathe to the correct dimensions for use as neutron absorbers in an experimental test irradiation in the High Flux Reactor (HFR) in Petten, Holland, in order to investigate the safety of americium based nuclear fuels

Powder-metallurgy preparation of NiTi shape-memory alloy using mechanical alloying and spark-plasma sintering.

Czech Academy of Sciences Publication Activity Database

Novák, P.; Moravec, H.; Vojtěch, V.; Knaislová, A.; Školáková, A.; Kubatík, Tomáš František; Kopeček, Jaromír

2017-01-01

Roč. 51, č. 1 (2017), s. 141-144 ISSN 1580-2949 R&D Projects: GA ČR(CZ) GA14-03044S Institutional support: RVO:61389021 ; RVO:68378271 Keywords : mechanical alloying * spark plasma sintering * NiTi * shape memory alloy Subject RIV: JG - Metallurgy; JG - Metallurgy (FZU-D) OBOR OECD: Materials engineering ; Materials engineering (FZU-D) Impact factor: 0.436, year: 2016 https://www.researchgate.net/publication/313900224_Powder-metallurgy_preparation_of_NiTi_shape-memory_alloy_using_mechanical_alloying_and_spark-plasma_sintering

Heterojunction p-Cu2O/ZnO-n solar cell fabricated by spark plasma sintering

Directory of Open Access Journals (Sweden)

Christophe Tenailleau

2017-09-01

Full Text Available Abstract Cuprous oxide and zinc oxide nanoparticles were prepared at room temperature by inorganic polycondensation. X-ray diffraction (XRD analyses show that the oxide phases formed are pure and well crystallized. The spark plasma sintering (SPS technique was successfully used to prepare dense nanoceramics with superimposed layers of Cu2O and ZnO nanopowders. Sintering conditions were optimized to densify the ceramics without phase transformation or diffusion. These ceramics were also characterized by XRD and scanning electron microscopy (SEM, as well as X-ray computed tomography (XCT. SEM and XCT showed that nanograins are preserved after SPS throughout both oxide materials, while a smaller layer (~20 µm of pure oxide phase with larger grains is formed in between Cu2O and ZnO during the sintering process. The SPS technique results in high material density, with the absence of porosity and cracks, homogenous distribution, and a good phase separation. This is the first time that such as-prepared dense oxide-based heterojunction exhibits a photovoltaic effect under illumination opening a new route for preparing solar cells.

Granulation of coke breeze fine for using in the sintering process

Directory of Open Access Journals (Sweden)

Mohamed F.M.

2010-01-01

Full Text Available Coke breeze is the main fuel used in the sintering process. The value of -3+1 mm. represents the most favorable particle size for coke breeze in the sintering process. About 20% of total coke fines (-0.5 mm are produced during different steps of preparation. Introducing these fines during the sintering process proves to be very harmful for different operating parameters. Thus ,this study aims at investigating the production of granules resulting from these fines using molasses as organic binder and its application in sintering of an iron ore. The results showed that the granules having the highest mechanical properties were obtained with 14.5 wt % molasses addition. The sintering experiments were performed by using coke breeze in different shapes (-3+1 mm in size, coke breeze without sieving and coke breeze granules -3+1 mm. The reduction experiments, microscopic structure and X-ray analysis for the produced sinter were carried out. The results revealed that, all sinter properties (such as shatter test, productivity of sinter machine and blast furnace, reduction time and chemical composition for produced sinter by using coke breeze with size -3+1 mm and coke breeze granules were almost the same. The iron ore sinter which was produced by using coke breeze without sieving yielded low productivity for both sinter machine and blast furnace. Furthermore, using coke breeze without sieving in sintering of an iron ore decreases the vertical velocity of sinter machine and increases the reduction time.

Process parameter influence on Electro-sinter-forging (ESF) of titanium discs

DEFF Research Database (Denmark)

Cannella, Emanuele; Nielsen, Chris Valentin; Bay, Niels

Electro-sinter-forging (ESF) is a sintering process based on the resistance heating principle, which makes it faster than conventional sintering. The process is investigated as a function of the main process parameters, namely compacting pressure, electrical current density and sintering time....... The present work is focused on analysing the influence of these process parameters on the final density of a disc sample made from commercially pure titanium powder. Applying the design of experiments (DoE) approach, the electrical current was seen to be of largest influence. The maximum obtained density...

Identification of microstructural mechanisms during densification of a TiAl alloy by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Jabbar, Houria; Couret, Alain; Durand, Lise [CNRS, CEMES-UPR 8011, Centre d' Elaboration de Materiaux et d' Etudes Structurales, BP 94347, 29 rue J. Marvig, F-31055 Toulouse (France); Universite de Toulouse, UPS, F-31055 Toulouse (France); Monchoux, Jean-Philippe, E-mail: monchoux@cemes.fr [CNRS, CEMES-UPR 8011, Centre d' Elaboration de Materiaux et d' Etudes Structurales, BP 94347, 29 rue J. Marvig, F-31055 Toulouse (France); Universite de Toulouse, UPS, F-31055 Toulouse (France)

2011-10-13

Graphical abstract: Highlights: > Mechanisms of a TiAl alloy powder densified by spark plasma sintering are identified. > Microstructure evolution of the powder is followed during the sintering cycle. > As-atomized supersaturated powder comes back to equilibrium. > Densification occurs by plastification of the particles at high temperature. > No mechanisms related to electric current are observed. - Abstract: This work aims at identifying, by coupled scanning and transmission electron microscopy (SEM and TEM) observations, the densification mechanisms occurring when an atomized Ti-47Al-1W-1Re-0.2Si powder is densified by spark plasma sintering (SPS). For this purpose, interruptions of the SPS cycle have been performed to follow the evolution of the microstructure step by step. The powder particles exhibit a classical dendritic microstructure containing a large amount of out-of-equilibrium {alpha} phase. During heating-up, the microstructure undergoes successive transformations. At T = 525-875 deg. C the {alpha} phase transforms into {gamma}. The {gamma} phase formed is supersaturated in W and Re. It de-saturates for T above 875 deg. C by discontinuous precipitation of W and Re-rich B2 phase. Densification takes place for T between 900 deg. C and 1150 deg. C by plastic deformation of the powder particles. TEM observations show that the repartition of the plastic deformation is correlated to the dendritic microstructure, and that dynamic recrystallization mechanisms occur. Microstructural phenomena directly resulting from the high currents involved in the SPS process have not been observed.

Orientation distribution in Bi2Te3-based compound prepared by spark plasma sintering

International Nuclear Information System (INIS)

Kim, K.T.; Kim, Y.H.; Lim, C.H.; Cho, D.C.; Lee, Y.S.; Lee, C.H.

2005-01-01

P-type Bi 0.5 Sb 1.5 Te 3 compounds doped with 3wt.% Te were fabricated by spark plasma sintering after mixing large powders(P L ) and small powders(P S ). We could obtained the highest figure of merit(Z C ) of 2.89 x 10 -3 /K in sintered compound mixed to P L :P S =80:20. This resulted from the increase of orientation by large powders(P S ) and the reduce of pores by small powders. The figure of merit(Z C ) of the sintered compound using only small powders(P S ) showed lower value of 2.67 x 10 -3 /K compared with that of sintered compound mixed to P L :P S =80:20 due to the increase of electrical resistivity. (orig.)

Synergistic effect of carbon nanotube as sintering aid and toughening agent in spark plasma sintered molybdenum disilicide-hafnium carbide composite

Energy Technology Data Exchange (ETDEWEB)

Mukherjee, Biswajyoti; Asiq Rahman, O.S.; Sribalaji, M [Materials Science and Engineering, Indian Institute of Technology Patna, Bihta Kanpa Road, Bihta, Patna, Bihar 801103 (India); Bakshi, Srinivasa Rao [Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600036 (India); Keshri, Anup Kumar, E-mail: anup@iitp.ac.in [Materials Science and Engineering, Indian Institute of Technology Patna, Bihta Kanpa Road, Bihta, Patna, Bihar 801103 (India)

2016-12-15

Hafnium carbide (HfC) along with sintering aids was consolidated at a relatively lower temperature i.e. 1600 °C (i.e. T=~0.41 T{sub m}) under a uniaxial load of 50 MPa by spark plasma sintering. Two different sintering aids such as molybdenum disilicide (MoSi{sub 2}) and carbon nanotube (CNT) were added to enhance the densification and lower the extent of grain growth in the sintered pellets. Density of the sintered pellet increased from 96.0±0.8% in HfC +5 wt% MoSi{sub 2} (HM) to 99.0±0.5% with the addition of 2 wt% CNT in HfC+5 wt% MoSi{sub 2} (HMC) at sintering temperature of 1600 °C. Further, the extent of grain growth drastically reduced from 204% in HM to 50% in HMC. Analysis of linear shrinkage during densification revealed that CNT addition increased densification rate and decreased the time required to reach the density of 99.0±0.5% at 1600 °C. Increased densification and lower degree of grain growth could be due to the synergistic effect offered by the CNT, which are as follows: (i) Lubrication effect of CNT, (ii) Lower activation energy for grain boundary diffusion (iii) Reduction in liquid phase sintering temperature and (iv) Grain boundary pinning. Fracture toughness of the sintered HM and HMC composite was obtained using indentation technique. By the addition of 2 wt% CNT in HM, drastic increase of 91% in fracture toughness was seen. This significant improvement in fracture toughness was due to the enhanced densification and relatively lower grain size of HMC. Also crack bridging, crack deflection, crack arrest, CNT and graphene sheet pull-out and swording played major role in toughening of HMC pellet.

Spark-plasma sintering and mechanical property of mechanically alloyed NiAl powder compact and ball-milled (Ni+Al) mixed powder compact

International Nuclear Information System (INIS)

Kim, J.S.; Jang, Y.I.; Kwon, Y.S.; Kim, Y.D.; Ahn, I.S.

2001-01-01

Mechanically-alloyed NiAl powder and (Ni+Al) powder mixture prepared by ball-milling were sintered by spark-plasma sintering (SPS) process. Densification behavior and mechanical property were determined from the experimental results and analysis such as changes in linear shrinkage, shrinkage rate, microstructure, and phase during sintering process, Vicker's hardness and transverse rupture strength tests. Densification mechanisms for MA-NiAl powder compact and (Ni+Al) powder mixture were different from each other. While the former showed a rapid increase in densification rate only at higher temperature region of 800-900 o C, the latter revealed firstly a rapid increase in densification rate even at low temperature of 300 o C and a subsequent increase up to 500 o C. Densities of both powder compact (MA and mixture) sintered at 1150 o C for 5 min were 98 and above 99 %, respectively. Sintered bodies were composed mainly of NiAl phase with Ni 3 Al as secondary phase for both powders. Sintered body of MA-NiAl powder showed a very fine grain structure. Crystallite size determined by XRD result and the Sherrer's equation was approximately 80 nm. Vicker's hardness for the sintered bodies of (Ni+Al) powder mixture and MA-NiAl powder were 410±12 H v and 555±10 H v , respectively, whereas TRS values 1097±48 MPa and 1393±75 MPa. (author)

Ceramic-intermetallic composites produced by mechanical alloying and spark plasma sintering

CERN Document Server

Cabanas-Moreno, J G; Martínez-Sanchez, R; Delgado-Gutierrez, O; Palacios-Gomez, J; Umemoto, M

1998-01-01

Nano-and microcomposites of intermetallic (Co/sub 3/Ti, AlCo/sub 2 /Ti) and ceramic (TiN, Ti(C, N), Al/sub 2/O/sub 3/) phases have been produced by spark plasma sintering (SPS) of powders resulting from mechanical alloying of Al-Co-Ti elemental powder mixtures. The mechanically alloyed powders consisted of mixtures of nanocrystalline and amorphous phases which, on sintering, transformed into complex microstructures of the intermetallic and ceramic phases. For Al contents lower than about 30 at% in the original powder mixtures, the use of SPS led to porosities of 1-2% in the sintered compacts and hardness values as high as ~1700 kg/mm/sup 2/; in these cases, the composite matrix was TiN and Ti(C, N), with the Al/sub 2/O/sub 3/ phase found as finely dispersed particles in the matrix and the Co /sub 3/Ti and AlCo/sub 2/Ti phases as interdispersed grains. (19 refs).

Spark plasma sintering of hydrothermally derived ultrafine Ca doped lanthanum chromite powders

Directory of Open Access Journals (Sweden)

Rendón-Angeles, J. C.

2006-08-01

Full Text Available Lanthanum chromite nano-particles, with a composition of La0.9Ca0.1CrO3 and La0.8Ca0.2CrO3, were produced by 1 h of hydrothermal reaction at 400 and 425°C respectively. The sintering of the powders was conducted using a spark plasma apparatus over the temperature range 1300-1550ºC for 1 min with a constant loading pressure of 45 MPa. Additional sintering experiments using conventional firing were carried out for comparison. Fully densified (98 % r.d. lanthanum chromite pellets with fine equiaxial grains 2.3 μm in size were obtained using the SPS (spark plasma sintering method. In contrast, a maximum relative density of 97 % was produced using La0.8Ca0.2CrO3 sintered conventionally at 1400ºC for 300 min, and the average grain size of the resulting sintered sample was 6 μm.

Partículas ultrafinas de cromita de lantano, con una composición de La0.9Ca0.1CrO3 y La0.8Ca0.2CrO3, se obtuvieron después de 1 hora de síntesis hidrotermal a las temperaturas de 400 y 425°C respectivamente. Los compuestos obtenidos, con un tamaño de partícula de ~ 200 nm, se caracterizaron utilizando las técnicas de DRX, MEB y MET. La sinterización de estos polvos se efectuó en un equipo de chispa de plasma en el rango de temperatura de 1300-1500°C durante 1 min, y a una presión de compactación de 45 MPa. Ambos polvos también se sinterizaron siguiendo un tratamiento térmico convencional, en aire, con el propósito de comparar ambos métodos de sinterización. Las muestras de cromita de lantano sinterizadas por plasma presentaban una densidad relativa del 98 % (/t; y una microestructura monofásica con granos equaxiales con un tamaño medio de grano menor de 2.3 μm. En contraste, la composición La0.8Ca0.2CrO3, sinterizada a 1400°C/300 min, por métodos convencionales alcanzó una densidad relativa máxima del 97 % y su microestructura estaba formada por una sola fase con un tamaño medio de grano de 6 μm.

Microstructural designs of spark-plasma sintered silicon carbide ceramic scaffolds

Directory of Open Access Journals (Sweden)

Román-Manso, B.

2014-04-01

Full Text Available Concentrated ceramic inks based on β-SiC powders, with different amounts of Y2O3 and Al2O3 as sintering aids, are developed for the adequate production of SiC scaffolds, with different patterned morphologies, by the Robocasting technique. The densifi cation of the as-produced 3D structures, previously heat treated in air at 600 ºC for the organics burn-out, is achieved with a Spark Plasma Sintering (SPS furnace. The effects of the amount of sintering additives (7 - 20 wt. % and the size of the SiC powders (50 nm and 0.5 μm on the processing of the inks, microstructure, hardness and elastic modulus of the sintered scaffolds, are studied. The use of nano-sized β-SiC powders significantly restricts the attainable maximum solids volume fraction of the ink (0.32 compared to 0.44 of the submicron-sized powders-based ink, involving a much larger porosity of the green ceramic bodies. Furthermore, reduced amounts of additives improve the mechanical properties of the ceramic skeleton; particularly, the stiffness. The grain size and specific surface area of the starting powders, the ink solids content, green porosity, amount of sintering additives and SPS temperatures are the main parameters to be taken into account for the production of these SiC cellular ceramics.Se han fabricado andamiajes de carburo de silicio (SiC usando la técnica de “Robocasting”, a partir de tintas cerámicas conteniendo β-SiC y distintas cantidades de Y2O3 and Al2O3, como aditivos de sinterización. La densificación de las estructuras tridimensionales, previamente calcinadas a 600 ºC para eliminar los aditivos orgánicos, se realizó en un horno de “Spark Plasma Sintering” (SPS. Se analizó el efecto de la cantidad de aditivos de sinterización (7-20 % en peso y del tamaño de partícula inicial del polvo de SiC (50 nm y 0.5 μm en el procesado de las tintas, en la microestructura, la dureza y el módulo elástico de las estructuras sinterizadas. El uso de polvo

Grain growth control and transparency in spark plasma sintered self-doped alumina materials

International Nuclear Information System (INIS)

Suarez, M.; Fernandez, A.; Menendez, J.L.; Torrecillas, R.

2009-01-01

Doping alumina particles with aluminum alkoxides allows dense spark plasma sintered (SPSed) materials to be obtained that have a refined grain size compared to pure materials, which is critical for their transparency. An optical model considering pore and grain size distributions has been developed to obtain information about porosity in dense materials. This work suggests that the atomic diffusion mechanisms do not depend on the sintering technique. A reduction in the activation energy by a factor of 2 has been found in SPSed materials.

Contribution to the densification study of silicon and zirconium carbides by an innovating process: the Spark Plasma Sintering; Contribution a l'etude de la densification des carbures de silicium et de zirconium par un procede innovant: le spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Allemand, A. [CEA Saclay, Dept. des Materiaux pour le Nucleaire (DEN/DMN/SRMA/LTMEx), 91 - Gif-sur-Yvette (France); Guillard, F.; Galy, J. [Centre d' Elaboration de Materiaux et d' Etudes Structurales (CEMES-CNRS), 31 - Toulouse (France)

2007-07-01

In the framework of the CPR ISMIR, the works presented here take up the results of the thesis of F. Guillard defended on december 2006. This thesis has dealt with the Spark Plasma Sintering (SPS) technique and more particularly have been studied: 1)the {beta}SiC and ZrC sintering 2)the modelling of ZrC sintering by the SPS technique and 3)the studies of the carbides/oxides interfaces carried out by SPS. Concerning the {beta}SiC and ZrC sintering: the two carbides have been sintered between 1450 and 1950 C with times periods of 10 minutes and pressures between 50 and 150 MPa. These experiments have shown that the way to apply the pressure is of major importance. Moreover, 92% of densification can be reached after 5 minutes in 1850 C for SiC. For ZrC, 95% of densification is reached as soon as 5 minutes in 1750 C. Different correlations between grains size, density and the way to apply pressure are presented. For the SPS modelling of ZrC, two existing models, taking into account the diffusion laws, are used to try to model the SPS. The results are presented and discussed. At last, the SPS allows to make interfaces starting from powders or materials previously sintered. The SiC/ZrC and ZrO{sub 2}/SiC interfaces have been studied. A microstructural study is presented as well as a technique which allows the assembling with no cracks of SiC and ZrC. (O.M.)

Compaction of lithium-silicate ceramics using spark plasma sintering

Czech Academy of Sciences Publication Activity Database

Kubatík, Tomáš František; Lukáč, František; Mušálek, Radek; Brožek, Vlastimil; Stehlíková, K.; Chráska, Tomáš

2017-01-01

Roč. 61, č. 1 (2017), s. 40-44 ISSN 0862-5468 R&D Projects: GA ČR GB14-36566G Institutional support: RVO:61389021 Keywords : Li2Si2O5 * Li2SiO3 * Spark plasma sintering (SPS) * Quantitative Rietveld refinement * X-ray diffraction (XRD) Subject RIV: JG - Metallurgy OBOR OECD: Materials engineering Impact factor: 0.439, year: 2016 http://www.ceramics-silikaty.cz/index.php?page=cs_detail_doi&id=789

Phase characterisation in spark plasma sintered TiPt alloy

CSIR Research Space (South Africa)

Chikosha, S

2011-12-01

Full Text Available stream_source_info chikosha_2011.pdf.txt stream_content_type text/plain stream_size 4354 Content-Encoding UTF-8 stream_name chikosha_2011.pdf.txt Content-Type text/plain; charset=UTF-8 PHASE CHARACTERISATION IN SPARK... to form “necks”  Radiant Joule heat and pressure drives “neck” growth and material transfer © CSIR 2006 www.csir.co.za Page 6 Objective  Produce TiPt alloy compacts by Spark plasma sintering (SPS) of equiatomic...

Mechanical characterization of cemented carbide WC-6Co (%wt) manufactured by SPS (Spark Plasma Sintering

International Nuclear Information System (INIS)

Boidi, G.; Tertuliano, A.J.; Machado, I.F.

2016-01-01

This work aimed to manufacture cemented carbide (WC-6%wtCo) obtained by SPS (Spark Plasma Sintering) process and to carry out the mechanical characterization by hardness and fracture toughness. The material was consolidated at 1100 deg C for different holding times (1 min, 5 min, 10 min), in order to evaluate the densification. A reference sample was also used to be compared to SPS. Optical and scanning electron microscopy were carried out to characterize the microstructural features of the samples and mechanical properties were obtained by hardness measurements (micro and macro) and instrumented indentation. The fracture toughness was calculated with the method of Palmqvist. Best results were found in the material sintered by SPS for 10 minutes of holding time, in which 97% of relative density and about 1600 HV_1_0 was reached. (author)

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

Science.gov (United States)

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.

The Influence of Spark Plasma Sintering Temperature on the Microstructure and the Thermoelectric Properties of Al, Ga dually-doped ZnO

DEFF Research Database (Denmark)

Han, Li; Le, Thanh Hung; Van Nong, Ngo

2012-01-01

Al, Ga dually-doped ZnO was prepared by spark plasma sintering with different sintering temperatures. The microstructural evolution and thermoelectric properties of the samples were investigated in detail. The samples with a sintering temperature above 1223K obtained higher relative densities...

Effect of grain size on the hardness and reactivity of plasma-sintered beryllium

International Nuclear Information System (INIS)

Kim, Jae-Hwan; Nakamichi, Masaru

2014-01-01

Beryllium and its intermetallic compounds have attracted great attention as promising neutron multipliers in fusion reactors. In this study, mechanical and chemical properties of fabricated plasma-sintered beryllium (PS-Be) with different grain-sizes are investigated. Density and hardness analysis results of the fabricated PS-Be samples infer that a smaller grain size in the sintered Be indicates higher porosity and hardness. Sintered Be with a large grain size exhibits better resistance toward oxidation at 1273 K in dry air and at 1073 K in Ar/1% H 2 O, since oxidation at the grain boundaries of the determines the rate. In contrast, at 1273 K in Ar/1% H 2 O, a catastrophic oxidation is indicated by the increase of weight of the samples and the generation of H 2 from the bulk Be

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

Science.gov (United States)

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

2018-04-01

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

Microstructures and mechanical properties of 9Cr oxide dispersion strengthened steel produced by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Xie, Rui [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); School of Metallurgy, Northeastern University, Shenyang 110819 (China); Lu, Zheng, E-mail: luz@atm.neu.edu.cn [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); Lu, Chenyang; Li, Zhengyuan [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); Ding, Xueyong [School of Metallurgy, Northeastern University, Shenyang 110819 (China); Liu, Chunming [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China)

2017-02-15

Highlights: • A 9Cr-ODS steel was produced by mechanical alloying and spark plasma sintering. • Bimodal grain size distribution was observed. • Formation mechanism of bimodal grain size distribution was discussed. • The size and number density of nanoscale particles were obtained by SAXS and HRTEM. • The contribution of nano-sized particles to yield strength is dominating. - Abstract: 9Cr oxide dispersion strengthened (ODS) steel was fabricated by mechanical alloying (MA) and spark plasma sintering (SPS). The nano-sized particles, grain size distribution and mechanical properties of 9Cr-ODS steel sintered at 950 °C were studied by synchrotron radiation small angle X-ray scattering (SAXS), high-resolution transmission electron microscopy (HRTEM), electron backscatter diffraction (EBSD) and tensile experiment. The results showed that bimodal grain size distribution in the matrix is observed, which is attributed to the heterogeneous recrystallization process during the SPS. High-density nano-sized Y{sub 2}Ti{sub 2}O{sub 7} and some large oxides of Cr{sub 2}Mn(Ti)O{sub 4} are formed in 9Cr-ODS steel. The number density and average size of Y{sub 2}Ti{sub 2}O{sub 7} obtained from SAXS are 4.72 × 10{sup 22}/m{sup 3} and 4.4 nm, respectively. The yield strengths of 9Cr-ODS steel fabricated by SPS are compared with the typical 9Cr-ODS steel produced by HIP.

Plasma sintering of ferritic steel reinforced with niobium carbide prepared by high energy milling; Sinterizacao a plasma de aco ferritico reforcado com carbeto de niobio preparado por moagem de alta energia

Energy Technology Data Exchange (ETDEWEB)

Silva Junior, J.F. da; Almeida, E.O.; Gomes, U.U.; Alves Junior, C.; Messias, A.P. [Universidade Federal do Rio Grande do Norte (UFRN), Natal (Brazil). Lab. de Materiais Ceramicos e Metais Especiais; Universidade Federal do Rio Grande do Norte (UFRN), Natal (Brazil). Lab. de Processamento de Materiais por Plasma

2010-07-01

Plasma is an ionized gas where ions are accelerated from anode to cathode surface, where the sample is placed. There are a lot of collisions on cathode surface by ions heating and sintering the sample. High energy milling (HEM) is often used to produce composite particles to be used on powder metallurgy. These particles can exhibit fine particles and high phase dispersion. This present work aim to study ferritic steels reinforced with 3%NbC prepared by HEM and sintered on plasma furnace. Ferritic steel and NbC powders were milled during 5 hours and characterized by SEM, XRD and laser scattering. Then, these composite powders were compacted in a cylindrical steel die and then sintered in a plasma furnace. Vickers microhardness tests and SEM and XRD analysis were performed on sintered samples. (author)

The Influence of Spark Plasma Sintering Temperature on the Microstructure and Thermoelectric Properties of Al,Ga Dual-Doped ZnO

DEFF Research Database (Denmark)

Han, Li; Le, Thanh Hung; Van Nong, Ngo

2013-01-01

ZnO dual-doped with Al and Ga was prepared by spark plasma sintering using different sintering temperatures. The microstructural evolution and thermoelectric properties of the samples were investigated in detail. The samples obtained with sintering temperature above 1223 K had higher relative...... of ZnO particles and microstructure evolution at different sintering temperatures were investigated by simulation of the self-Joule-heating effect of the individual particles....

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

Energy Technology Data Exchange (ETDEWEB)

Scott, Spencer M.; Yao, Tiankai [Department of Mechanical, Aerospace, and Nuclear Engineering, Rensselaer Polytechnic Institute, 110 8th Street, Troy, NY 12180 (United States); Lu, Fengyuan [Department of Mechanical & Industrial Engineering, Louisiana State University, Baton Rouge, LA 70803 (United States); Xin, Guoqing; Zhu, Weiguang [Department of Mechanical, Aerospace, and Nuclear Engineering, Rensselaer Polytechnic Institute, 110 8th Street, Troy, NY 12180 (United States); Lian, Jie, E-mail: lianj@rpi.edu [Department of Mechanical, Aerospace, and Nuclear Engineering, Rensselaer Polytechnic Institute, 110 8th Street, Troy, NY 12180 (United States)

2017-03-15

Abstract: High-energy ball milling was used to synthesize Th{sub 1-x}La{sub x}O{sub 2-0.5x} (x = 0.09, 0.23) solid solutions, as well as improve the sinterability of ThO{sub 2} powders. Dense La-doped ThO{sub 2} pellets with theoretical density above 94% were consolidated by spark plasma sintering at temperatures above 1400 °C for 20 min, and the densification behavior and the non-equilibrium effects on phase and structure were investigated. A lattice contraction of the SPS-densified pellets occurred with increasing ball milling duration, and a secondary phase with increased La-content was observed in La-doped pellets. A dependence on the La-content and sintering duration for the onset of localized phase segregation has been proposed. The effects of high-energy ball milling, La-content, and phase formation on the thermal diffusivity were also studied for La-doped ThO{sub 2} pellets by laser flash measurement. Increasing La-content and high energy ball milling time decreases thermal diffusivity; while the sintering peak temperature and holding time beyond 1600 °C dramatically altered the temperature dependence of the thermal diffusivity beyond 600 °C. - Highlights: • Lanthanum incorporation into ThO{sub 2} by high energy ball milling and rapid consolidation by spark plasma sintering. • Elucidation of phase behavior of the La-doped ThO{sub 2} and the contributions of La incorporation and SPS sintering conditions. • Investigation of the effects of La incorporation and high energy ball milling on the thermal behavior of La-doped ThO{sub 2}.

Thermoelectric transport properties of polycrystalline titanium diselenide co-intercalated with nickel and titanium using spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Holgate, T.C. [Department of Energy Storage and Conversion, Technical University of Denmark, Riso Campus, 4000 Roskilde (Denmark); Zhu, S.; Zhou, M. [Department of Physics and Astronomy, Clemson University, Clemson, SC 29634 (United States); Bangarigadu-Sanasy, S.; Kleinke, H. [Department of Chemistry, University of Waterloo, Waterloo, Ontario, N2L 3G1 (Canada); He, J. [Department of Physics and Astronomy, Clemson University, Clemson, SC 29634 (United States); Tritt, T.M., E-mail: ttritt@clemson.edu [Department of Physics and Astronomy, Clemson University, Clemson, SC 29634 (United States)

2013-01-15

Polycrystalline samples of nickel intercalated (0-5%) TiSe{sub 2} were attempted via solid-state reaction in evacuated quartz tubes followed by densification using a spark plasma sintering process. X-ray diffraction data indicated that mixed NiSe{sub 2} and TiSe{sub 2} phases were present after initial synthesis by solid-state reaction, but a pure TiSe{sub 2} phase was present after the spark plasma sintering. While EPMA data reveals the stoichiometry to be near 1:1.8 (Ti:Se) for all samples, comparisons of the measured bulk densities to the theoretical densities suggest that the off stoichiometry is a result of the co-intercalation of both Ni and Ti rather than Se vacancies. Due to the presence of excess Ti (0.085-0.130 per formula) in the van der Waals gap of all the samples, the sensitive electron-hole balance is offset by the additional Ti-3d electrons, leading to an increase in the thermopower (n-type) over pristine, stoichiometric TiSe{sub 2}. The effects of the co-intercalation of both Ni and Ti in TiSe{sub 2} on the structural, thermal, and electrical properties are discussed herein. - Graphical abstract: Co-intercalation of nickel and excess titanium into the van der Waals gap of TiSe{sub 2} via solid state synthesis followed by spark plasma sintering results in a systematic shift in the ratio of hole and electron carrier concentration, which is close to unity for pristine TiSe{sub 2}. This directly affects the electrical transport properties, and as the structural disorder induced by intercalation suppresses the lattice thermal conductivity, co-intercalation is an effective route to enhance the thermoelectric properties of transition metal diselenides. Highlights: Black-Right-Pointing-Pointer Single phase bulk Ni and Ti co-intercalated TiSe{sub 2} samples prepared by spark plasma sintering. Black-Right-Pointing-Pointer Density and X-ray diffraction suggest that the Ni and excess Ti are ordered in the Van der Waals gap. Black-Right-Pointing-Pointer Co

Spark Plasma Sintering of Co{sub 80}Ni{sub 20} nanopowders synthesized by polyol process and their magnetic and mechanical properties

Energy Technology Data Exchange (ETDEWEB)

Ouar, Nassima [Laboratoire des Sciences des Procédés et Matériaux, LSPM, CNRS, UPR 3407, Université Paris XIII, 99 Avenue J.B. Clément, 93430 Villetaneuse (France); Bousnina, Mohamed Ali [Laboratoire des Sciences des Procédés et Matériaux, LSPM, CNRS, UPR 3407, Université Paris XIII, 99 Avenue J.B. Clément, 93430 Villetaneuse (France); Unité de Recherche 99/UR12-30, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Jarzouna (Tunisia); Schoenstein, Frédéric; Mercone, Silvana; Brinza, Ovidiu; Farhat, Samir [Laboratoire des Sciences des Procédés et Matériaux, LSPM, CNRS, UPR 3407, Université Paris XIII, 99 Avenue J.B. Clément, 93430 Villetaneuse (France); Jouini, Noureddine, E-mail: jouini@univ-paris13.fr [Laboratoire des Sciences des Procédés et Matériaux, LSPM, CNRS, UPR 3407, Université Paris XIII, 99 Avenue J.B. Clément, 93430 Villetaneuse (France)

2014-12-05

Highlights: • Nanoparticles of Co{sub 80}Ni{sub 20} alloy were prepared by reduction in polyol medium. • SPS consolidation of these nanoparticles led to bulk nanostructured alloy. • Nanowires present hard magnetic behavior contrarily to nanospheres. • Tunable magnetic properties are achieved from hard to soft character. • Tunable mechanical behavior is achieved from ductile material to almost brittle one. - Abstract: A bottom-up process to elaborate nanostructured cobalt materials is here described. We first, synthesized Co{sub 80}Ni{sub 20} nanowires with a mean length L ∼ 270 nm and a mean diameter d ∼ 7 nm and Co{sub 80}Ni{sub 20} nanospheres with a mean diameter D ∼ 200 nm. This was done by a polyol process in presence of Ruthenium (III) chloride hydrate nucleating agent. Then the as-obtained nanopowders were consolidated by spark plasma sintering (SPS) in order to limit the grain size growth. Nanostructures of powders and of the processed bulk samples were studied and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray (EDX) and field emission gun scanning electron microscope (FEGSEM). Standard VSM measurements were processed for magnetic characterizations. Magnetic static measurements were performed at 10 K and 300 K showing that magnetic properties of nanostructured cobalt bulk systems can be tuned from hard to soft just changing the shape of nano-systems used for compaction and/or the sintering conditions. Also the mechanical properties show a strong dependence on the relative bulk densities and on the characteristics of grain inside the consolidated samples. Preliminary results show that nanostructured cobalt obtained from nanowires compaction present higher Vickers Hardness value.

THE EFFECT OFCARBON NANOTUBES ON THE SINTERING BEHAVIOR OF ZIRCONIA BASED MATERIALS

OpenAIRE

A. M. Zahedi; H. R. Rezaie; J. Javadpour

2015-01-01

Different volume fractions (1.3, 2.6, and 7.6 Vol.%) of carbon nanotubes (CNTs) were dispersed within 8Y-TZP nanopowders. Mixed powder specimens were subsequently processed by spark plasma sintering (SPS) and effects of CNTs on the sintering process of 8Y-TZP/CNT composites was studied. Maintenance of CNTs through the SPS process was confirmed using TEM and Raman Spectroscopy. Studies on the sintering profile of zirconia-CNT composites (Z-xC composites) could, to some extent, clarify the effe...

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

Science.gov (United States)

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

2017-04-27

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

Study of automatic boat loading unit and horizontal sintering process of uranium dioxide pellet

International Nuclear Information System (INIS)

He Zhongjing; Chen Yu; Yao Dengfeng; Wang Youliang; Shu Binhua; Wu Genjiu

2014-01-01

Sintering process is a key process for the manufacture of nuclear fuel UO_2 pellet. In our factory, the continuous high temperature sintering furnace is used for sintering process. During the sintering of green pellets, the furnace, the boat and the accumulation way can influence the quality of the final product. In this text, on the basis of early process research, The automatic loading boat Unit and horizontal sintering process is studied successively. The results show that the physical and chemical properties of the products manufactured by automatic loading boat unit and horizontal sintering process can meet the technique requirements completely, and this system is reliable and continuous. (authors)

Magnetic microstructure and magnetic properties of spark plasma sintered NdFeB magnets

Energy Technology Data Exchange (ETDEWEB)

Huang, Y.L., E-mail: hyl1019_lin@163.com [School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Wang, Y.; Hou, Y.H.; Wang, Y.L.; Wu, Y.; Ma, S.C. [School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Liu, Z.W.; Zeng, D.C. [School of Materials Science and Engineering, South China University of Technology, Guangzhou 510640 (China); Tian, Y.; Xia, W.X. [Key Laboratory of Magnetic Materials and Devices, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201 (China); Zhong, Z.C., E-mail: zzhong2014@sina.com [School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063 (China)

2016-02-01

Nanocrystalline NdFeB magnets were prepared by spark plasma sintering (SPS) technique using melt-spun ribbons as starting materials. A distinct two-zone structure with coarse grain zone and fine grain zone was formed in the SPSed magnets. Multi-domain particle in coarse grain zone and exchange interaction domain for fine grain zone were observed. Intergranular non-magnetic phase was favorable to improve the coercivity due to the enhancement of domain wall pinning effects and increased exchange-decouple. The remanent polarization of 0.83 T, coercivity of 1516 kA/m, and maximum energy product of 118 kJ/m{sup 3} are obtained for an isotropic magnet. - Highlights: • Nanocrystalline NdFeB magnets were prepared by spark plasma sintering technique. • Multi-domain particle and exchange interaction domain were observed. • Magnetic microstructure and their relation to the properties were investigated.

An investigation on preparation of CIGS targets by sintering process

Energy Technology Data Exchange (ETDEWEB)

Zhang Ning, E-mail: zhn98@126.co [Department of Mechanical Engineering, Tsinghua University, Beijing 100084 (China); Zhuang Daming; Zhang Gong [Department of Mechanical Engineering, Tsinghua University, Beijing 100084 (China)

2010-01-15

Pressureless sintering process was used to fabricate CIGS targets with Cu{sub 2}Se, In{sub 2}Se{sub 3}, and Ga{sub 2}Se{sub 3} as raw powders mixed according to the stoichiometry of CuIn{sub 0.72}Ga{sub 0.28}Se{sub 2} (CIGS). The results showed that only CuIn{sub 0.7}Ga{sub 0.3}Se{sub 2} phase can be detected in the sintered targets. The pores in sintered specimen become smaller and distribute more homogeneously under the conditions of finer powders and higher cold pressure. Both mass loss caused by the formation of volatile phase relating to Ga and volume expansion occur during the sintering process, which result in the decrease of density. The tendency of anti-densification becomes stronger under the conditions of coarser powders and higher cold pressure. The sintering process and causes for anti-densification were discussed. Finally, a hot pressing process was carried out, which was proved to be fairly effective to increase the density of CIGS target. The fabricated target can be used for magnetron-sputtering deposition of CIGS absorbers.

Preparation of Nd–Fe–B sintered magnets from HDDR-processed powder

Energy Technology Data Exchange (ETDEWEB)

Takagi, Kenta, E-mail: k-takagi@aist.go.jp [Green Innovative Magnetic Materials Research Center, National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan); Akada, Misaho [Magnetic Materials R& D Center, Research Associations of Magnetic Materials for High-Efficiency Motors (MagHEM), Nagoya 463-8560 (Japan); Soda, Rikio; Ozaki, Kimihiro [Green Innovative Magnetic Materials Research Center, National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan)

2015-11-01

The electric-current sintering technique was used to fully densify hydrogenation–disproportionation–desorption–recombination (HDDR)-processed Nd–Fe–B powder at temperatures below the grain growth temperature in order to produce high-coercive bulk magnets. However, the sintered magnets exhibited anomalous coercivity reduction that depended on sintered density. Reheating examination of the sintered magnets revealed that the reduced coercivity was increased in proportion to the heating temperature, resulting in complete recovery of coercivity. As a result, the combination of electric-current sintering and post-annealing produced sintered magnets with a coercivity of 15 kOe. Scanning and transmission electron microscopy revealed no evidence that associated the anomalous coercivity reduction and recovery with grain boundary morphology. On the other hand, various HDDR powders with different particle sizes were sintered, and finer powders yielded lower coercivity after sintering, implying that the anomalous coercivity reduction was associated with particle surface oxides of the raw powder. - Highlights: • We conduct a sintering of HDDR-processed Nd–Fe–B powder without coercivity reduction. • Rapid current sintering allows densification of this powder without grain growth. • However, the sintered magnets show an anomalous coercivity reduction phenomenon. • It is found that post-annealing completely recovers the reduced coercivity. • The anomalous coercivity reduction would be due to surface oxide of the raw powder.

Synthesis and properties of nanostructured dense LaB6 cathodes by arc plasma and reactive spark plasma sintering

International Nuclear Information System (INIS)

Zhou Shenlin; Zhang Jiuxing; Liu Danmin; Lin Zulun; Huang Qingzhen; Bao Lihong; Ma Ruguang; Wei Yongfeng

2010-01-01

Nanostructured polycrystalline LaB 6 ceramics were prepared by the reactive spark plasma sintering method, using boron nanopowders and LaH 2 powders with a particle size of about 30 nm synthesized by hydrogen dc arc plasma. The reaction mechanism of sintering, crystal structure, microstructure, grain orientations and properties of the materials were investigated using differential scanning calorimetry, X-ray diffraction, Neutron powder diffraction, Raman spectroscopy, transmission electron microscopy and electron backscattered diffraction. It is shown that nanostructured dense LaB 6 with a fibrous texture can be fabricated by SPS at a pressure of 80 MPa and temperature of 1300 deg. C for 5 min. Compared with the coarse polycrystalline LaB 6 prepared by traditional methods, the nanostructured LaB 6 bulk possesses both higher mechanical and higher thermionic emission properties. The Vickers hardness was 22.3 GPa, the flexural strength was 271.2 MPa and the maximum emission current density was 56.81 A cm -2 at a cathode temperature of 1600 deg. C.

Plasma preparation and low-temperature sintering of spherical TiC-Fe composite powder

Institute of Scientific and Technical Information of China (English)

Jian-jun Wang; Jun-jie Hao; Zhi-meng Guo; Song Wang

2015-01-01

A spherical Fe matrix composite powder containing a high volume fraction (82vol%) of fine TiC reinforcement was produced us-ing a novel process combining in situ synthesis and plasma techniques. The composite powder exhibited good sphericity and a dense struc-ture, and the fine sub-micron TiC particles were homogeneously distributed in theα-Fe matrix. A TiC–Fe cermet was prepared from the as-prepared spherical composite powder using powder metallurgy at a low sintering temperature;the product exhibited a hardness of HRA 88.5 and a flexural strength of 1360 MPa. The grain size of the fine-grained TiC and special surface structure of the spherical powder played the key roles in the fabrication process.

Structure and strength of aluminum with sub-micrometer/micrometer grain size prepared by spark plasma sintering

DEFF Research Database (Denmark)

Le, G.M.; Godfrey, A.; Hansen, Niels

2013-01-01

A spark plasma sintering (SPS) technique has been applied to prepare fully dense Al samples from Al powder. By applying a sintering temperature of 600°C and a loading pressure of 50MPa, fully recrystallized samples of nearly 100% density with average grain sizes of 5.2μm, 1.3μm and 0.8μm have bee...... strengthening. © 2013 Elsevier Ltd....

Kinetics, Stability, and Thermal Contact Resistance of Nickel–Ca3Co4O9 Interfaces Formed by Spark Plasma Sintering

DEFF Research Database (Denmark)

Holgate, Tim; Wu, NingYu; Søndergaard, M.

2013-01-01

3Co4O9) have been formed directly by spark plasma sintering (SPS). An intermediate NiO phase is formed during the SPS processes, which grows during post-heating with Co entering from the cobaltate side to form a graded Ni1xCoxO interfacial layer. The electrical and thermal transport across...

Fe-Zn intermetallic phases prepared by diffusion annealing and spark-plasma sintering

Czech Academy of Sciences Publication Activity Database

Pokorný, P.; Cinert, Jakub; Pala, Zdeněk

2016-01-01

Roč. 50, č. 2 (2016), s. 253-256 ISSN 1580-2949 R&D Projects: GA ČR GB14-36566G Institutional support: RVO:61389021 Keywords : Fe-Zn intermetallics * spark-plasma sintering * diffusion annealing * phase composition * hardness Subject RIV: JK - Corrosion ; Surface Treatment of Materials Impact factor: 0.436, year: 2016

Fabrication mechanism of FeSe superconductors with high-energy ball milling aided sintering process

International Nuclear Information System (INIS)

Zhang, Shengnan; Liu, Jixing; Feng, Jianqing; Wang, Yao; Ma, Xiaobo; Li, Chengshan; Zhang, Pingxiang

2015-01-01

FeSe Superconducting bulks with high content of superconducting PbO-type β-FeSe phase were prepared with high-energy ball milling (HEBM) aided sintering process. During this process, precursor powders with certain Fe/Se ratio were ball milled first then sintered. The influences of HEBM process as well as initial Fe/Se ratio on the phase evolution process were systematically discussed. With HEBM process and proper initial Fe/Se ratio, the formation of non-superconducting hexagonal δ-FeSe phase were effectively avoided. FeSe bulk with the critical temperature of 9.0 K was obtained through a simple one-step sintering process with lower sintering temperature. Meanwhile, the phase evolution mechanism of the HEBM precursor powders during sintering was deduced based on both the thermodynamic analysis and step-by-step sintering results. The key function of the HEBM process was to provide a high uniformity of chemical composition distribution, thus to successfully avoide the formation of intermediate product during sintering, including FeSe 2 and Fe 7 Se 8 . Therefore, the fundamental principal for the synthesis of FeSe superconductors were concluded as: HEBM aided sintering process, with the sintering temperature of >635 °C and a slow cooling process. - Highlights: • A novel synthesis technique was developed for FeSe based superconductors. • FeSe bulks with high Tc and high β-FeSe phase content has been obtained. • Phase evolution process for the HEBM aided sintering process was proposed

Two-step flash light sintering process for crack-free inkjet-printed Ag films

International Nuclear Information System (INIS)

Park, Sung-Hyeon; Kim, Hak-Sung; Jang, Shin; Lee, Dong-Jun; Oh, Jehoon

2013-01-01

In this paper, a two-step flash light sintering process for inkjet-printed Ag films is investigated with the aim of improving the quality of sintered Ag films. The flash light sintering process is divided into two steps: a preheating step and a main sintering step. The preheating step is used to remove the organic binder without abrupt vaporization. The main sintering step is used to complete the necking connections among the silver nanoparticles and achieve high electrical conductivity. The process minimizes the damage on the polymer substrate and the interface between the sintered Ag film and polymer substrate. The electrical conductivity is calculated by measuring the resistance and cross-sectional area with an LCR meter and 3D optical profiler, respectively. It is found that the resistivity of the optimal flash light-sintered Ag films (36.32 nΩ m), which is 228.86% of that of bulk silver, is lower than that of thermally sintered ones (40.84 nΩ m). Additionally, the polyimide film used as the substrate is preserved with the inkjet-printed pattern shape during the flash light sintering process without delamination or defects. (paper)

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

International Nuclear Information System (INIS)

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

2012-01-01

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

Influence of graphite contamination on the optical properties of transparent spinel obtained by spark plasma sintering

International Nuclear Information System (INIS)

Bernard-Granger, G.; Benameur, N.; Guizard, C.; Nygren, M.

2009-01-01

The optical properties of transparent spinel sintered by spark plasma sintering have been investigated for incident electromagnetic radiations with wavelengths in the range 0.2-2 μm. It is shown that residual porosities and second-phase graphite particles have a strong influence on the in-line transmittance. Because of the graphite particles, the in-line transmittance measured does not approach that of monocrystalline spinel for wavelengths above 1 μm

Comparison of Ti(C,N)-based cermets processed by hot-pressing sintering and conventional pressureless sintering

International Nuclear Information System (INIS)

Xu, Qingzhong; Ai, Xing; Zhao, Jun; Qin, Weizhen; Wang, Yintao; Gong, Feng

2015-01-01

Highlights: • The HP sintered Ti(C,N)-based cermets exhibit high hardness with fine grain size. • The PLS sintered cermets possess high mechanical properties with low porosity. • The applied pressure can rearrange particles and contribute to grain refinement. • The heating rate can greatly affect the solid and liquid phase sintering of cermets. - Abstract: A suitable sintering method is important to obtain the Ti(C,N)-based cermets with superior properties. In this paper, Ti(C,N)-based cermets were fabricated by hot-pressing sintering (HP) and conventional pressureless sintering (PLS) technology, respectively, to investigate the influence of different sintering methods on the microstructure and mechanical properties of cermets materials. The microstructure, fracture morphology, indention cracks and phase composition were observed and detected using scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The transverse rupture strength (TRS), Vickers hardness (HV) and fracture toughness (K IC ) were also measured. The results reveal that all of the Ti(C,N)-based cermets exhibit core–rim microstructures with black cores, white cores and grey rims embedded into metal binder phases. The grain size of the samples fabricated by HP is much finer and the structure is more compact than those fabricated by PLS, while there exist pores in the HP sintered samples. The sintering process has no influence on the phase composition of cermets, but affects the phase content and crystallinity. The samples fabricated by PLS present higher transverse rupture strength, fracture toughness and density than samples fabricated by HP. However, the HP sintered samples possess a higher hardness

Structural and magnetic studies on spark plasma sintered SmCo{sub 5}/Fe bulk nanocomposite magnets

Energy Technology Data Exchange (ETDEWEB)

Rama Rao, N.V. [Defence Metallurgical Research Laboratory, Hyderabad 500 058 (India); Gopalan, R. [Defence Metallurgical Research Laboratory, Hyderabad 500 058 (India)]. E-mail: rg_gopy@yahoo.com; Manivel Raja, M. [Defence Metallurgical Research Laboratory, Hyderabad 500 058 (India); Chandrasekaran, V. [Defence Metallurgical Research Laboratory, Hyderabad 500 058 (India); Chakravarty, D. [International Advanced Research Centre for Powder Metallurgy and New Materials, Hyderabad 500 005 (India); Sundaresan, R. [International Advanced Research Centre for Powder Metallurgy and New Materials, Hyderabad 500 005 (India); Ranganathan, R. [Saha Institute of Nuclear Physics, Kolkata 700 064 (India); Hono, K. [National Institute for Materials Science, 1-2-1 Sengen, Tsukuba 305 0047 (Japan)

2007-05-15

SmCo{sub 5}+xwt% Fe (x=0, 5 and 10) nanocomposite powders were synthesized by mechanical milling and were consolidated into bulk shape by spark plasma sintering (SPS) technique. The evolution of structure and magnetic properties were systematically investigated in milled powders as well as in SPS samples. A maximum coercivity of 8.9kOe was achieved in spark plasma sintered SmCo{sub 5}+5wt% Fe sample. The exchange spring interaction between the hard and soft magnetic phases was evaluated using {delta}M-H measurements and the analysis revealed that the SPS sample containing 5wt% Fe had a stronger exchange coupling between the magnetic phases than that of the sample with10wt% Fe.

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

Science.gov (United States)

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.

Experimental investigations on the synthesis of W–Cu nanocomposite through spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Elsayed, Ayman, E-mail: aymanhamada@cmrdi.sci.eg [Central Metallurgical R& D Institute, Department of Powder Technology, P.O. Box 87, Helwan, Cairo 11421 (Egypt); Li, Wei [San Diego State University, College of Engineering, Department of Mechanical Engineering, 5500 Campanile Drive, San Diego, CA 92128-1326 (United States); El Kady, Omayma A. [Central Metallurgical R& D Institute, Department of Powder Technology, P.O. Box 87, Helwan, Cairo 11421 (Egypt); Daoush, Walid M. [Helwan University, Faculty of Industrial Education, Department of Production Technology, Cairo (Egypt); Olevsky, Eugene A.; German, Randall M. [San Diego State University, College of Engineering, Department of Mechanical Engineering, 5500 Campanile Drive, San Diego, CA 92128-1326 (United States)

2015-08-05

Highlights: • Tungsten–copper composites have been synthesized using SPS of nano powders. • Various preparation methods, namely mixing, milling and coating have been used. • Conventional compaction and sintering has also been used for comparison. • The composites by SPS have shown finer microstructure and better hardness. • Mixing has proven best preparation method with best physical/mechanical properties. - Abstract: Elemental powders of nanosized tungsten and chemically deposited nanosized copper were used for preparing tungsten/copper composites, which are used as electric contact components. A composite of 70 wt.%W/30 wt.%Cu (52 vol%W/48 vol%Cu) composition was prepared by three powder metallurgy techniques. Elemental mixing, mechanical milling and electroless Cu coating on tungsten particles were used for the synthesis. The obtained powder blends underwent consolidation by rapid hot pressing using the spark plasma sintering (SPS) route at 950 °C under vacuum and by conventional vacuum pressureless sintering for comparison. The elemental powders and the sintered composites were investigated by optical microscopy and SEM. Electrical conductivity, hardness, transverse rupture strength, and wear properties were measured. Results show that the synthesis of the composite by the investigated route yields good performance. Samples prepared by SPS have shown better mechanical properties than those prepared by compaction and sintering due to their fine microstructure.

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

Science.gov (United States)

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.

Chemically produced nanostructured ODS-lanthanum oxide-tungsten composites sintered by spark plasma

International Nuclear Information System (INIS)

Yar, Mazher Ahmed; Wahlberg, Sverker; Bergqvist, Hans; Salem, Hanadi G.; Johnsson, Mats; Muhammed, Mamoun

2011-01-01

High purity W and W-0.9La 2 O 3 (wt.%) nanopowders were produced by a wet chemical route. The precursor was prepared by the reaction of ammonium paratungstate (APT) with lanthanum salt in aqueous solutions. High resolution electron microscopy investigations revealed that the tungstate particles were coated with oxide precipitates. The precursor powder was reduced to tungsten metal with dispersed lanthanum oxide. Powders were consolidated by spark plasma sintering (SPS) at 1300 and 1400 o C to suppress grain growth during sintering. The final grain size relates to the SPS conditions, i.e. temperature and heating rate, regardless of the starting powder particle size. Scanning electron microscopy revealed that oxide phases were mainly accumulated at grain boundaries while the tungsten matrix constituted of nanosized sub-grains. The transmission electron microscopy revealed that the tungsten grains consist of micron-scale grains and finer sub-grains. EDX analysis confirmed the presence of W in dispersed oxide phases with varying chemical composition, which evidenced the presence of complex oxide phases (W-O-La) in the sintered metals.

Temperature Field Simulation of Powder Sintering Process with ANSYS

Science.gov (United States)

He, Hongxiu; Wang, Jun; Li, Shuting; Chen, Zhilong; Sun, Jinfeng; You, Ying

2018-03-01

Aiming at the “spheroidization phenomenon” in the laser sintering of metal powder and other quality problems of the forming parts due to the thermal effect, the finite element model of the three-dimensional transient metal powder was established by using the atomized iron powder as the research object. The simulation of the mobile heat source was realized by means of parametric design. The distribution of the temperature field during the sintering process under different laser power and different spot sizes was simulated by ANSYS software under the condition of fully considering the influence of heat conduction, thermal convection, thermal radiation and thermophysical parameters. The influence of these factors on the actual sintering process was also analyzed, which provides an effective way for forming quality control.

Characterization of In-Situ Cu–TiH2–C and Cu–Ti–C Nanocomposites Produced by Mechanical Milling and Spark Plasma Sintering

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Nguyen Thi Hoang Oanh

2017-03-01

Full Text Available This study focuses on the fabrication and microstructural investigation of Cu–TiH2–C and Cu–Ti–C nanocomposites with different volume fractions (10% and 20% of TiC. Two mixtures of powders were ball milled for 10 h, consequently consolidated by spark plasma sintering (SPS at 900 and 1000 °C producing bulk materials with relative densities of 95–97%. The evolution process of TiC formation during sintering process was studied by using X-ray diffraction (XRD, scanning electron microscopy (SEM, and high resolution transmission electron microscopy (HRTEM. XRD patterns of composites present only Cu and TiC phases, no residual Ti phase can be detected. TEM images of composites with (10 vol % TiC sintered at 900 °C show TiC nanoparticles about 10–30 nm precipitated in copper matrix, most of Ti and C dissolved in the composite matrix. At the higher sintering temperature of 1000 °C, more TiC precipitates from Cu–TiH2–C than those of Cu–Ti–C composite, particle size ranges from 10 to 20 nm. The hardness of both nanocomposites also increased with increasing sintering temperature. The highest hardness values of Cu–TiH2–C and Cu–Ti–C nanocomposites sintered at 1000 °C are 314 and 306 HV, respectively.

Solidification of high level liquid waste (HLLW) into ceramics by sintering process

International Nuclear Information System (INIS)

Masuda, Sumio; Oguino, Naohiko; Tsunoda, Naomi; O-oka, Kazuo; Ohta, Takao.

1979-01-01

One of the alternatives to vitrified solid which is acceptable and well characterized for storing radioactive HLLW with desirable long-term stability is ceramics. On the other hand, the solidification process of highly radioactive wastes should be simple and suitable for continuous production. On the above described basis, the authors have made preliminary study on the production of sintered ceramics by the addition of several oxides to HLLW. The simulated waste and additive oxides were pressed in a mold to make the preforms of 50 mm diameter and 10 to 15 mm thick. The preforms were then normally sintered at temperature from 1000 to 1400 deg C for 2 to 4 hours. The characterization of the sintered solids revealed the following facts. (1) X-ray diffraction analysis showed that the expected crystals were formed by normal-sintering as well as by hot-pressing. (2) The bulk density of the ceramics by normal-sintering was around 90 to 95% of the assumed theoretical values. (3) The leach-rate of the solids was affected by the bulk density. (4) Other properties of the solids, such as thermal expansion or thermal conductivity, are dominantly determined by those of main crystals in the solids. Sintering process is generally simple and productive as far as normal sintering is concerned. However, hot-pressing is an intermittent and time consuming process. From this fact, the authors intended to adopt the normal sintering process for the ceramic solidification of high level liquid wastes. (Wakatsuki, Y.)

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

Science.gov (United States)

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

2018-05-01

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

Assessment of consolidation of oxide dispersion strengthened ferritic steels by spark plasma sintering: from laboratory scale to industrial products

International Nuclear Information System (INIS)

Boulnat, X.; Fabregue, D.; Perez, M.; Urvoy, S.; Hamon, D.; Carlan, Y. de

2014-01-01

Oxide dispersion strengthened steels are new generation alloys that are usually processed by hot isostatic pressing (HIP). In this study, spark plasma sintering (SPS) was studied as an alternative consolidation technique. The influence of the processing parameters on the microstructure was quantified. The homogeneity of the SPSed materials was characterised by electron microprobe and microhardness. A combination of limited grain growth and minimised porosity can be achieved on semi-industrial compact. Excellent tensile properties were obtained compared to the literature. (authors)

Processing, Mechanical and Optical Properties of Additive-Free ZrC Ceramics Prepared by Spark Plasma Sintering

Directory of Open Access Journals (Sweden)

Clara Musa

2016-06-01

Full Text Available In the present study, nearly fully dense monolithic ZrC samples are produced and broadly characterized from microstructural, mechanical and optical points of view. Specifically, 98% dense products are obtained by Spark Plasma Sintering (SPS after 20 min dwell time at 1850 °C starting from powders preliminarily prepared by Self-propagating High-temperature Synthesis (SHS followed by 20 min ball milling. A prolonged mechanical treatment up to 2 h of SHS powders does not lead to appreciable benefits. Vickers hardness of the resulting samples (17.5 ± 0.4 GPa is reasonably good for monolithic ceramics, but the mechanical strength (about 250 MPa up to 1000 °C could be further improved by suitable optimization of the starting powder characteristics. The very smoothly polished ZrC specimen subjected to optical measurements displays high absorption in the visible-near infrared region and low thermal emittance at longer wavelengths. Moreover, the sample exhibits goodspectral selectivity (2.1–2.4 in the 1000–1400 K temperature range. These preliminary results suggest that ZrC ceramics produced through the two-step SHS/SPS processing route can be considered as attractive reference materials for the development of innovative solar energy absorbers.

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

Directory of Open Access Journals (Sweden)

Philipp Drescher

2016-12-01

Full Text Available 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.

Strengthening mechanisms in a high-strength bulk nanostructured Cu–Zn–Al alloy processed via cryomilling and spark plasma sintering

International Nuclear Information System (INIS)

Wen, Haiming; Topping, Troy D.; Isheim, Dieter; Seidman, David N.; Lavernia, Enrique J.

2013-01-01

A bulk nanostructured alloy with the nominal composition Cu–30Zn–0.8Al wt.% (commercial designation brass 260) was fabricated by cryomilling of brass powders and subsequent spark plasma sintering (SPS) of the cryomilled powders, yielding a compressive yield strength of 950 MPa, which is significantly higher than the yield strength of commercial brass 260 alloys (∼200–400 MPa). Transmission electron microscopy investigations revealed that cryomilling results in an average grain diameter of 26 nm and a high density of deformation twins. Nearly fully dense bulk samples were obtained after SPS of cryomilled powders, with average grain diameter 110 nm. After SPS, 10 vol.% of twins is retained with average twin thickness 30 nm. Three-dimensional atom-probe tomography studies demonstrate that the distribution of Al is highly inhomogeneous in the sintered bulk samples, and Al-containing precipitates including Al(Cu,Zn)–O–N, Al–O–N and Al–N are distributed in the matrix. The precipitates have an average diameter of 1.7 nm and a volume fraction of 0.39%. Quantitative calculations were performed for different strengthening contributions in the sintered bulk samples, including grain boundary, twin boundary, precipitate, dislocation and solid-solution strengthening. Results from the analyses demonstrate that precipitate and grain boundary strengthening are the dominant strengthening mechanisms, and the calculated overall yield strength is in reasonable agreement with the experimentally determined compressive yield strength

Luminescence properties of the Mg co–doped Ce:SrHfO_3 ceramics prepared by the Spark Plasma Sintering Method

International Nuclear Information System (INIS)

Chiba, Hiroyuki; Kurosawa, Shunsuke; Harata, Koichi; Murakami, Rikito; Yamaji, Akihiro; Ohashi, Yuji; Pejchal, Jan; Kamada, Kei; Yokota, Yuui; Yoshikawa, Akira

2016-01-01

1300 or 1400 °C pre–sintered Al/Ce/Mg:SrHfO_3 and Al/Ce:SrHfO_3 ceramics were prepared by the Spark Plasma Sintering (SPS) in order to search for a new scintillation material with a high–effective atomic number(Z_e_f_f) and good light output. The SrHfO_3 has a high Z_e_f_f of 60, and high gamma–ray detection efficiency is expected. Meanwhile it has a high melting point of over 2500 °C, and single crystal is hard to be grown. On the other hand, high melting materials can be prepared as ceramics, and the SPS method is a simple process to fabricate the ceramics within a few hours. Thus, we prepared the samples using the SPS method, and their optical and scintillation properties were investigated. We found that Al/Ce/Mg:SrHfO_3 and Al/Ce:SrHfO_3 ceramics had an emission wavelength at around 400 nm originating from 5d–4f transition of Ce"3"+. Moreover, Al/Ce/Mg:SrHfO_3 pre-sintered at a temperature of 1400 °C had a light output of approximately 5,000 ph/MeV. In this paper, the light output of Mg-co-doped samples was improved compared with the Mg-free ones. The light output also depends on the pre-sintering temperature. - Highlights: • Luminescence Properties of Al/Ce/Mg:SrHfO_3 ceramics scintillator was investigated. • These ceramics were prepared by the Spark Plasma Sintering Method. • Light output of the Al/Ce/Mg:SrHfO_3 ceramics was approximately 5,000 ph/MeV.

Microstructural stability of spark-plasma-sintered Wf/W composite with zirconia interface coating under high-heat-flux hydrogen beam irradiation

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M. Avello de Lama

2017-12-01

In this paper, the durability and chemical stability of Wf/W composite specimens under cyclic heat-flux loads up to 20 MW/m² (surface temperature: 1260 °C was investigated using hydrogen neutral beam. The bulk material was fabricated by means of spark-plasma-sintering (SPS method using fine tungsten powder and a stack of tungsten wire meshes as reinforcement where the surface of the wire was coated with zirconia thin film to produce an engineered interface. The impact of plasma beam irradiation on microstructure was examined for two kinds of specimens produced at different sintering temperatures, 1400 °C and 1700 °C. Results of microscopic (SEM and chemical (EDX analysis are presented comparing the microstructure and element distribution maps obtained before and after heat flux loading. Effects of different sintering temperatures on damage behaviour are discussed. The present composite materials are shown to be applicable as plasma-facing material for high-heat-flux components.

Dry Sliding Wear Behavior of Spark Plasma Sintered Fe-Based Bulk Metallic Glass/Graphite Composites

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Xiulin Ji

2016-09-01

Full Text Available Bulk metallic glass (BMG and BMG-graphite composites were fabricated using spark plasma sintering at the sintering temperature of 575 °C and holding time of 15 min. The sintered composites exhibited partial crystallization and the presence of distributed porosity and graphite particles. The effect of graphite reinforcement on the tribological properties of the BMG/graphite composites was investigated using dry ball-on-disc sliding wear tests. The reinforcement of graphite resulted in a reduction in both the wear rate and the coefficient of friction as compared to monolithic BMG samples. The wear surfaces of BMG/graphite composites showed regions of localized wear loss due to microcracking and fracture, as was also the case with the regions covered with graphite-rich protective film due to smearing of pulled off graphite particles.

Low-temperature plasma nitriding of sintered PIM 316L austenitic stainless steel

Energy Technology Data Exchange (ETDEWEB)

Mendes, Aecio Fernando; Scheuer, Cristiano Jose; Joanidis, Ioanis Labhardt; Cardoso, Rodrigo Perito; Mafra, Marcio; Klein, Aloisio Nelmo; Brunatto, Silvio Francisco, E-mail: brunatto@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Engenharia Mecanica. Grupo de Tecnologia de Fabricacao Assistida pro Plasma e Metalurgia do Po

2014-08-15

This work reports experimental results on sintered PIM 316L stainless steel low-temperature plasma nitriding. The effect of treatment temperature and time on process kinetics, microstructure and surface characteristics of the nitrided samples were investigated. Nitriding was carried out at temperatures of 350, 380, 410 and 440 °C , and times of 4, 8 and 16 h, using a gas mixture composed by 60% N2 + 20% H2 + 20% Ar, at a gas flow rate of 5.00 X 10{sup 6} Nm{sup 3-1}, and a pressure of 800 Pa. The treated samples were characterized by scanning electron microscopy, X-ray diffractometry and microhardness measurements. Results indicate that low-temperature plasma nitriding is a diffusion controlled process. The calculated activation energy for nitrided layer growth was 111.4 kJmol{sup -1}. Apparently precipitation-free layers were produced in this study. It was also observed that the higher the treatment temperature and time the higher is the obtained surface hardness. Hardness up to 1343 HV{sub 0.025} was verified for samples nitrided at 440 °C. Finally, the characterization of the treated surface indicates the formation of cracks, which were observed in regions adjacent to the original pores after the treatment. (author)

Process for the production of metal nitride sintered bodies and resultant silicon nitride and aluminum nitride sintered bodies

Science.gov (United States)

Yajima, S.; Omori, M.; Hayashi, J.; Kayano, H.; Hamano, M.

1983-01-01

A process for the manufacture of metal nitride sintered bodies, in particular, a process in which a mixture of metal nitrite powders is shaped and heated together with a binding agent is described. Of the metal nitrides Si3N4 and AIN were used especially frequently because of their excellent properties at high temperatures. The goal is to produce a process for metal nitride sintered bodies with high strength, high corrosion resistance, thermal shock resistance, thermal shock resistance, and avoidance of previously known faults.

Barium titanate nanometric polycrystalline ceramics fired by spark plasma sintering.

Czech Academy of Sciences Publication Activity Database

Ctibor, Pavel; Sedláček, J.; Ryukhtin, Vasyl; Cinert, Jakub; Lukáč, František

2016-01-01

Roč. 42, č. 14 (2016), s. 15989-15993 ISSN 0272-8842 R&D Projects: GA ČR GB14-36566G; GA MŠk LM2015056 Institutional support: RVO:61389021 ; RVO:61389005 Keywords : BaTiO3 * Spark plasma sintering * Electrical properties Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass; JH - Ceramics, Fire-Resistant Materials and Glass (UJF-V) Impact factor: 2.986, year: 2016 http://www.sciencedirect.com/science/article/pii/S0272884216311695

High-performance Ag0.8Pb18+xSbTe20 thermoelectric bulk materials fabricated by mechanical alloying and spark plasma sintering

International Nuclear Information System (INIS)

Wang Heng; Li Jingfeng; Nan Cewen; Zhou Min; Liu Weishu; Zhang Boping; Kita, Takuji

2006-01-01

Polycrystalline Ag n Pb m SbTe m+2n thermoelectric materials, whose compositions can be described as Ag 0.8 Pb 18+x SbTe 20 were prepared using a combined process of mechanical alloying and spark plasma sintering. Electric properties of the sintered samples with different Pb contents were measured from room temperature to 700 K. The maximum power factor of 1.766 mW/mK 2 was obtained at 673 K for the Ag 0.8 Pb 22 SbTe 20 sample, which corresponds to a high dimensionless figure of merit, ZT=1.37. This best composition is different from that reported before

Fabrication and thermoelectric performance of textured n-type Bi2(Te,Se)3 by spark plasma sintering

International Nuclear Information System (INIS)

Jiang Jun; Chen Lidong; Bai Shengqiang; Yao Qin; Wang Qun

2005-01-01

The n-type Bi 2 (Te,Se) 3 thermoelectric materials with preferred grain orientation have been fabricated through the spark plasma sintering (SPS) technique. The c-axis of the grains in the sintered samples were preferentially oriented parallel to the pressing direction, the orientation factor of the (0 0 l) planes changed from 0.4 to 0.85 with the sintering conditions. The anisotropy was investigated by measuring the electrical conductivities in the two directions perpendicular and parallel to the pressing direction. The optimal figure of merit ZT (ZT = α 2 σT/κ) of the sintered materials in the direction perpendicular to the pressing direction was comparative to that of the zone-melted materials in the same crystallographic direction, while the bending strength reached about 80 MPa, which is 7-8 times of that of the zone-melted materials

Spark Plasma Co-Sintering of Mechanically Milled Tool Steel and High Speed Steel Powders.

Science.gov (United States)

Pellizzari, Massimo; Fedrizzi, Anna; Zadra, Mario

2016-06-16

Hot work tool steel (AISI H13) and high speed steel (AISI M3:2) powders were successfully co-sintered to produce hybrid tool steels that have properties and microstructures that can be modulated for specific applications. To promote co-sintering, which is made difficult by the various densification kinetics of the two steels, the particle sizes and structures were refined by mechanical milling (MM). Near full density samples (>99.5%) showing very fine and homogeneous microstructure were obtained using spark plasma sintering (SPS). The density of the blends (20, 40, 60, 80 wt % H13) was in agreement with the linear rule of mixtures. Their hardness showed a positive deviation, which could be ascribed to the strengthening effect of the secondary particles altering the stress distribution during indentation. A toughening of the M3:2-rich blends could be explained in view of the crack deviation and crack arrest exerted by the H13 particles.

Spark Plasma Co-Sintering of Mechanically Milled Tool Steel and High Speed Steel Powders

Directory of Open Access Journals (Sweden)

Massimo Pellizzari

2016-06-01

Full Text Available Hot work tool steel (AISI H13 and high speed steel (AISI M3:2 powders were successfully co-sintered to produce hybrid tool steels that have properties and microstructures that can be modulated for specific applications. To promote co-sintering, which is made difficult by the various densification kinetics of the two steels, the particle sizes and structures were refined by mechanical milling (MM. Near full density samples (>99.5% showing very fine and homogeneous microstructure were obtained using spark plasma sintering (SPS. The density of the blends (20, 40, 60, 80 wt % H13 was in agreement with the linear rule of mixtures. Their hardness showed a positive deviation, which could be ascribed to the strengthening effect of the secondary particles altering the stress distribution during indentation. A toughening of the M3:2-rich blends could be explained in view of the crack deviation and crack arrest exerted by the H13 particles.

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

Science.gov (United States)

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

2018-02-01

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

Fabrication of Ni-Ti Alloy by Self-Propagating High-Temperature Synthesis and Spark Plasma Sintering Technique

Czech Academy of Sciences Publication Activity Database

Salvetr, P.; Kubatík, Tomáš František; Pignol, D.; Novák, P.

2017-01-01

Roč. 48, č. 2 (2017), s. 772-778 ISSN 1073-5615 Institutional support: RVO:61389021 Keywords : powder metallurgy * Spark plasma sintering Subject RIV: JJ - Other Materials OBOR OECD: Materials engineering Impact factor: 1.642, year: 2016

Hydrogen Plasma Processing of Iron Ore

Science.gov (United States)

Sabat, Kali Charan; Murphy, Anthony B.

2017-06-01

Iron is currently produced by carbothermic reduction of oxide ores. This is a multiple-stage process that requires large-scale equipment and high capital investment, and produces large amounts of CO2. An alternative to carbothermic reduction is reduction using a hydrogen plasma, which comprises vibrationally excited molecular, atomic, and ionic states of hydrogen, all of which can reduce iron oxides, even at low temperatures. Besides the thermodynamic and kinetic advantages of a hydrogen plasma, the byproduct of the reaction is water, which does not pose any environmental problems. A review of the theory and practice of iron ore reduction using a hydrogen plasma is presented. The thermodynamic and kinetic aspects are considered, with molecular, atomic and ionic hydrogen considered separately. The importance of vibrationally excited hydrogen molecules in overcoming the activation energy barriers, and in transferring energy to the iron oxide, is emphasized. Both thermal and nonthermal plasmas are considered. The thermophysical properties of hydrogen and argon-hydrogen plasmas are discussed, and their influence on the constriction and flow in the of arc plasmas is considered. The published R&D on hydrogen plasma reduction of iron oxide is reviewed, with both the reduction of molten iron ore and in-flight reduction of iron ore particles being considered. Finally, the technical and economic feasibility of the process are discussed. It is shown that hydrogen plasma processing requires less energy than carbothermic reduction, mainly because pelletization, sintering, and cokemaking are not required. Moreover, the formation of the greenhouse gas CO2 as a byproduct is avoided. In-flight reduction has the potential for a throughput at least equivalent to the blast furnace process. It is concluded that hydrogen plasma reduction of iron ore is a potentially attractive alternative to standard methods.

High coercivity, anisotropic, heavy rare earth-free Nd-Fe-B by Flash Spark Plasma Sintering.

Science.gov (United States)

Castle, Elinor; Sheridan, Richard; Zhou, Wei; Grasso, Salvatore; Walton, Allan; Reece, Michael J

2017-09-11

In the drive to reduce the critical Heavy Rare Earth (HRE) content of magnets for green technologies, HRE-free Nd-Fe-B has become an attractive option. HRE is added to Nd-Fe-B to enhance the high temperature performance of the magnets. To produce similar high temperature properties without HRE, a crystallographically textured nanoscale grain structure is ideal; and this conventionally requires expensive "die upset" processing routes. Here, a Flash Spark Plasma Sintering (FSPS) process has been applied to a Dy-free Nd 30.0 Fe 61.8 Co 5.8 Ga 0.6 Al 0.1 B 0.9 melt spun powder (MQU-F, neo Magnequench). Rapid sinter-forging of a green compact to near theoretical density was achieved during the 10 s process, and therefore represents a quick and efficient means of producing die-upset Nd-Fe-B material. The microstructure of the FSPS samples was investigated by SEM and TEM imaging, and the observations were used to guide the optimisation of the process. The most optimal sample is compared directly to commercially die-upset forged (MQIII-F) material made from the same MQU-F powder. It is shown that the grain size of the FSPS material is halved in comparison to the MQIII-F material, leading to a 14% increase in coercivity (1438 kA m -1 ) and matched remanence (1.16 T) giving a BH max of 230 kJ m -3 .

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

Science.gov (United States)

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

Processing and Properties of Distaloy Sa Sintered Alloys with Boron and Carbon

Directory of Open Access Journals (Sweden)

Karwan-Baczewska J.

2015-04-01

Full Text Available Prealloyed iron-based powders, manufactured in Höganäs Company, are used in the automotive parts industry. The properties and life time of such sintered parts depend, first of all, on their chemical composition, the production method of the prealloyed powder as well as on the technology of their consolidation and sintering. One of simpler and conventional methods aimed at increasing the density in sintered products is the process of activated sintering, performed, for example, by adding boron as elementary boron powder. Under this research project obtained were novel sintered materials, based on prealloyed and diffusion bonded powder, type: Distaloy SA, with the following chemical composition: Fe-1.75% Ni-1.5%Cu- 0.5%Mo with carbon (0.55%; 0.75% and boron (0.2%, 0.4% and 0.6%. Distaloy SA samples alloyed with carbon and boron were manufactured by mixing powders in a Turbula mixer, then compressed using a hydraulic press under a pressure of 600 MPa and sintered in a tube furnace at 1473 K, for a 60 minute time, in the hydrogen atmosphere. After the sintering process, there were performed density and porosity measurements as well as hardness tests and mechanical properties were carried out, too. Eventually, analyzed was the effect of boron upon density, hardness and mechanical properties of novel sintered construction parts made from Distaloy SA powder.

The effect of sintering conditions and ZrN volume fraction on the mechanical properties of spark plasma sintered W/ZrN composites

International Nuclear Information System (INIS)

Lee, Dongju; Umer, Malik Adeel; Shin, Yoochul; Jeon, Seokwoo; Hong, Soonhyung

2012-01-01

Highlights: ► Effect of sintering conditions on properties of W composites was investigated. ► Effect of ZrN volume fraction on properties of W composites was investigated. ► The grain size and relative density increased with increasing sintering temperature. ► ZrN particles led to an increase in strength of W and a decrease in grain size. ► Highest flexural strength was obtained for 10 vol.% W/ZrN with lowest agglomeration. - Abstract: In an effort to improve the room temperature mechanical properties of tungsten, W/ZrN composites were fabricated by high energy ball milling followed by spark plasma sintering at temperatures in a range of 1200–1700 °C under a pressure of 50 MPa. The effects of sintering conditions and ZrN volume fraction on the mechanical properties of the W/ZrN composites were studied and the results were compared to the properties of monolithic tungsten. The grain size of monolith tungsten and W/ZrN composites was found to increase with an increase in sintering temperature and time. In the case of the W/ZrN composites, ZrN particles led to an increase in the compressive strength of tungsten and a decrease in grain size. The increase in compressive strength of the composites was attributed to a reinforcement effect of ZrN particles as well as grain size refinement according to the Hall–Petch relation. Compressive strength of the composites increased with increasing ZrN content while the flexural strength decreased for samples with ZrN content exceeding 10 vol.%. This was attributed to the effects of ZrN agglomeration within the tungsten matrix.

On the Role of the Electrical Field in Spark Plasma Sintering of UO2+x

Science.gov (United States)

Tyrpekl, Vaclav; Naji, Mohamed; Holzhäuser, Michael; Freis, Daniel; Prieur, Damien; Martin, Philippe; Cremer, Bert; Murray-Farthing, Mairead; Cologna, Marco

2017-01-01

The electric field has a large effect on the stoichiometry and grain growth of UO2+x during Spark Plasma Sintering. UO2+x is gradually reduced to UO2.00 as a function of sintering temperature and time. A gradient in the oxidation state within the pellets is observed in intermediate conditions. The shape of the gradient depends unequivocally on the direction of the electrical field. The positive surface of the pellet shows a higher oxidation state compared to the negative one. An area with larger grain size is found close to the positive electrode, but not in contact with it. We interpret these findings with the redistribution of defects under an electric field, which affect the stoichiometry of UO2+x and thus the cation diffusivity. The results bear implications for understanding the electric field assisted sintering of UO2 and non-stoichiometric oxides in general. PMID:28422164

Microstructure and phase stability of W-Cr alloy prepared by spark plasma sintering

Czech Academy of Sciences Publication Activity Database

Vilémová, Monika; Illková, Ksenia; Lukáč, František; Matějíček, Jiří; Klečka, Jakub; Leitner, J.

2018-01-01

Roč. 127, February (2018), s. 173-178 ISSN 0920-3796 R&D Projects: GA ČR(CZ) GA17-23964S Institutional support: RVO:61389021 Keywords : Tungsten-chromium alloy * Phase stability * Decomposition * Thermal conductivity * Self-passivating alloys * Spark plasma sintering Subject RIV: JJ - Other Materials OBOR OECD: Materials engineering Impact factor: 1.319, year: 2016 https://www.sciencedirect.com/science/article/pii/S092037961830005X

Spark Plasma Sintering of a Gas Atomized Al7075 Alloy: Microstructure and Properties

Czech Academy of Sciences Publication Activity Database

Molnárová, O.; Málek, P.; Lukáč, František; Chráska, Tomáš

2016-01-01

Roč. 9, č. 12 (2016), č. článku 1004. ISSN 1996-1944 R&D Projects: GA ČR(CZ) GA15-15609S Institutional support: RVO:61389021 Keywords : gas atomized Al7075 alloy * spark plasma sintering * microstructure * microhardness * high temperature stability Subject RIV: JJ - Other Materials Impact factor: 2.654, year: 2016 http://www.mdpi.com/1996-1944/9/12/1004

Dynamic Fracture Toughness of TaC/CNTs/SiC CMCs Prepared by Spark Plasma Sintering

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Qiaoyun Xie

2015-01-01

Full Text Available This study focuses on the fracture toughness of TaC and carbon nanotubes (CNTs reinforced SiC ceramic matrix composites (CMCs, prepared by spark plasma sintering (SPS technique. A high densification of 98.4% was achieved under the sintering parameter of 133°C/min, 1800°C, and 90 MPa pressure. Vickers indentation was employed to measure the indentation toughness on the polished surface of ceramic samples, SEM was applied to directly observe the crack propagation after indentation, and split Hopkinson pressure bar (SHPB was developed to determine the dynamic fracture toughness within the ceramic samples subjected to an impact in a three-point bending configuration.

High-strength bulk nano-crystalline silver prepared by selective leaching combined with spark plasma sintering

Czech Academy of Sciences Publication Activity Database

Marek, I.; Vojtěch, D.; Michalcová, A.; Kubatík, Tomáš František

2015-01-01

Roč. 627, March (2015), s. 326-332 ISSN 0921-5093 Institutional support: RVO:61389021 Keywords : Nano-crystalline material * Selective leaching * Silver * Spark plasma sintering * Strength Subject RIV: JK - Corrosion ; Surface Treatment of Materials Impact factor: 2.647, year: 2015 http://dx.doi.org/10.1016/j.msea.2015.01.014

High Temperature Oxidation of Spark Plasma Sintered and Thermally Sprayed FeAl-Based Iron Aluminides

Czech Academy of Sciences Publication Activity Database

Haušild, P.; Karlík, M.; Skiba, T.; Sajdl, P.; Dubský, Jiří; Palm, M.

2012-01-01

Roč. 122, č. 3 (2012), s. 465-468 ISSN 0587-4246. [International Symposium on Physics of Materials (ISPMA)/12./. Prague, 04.09.2011-08.09.2011] Institutional support: RVO:61389021 Keywords : thermal spraying * plasma sintering Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass Impact factor: 0.531, year: 2012

Spark Plasma Sintering of Dielectric Ceramics Zr0.8Sn0.2TiO4

Czech Academy of Sciences Publication Activity Database

Ctibor, P.; Kubatík, Tomáš František; Sedláček, J.; Kotlan, Jiří

2016-01-01

Roč. 22, č. 3 (2016), s. 435-439 ISSN 1392-1320 Institutional support: RVO:61389021 Keywords : titanates * dielectric ceramics * spark plasma sintering Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass Impact factor: 0.393, year: 2016 http://www.matsc.ktu.lt/index.php/MatSc/article/view/8767

Data on the impact of increasing the W amount on the mass density and compressive properties of Ni-W alloys processed by spark plasma sintering.

Science.gov (United States)

Sadat, T; Hocini, A; Lilensten, L; Faurie, D; Tingaud, D; Dirras, G

2016-06-01

Bulk Ni-W alloys having composite-like microstructures are processed by spark plasma sintering (SPS) route of Ni and W powder blends as reported in a recent study of Sadat et al. (2016) (DOI of original article: doi:10.1016/j.matdes.2015.10.083) [1]. The present dataset deals with determination of mass density and evaluation of room temperature compressive mechanical properties as function of the amount of W (%wt. basis). The presented data concern: (i) measurement of the mass of each investigated Ni-W alloy which is subsequently used to compute the mass density of the alloy and (ii) the raw (stress (MPa) and strain ([Formula: see text])) data, which can be subsequently used for stress/ strain plots.

Magnetic and structural properties of spark plasma sintered nanocrystalline NdFeB-powders

Energy Technology Data Exchange (ETDEWEB)

Wuest, H., E-mail: holger.wuest@de.bosch.com [Robert Bosch GmbH, Postfach 10 60 50, 70049 Stuttgart (Germany); Bommer, L., E-mail: lars.bommer@de.bosch.com [Robert Bosch GmbH, Postfach 10 60 50, 70049 Stuttgart (Germany); Weissgaerber, T., E-mail: thomas.weissgaerber@ifam-dd.fraunhofer.de [Fraunhofer Institute for Manufacturing Technology and Advanced Materials (IFAM), Branch Lab Dresden, Winterbergstraße 28, 01277 Dresden (Germany); Kieback, B., E-mail: bernd.kieback@ifam-dd.fraunhofer.de [Fraunhofer Institute for Manufacturing Technology and Advanced Materials (IFAM), Branch Lab Dresden, Winterbergstraße 28, 01277 Dresden (Germany); Technische Universität Dresden, Institute for Materials Science, Helmholtzstraße 7, 01069 Dresden (Germany)

2015-10-15

Near-stoichiometric NdFeB melt-spun ribbons have been subjected to spark plasma sintering varying the process temperature T{sub SPS} and pressure p{sub SPS} between 600 and 800 °C and 50–300 MPa, respectively. Produced bulk magnets were analyzed regarding microstructure and magnetic properties. For all samples the intrinsic coercivity H{sub c,J} gradually decreases with increasing sintering temperature and pressure, while residual induction B{sub r} increases simultaneously with sample density. Densities close to the theoretical limit were achieved for p{sub SPS}≥90 MPa and T{sub SPS}≥650 °C. With increasing T{sub SPS} precipitations of Nd-rich and Fe-rich phases have been observed as a result of a decomposition of the hard magnetic Nd{sub 2}Fe{sub 14}B phase. Under optimum sintering conditions of p{sub SPS}=300 MPa and T{sub SPS}=650 °C high-density bulk magnets with H{sub c,J}=652 kA/m, B{sub r}=0.86 T and (BH){sub max}=106 kJ/m{sup 3} have been produced. - Highlights: • Consolidation close to the theoretical density for p{sub SPS}≥90 MPa and T{sub SPS}≥650 °C. • Highest (BH){sub max} of 106 kJ/m{sup 3} for p{sub SPS}=300 MPa and T{sub SPS}=650 °C with 98% theo. • H{sub c,J} gradually decreases with increasing T{sub SPS}, while B{sub r} increases simultaneously with. • With increasing T{sub SPS}, Nd- and Fe-rich precipitations are observed. • Reduction in t{sub SPS} is economic but does not increase (BH){sub max} significantly.

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

Science.gov (United States)

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.

Liquid Film Capillary Mechanism for Densification of Ceramic Powders during Flash Sintering

Directory of Open Access Journals (Sweden)

Rachman Chaim

2016-04-01

Full Text Available Recently, local melting of the particle surfaces confirmed the formation of spark and plasma during spark plasma sintering, which explains the rapid densification mechanism via liquid. A model for rapid densification of flash sintered ceramics by liquid film capillary was presented, where liquid film forms by local melting at the particle contacts, due to Joule heating followed by thermal runaway. Local densification is by particle rearrangement led by spreading of the liquid, due to local attractive capillary forces. Electrowetting may assist this process. The asymmetric nature of the powder compact represents an invasive percolating system.

Effect of sintering process parameters on the properties of 3Y-PSZ ceramics

International Nuclear Information System (INIS)

Chu, H L; Chen, R S; Wang, C L; Hwang, W S; Lee, H E; Sie, Y Y; Wang, M C

2013-01-01

The effect of sintering process parameters on the properties of 3 mol% yttria partially stability zirconia (3Y-PSZ) ceramics has been investigated. The relative density of the sintered pellet rapidly increases from 70.5 to 93.6% with rose temperature from 1473 to 1573 K. In addition, the relative density only slightly increases from 94.9 to 96.6 %, when rose sintered temperature from 1573 to 1773 K. This result shows that no significant influence on the densification behavior when sintering at 1573 to 1773 K for 2 h. The Vickers hardness and toughness also increase with the sintered temperature

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

Science.gov (United States)

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

2015-10-01

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

Effect of spark plasma sintering conditions on the thermoelectric properties of (Bi{sub 0.25}Sb{sub 0.75}){sub 2}Te{sub 3} alloys

Energy Technology Data Exchange (ETDEWEB)

Lim, Sang-Soon [Center for Electronic Materials, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); Department of Materials Science and Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of); Kim, Ju-Heon [High Temp. Energy Materials Research Center, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); Kwon, Beomjin; Kim, Seong Keun [Center for Electronic Materials, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); Park, Hyung-Ho [Department of Materials Science and Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of); Lee, Ki-Suk; Baik, Jeong Min [School of Materials and Science Engineering, UNIST, Ulsan 689-798 (Korea, Republic of); KIST-UNIST Ulsan Center for Convergent Materials, UNIST, Ulsan 689-798 (Korea, Republic of); Choi, Won Jun [Center for Opto-Electronic Materials and Devices, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); Kim, Dong-Ik [High Temp. Energy Materials Research Center, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); Hyun, Dow-Bin; Kim, Jin-Sang [Center for Electronic Materials, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); Baek, Seung-Hyub, E-mail: shbaek77@kist.re.kr [Center for Electronic Materials, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); KIST-UNIST Ulsan Center for Convergent Materials, UNIST, Ulsan 689-798 (Korea, Republic of); Department of Nanomaterials Science and Technology, Korea University of Science and Technology, Daejeon, 305-333 (Korea, Republic of)

2016-09-05

As a field-assisted technique, spark plasma sintering (SPS) enables densification of specimens in a very short period of time compared to other sintering techniques. For high performance thermoelectric material synthesis, SPS is widely used to fabricate nanograin-structured thermoelectric materials by rapidly densifying the nanopowders suppressing grain growth. However, the microstructural evolution behavior of thermoelectric materials by SPS, another important process during sintering, has been rarely studied. Here, we explore SPS as a tool to control the microstructure by long-time SPS. Using p-type (Bi{sub 0.25}Sb{sub 0.75}){sub 2}Te{sub 3} thermoelectric materials as a model system, we systematically vary SPS temperature and time to understand the correlations between SPS conditions, microstructural evolution, and the thermoelectric properties. Our results show that the relatively low eutectic temperature (∼420 °C) and the existence of volatile tellurium (Te) are critical factors to determine both microstructure and thermoelectric property. In the liquid-phase sintering regime, rapid evaporation of Te leads to a strong dependence of thermoelectric property on SPS time. On the other hand, in the solid-phase sintering regime, there is a weak dependence on SPS time. The optimum thermoelectric figure-of-merit (Z) of 2.93 × 10{sup −3}/K is achieved by SPS at 500 °C for 30 min. Our results will provide an insight on the optimization of SPS conditions for materials containing volatile elements with low eutectic temperature. - Highlights: • Spark plasma sintering (SPS) is used to synthesize the thermoelectric (Bi{sub 0.25}Sb{sub 0.75}){sub 2}Te{sub 3}. • Liquid phase and volatile element are a key for the microstructure and thermoelectric property. • Thermoelectric figure-of-merit of 2.9 × 10{sup −3}/K is achieved at 500 °C for 30 min.

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

Energy Technology Data Exchange (ETDEWEB)

Tyrpekl, V., E-mail: vaclav.tyrpekl@ec.europa.eu, E-mail: vaclav.tyrpekl@gmail.com; Berkmann, C.; Holzhäuser, M.; Köpp, F.; Cologna, M.; Somers, J. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, 76125 Karlsruhe (Germany); Wangle, T. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, 76125 Karlsruhe (Germany); Faculty of Nuclear Sciences and Physical Engineering, Czech Technical University in Prague, Břehová 7, Praha 1, 115 19 (Czech Republic)

2015-02-15

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

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

Science.gov (United States)

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.

Phase Evolution and Mechanical Properties of AlCoCrFeNiSi x High-Entropy Alloys Synthesized by Mechanical Alloying and Spark Plasma Sintering

Science.gov (United States)

Kumar, Anil; Swarnakar, Akhilesh Kumar; Chopkar, Manoj

2018-05-01

In the current investigation, AlCoCrFeNiSi x (x = 0, 0.3, 0.6 and 0.9 in atomic ratio) high-entropy alloy systems are prepared by mechanical alloying and subsequently consolidated by spark plasma sintering. The microstructural and mechanical properties were analyzed to understand the effect of Si addition in AlCoCrFeNi alloy. The x-ray diffraction analysis reveals the supersaturated solid solution of the body-centered cubic structure after 20 h of ball milling. However, the consolidation promotes the transformation of body-centered phases partially into the face-centered cubic structure and sigma phases. A recently proposed geometric model based on the atomic stress theory has been extended for the first time to classify single phase and multi-phases on the high-entropy alloys prepared by mechanical alloying and spark plasma sintering process. Improved microhardness and better wear resistance were achieved as the Si content increased from 0 to 0.9 in the present high-entropy alloy.

Microstructure and mechanical behavior of ODS and non-ODS Fe–14Cr model alloys produced by spark plasma sintering

International Nuclear Information System (INIS)

Auger, M.A.; Castro, V. de; Leguey, T.; Muñoz, A.; Pareja, R.

2013-01-01

In this work the spark plasma sintering (SPS) technique has been explored as an alternative consolidation route for producing ultra-fine grained Fe–14Cr model alloys containing a dispersion of oxide nanoparticles. Elemental powders of Fe and Cr, and nanosized Y 2 O 3 powder have been mechanically alloyed in a planetary ball mill and rapidly sintered in a spark plasma furnace. Two alloys, with nominal compositions Fe–14%Cr and Fe–14%Cr–0.3%Y 2 O 3 (wt.%), have been fabricated and their microstructure and mechanical properties investigated. The results have been compared with those obtained for other powder metallurgy processed alloys of the same composition but consolidated by hot isostatic pressing. The SPS technique under the present conditions has produced Fe–14Cr materials that apparently exhibit different microstructures yielding inferior mechanical properties than the counterpart material consolidated by hot isostatic pressing. Although the presence of a dispersion of Y-rich particles is evident, the oxide dispersion strengthened (ODS) Fe–14Cr alloy consolidated by SPS exhibits poor tensile properties. The extensive decoration of the powder particle surfaces with Cr-rich precipitates and the residual porosity appear to be responsible for the impaired properties of this ODS alloy consolidated by SPS

Microstructure and mechanical behavior of ODS and non-ODS Fe–14Cr model alloys produced by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Auger, M.A.; Castro, V. de [Departamento de Física, Universidad Carlos III de Madrid, 28911 Leganés (Spain); Leguey, T., E-mail: leguey@fis.uc3m.es [Departamento de Física, Universidad Carlos III de Madrid, 28911 Leganés (Spain); Muñoz, A.; Pareja, R. [Departamento de Física, Universidad Carlos III de Madrid, 28911 Leganés (Spain)

2013-05-15

In this work the spark plasma sintering (SPS) technique has been explored as an alternative consolidation route for producing ultra-fine grained Fe–14Cr model alloys containing a dispersion of oxide nanoparticles. Elemental powders of Fe and Cr, and nanosized Y{sub 2}O{sub 3} powder have been mechanically alloyed in a planetary ball mill and rapidly sintered in a spark plasma furnace. Two alloys, with nominal compositions Fe–14%Cr and Fe–14%Cr–0.3%Y{sub 2}O{sub 3} (wt.%), have been fabricated and their microstructure and mechanical properties investigated. The results have been compared with those obtained for other powder metallurgy processed alloys of the same composition but consolidated by hot isostatic pressing. The SPS technique under the present conditions has produced Fe–14Cr materials that apparently exhibit different microstructures yielding inferior mechanical properties than the counterpart material consolidated by hot isostatic pressing. Although the presence of a dispersion of Y-rich particles is evident, the oxide dispersion strengthened (ODS) Fe–14Cr alloy consolidated by SPS exhibits poor tensile properties. The extensive decoration of the powder particle surfaces with Cr-rich precipitates and the residual porosity appear to be responsible for the impaired properties of this ODS alloy consolidated by SPS.

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

Science.gov (United States)

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.

Comparison of Reactive and Non-Reactive Spark Plasma Sintering Routes for the Fabrication of Monolithic and Composite Ultra High Temperature Ceramics (UHTC Materials

Directory of Open Access Journals (Sweden)

Roberto Orrù

2013-04-01

Full Text Available A wider utilization of ultra high temperature ceramics (UHTC materials strongly depends on the availability of efficient techniques for their fabrication as dense bodies. Based on recent results reported in the literature, it is possible to state that Spark Plasma Sintering (SPS technology offers a useful contribution in this direction. Along these lines, the use of two different SPS-based processing routes for the preparation of massive UHTCs is examined in this work. One method, the so-called reactive SPS (R-SPS, consists of the synthesis and densification of the material in a single step. Alternatively, the ceramic powders are first synthesized by Self-propagating High-temperature Synthesis (SHS and then sintered by SPS. The obtained results evidenced that R-SPS method is preferable for the preparation of dense monolithic products, while the sintering of SHS powders requires relatively milder conditions when considering binary composites. The different kinetic mechanisms involved during R-SPS of the monolithic and composite systems, i.e., combustion-like or gradual solid-diffusion, respectively, provides a possible explanation. An important role is also played by the SHS process, particularly for the preparation of composite powders, since stronger interfaces are established between the ceramic constituents formed in situ, thus favoring diffusion processes during the subsequent SPS step.

Improvement of the mechanical properties of spark plasma sintered hap bioceramics by decreasing the grain size and by adding multi-walled carbon nanotubes

Directory of Open Access Journals (Sweden)

Veljović Đ.

2013-01-01

Full Text Available Composites based on HAP and oxidized multi-walled carbon nanotubes (o-MWCNT and monophase HAP materials were processed by spark plasma sintering. Starting from stoichiometric nano-sized HAP powder, monophase bioceramics were obtained with a density close to the theoretical one and with an average grain size of several hundred nanometers to micron dimensions. It was shown that decreasing the sintering temperature resulted in a decrease of the grain size, which affected an increase in the fracture toughness and hardness. The fracture toughness of an HAP/ o-MWCNT bioceramic processed at 900°C for only 5 min was 30 % higher than that of monophase HAP materials obtained under the same conditions. The addition of MWCNT during SPS processing of HAP materials caused a decrease in the grain size to the nano-dimension, which was one of the reasons for the improved mechanical properties. [Projekat Ministarstva nauke Republike Srbije, br. III45019 i FP7-REGPOT-2009-1 NANOTECH FTM, Grant Agreement Number: 245916

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

Science.gov (United States)

Sagar, M. B.; Elangovan, K.

2017-08-01

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

Liquid phase sintered SiC. Processing and transformation controlled microstructure tailoring

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V.A. Izhevskyi

2000-10-01

Full Text Available Microstructure development and phase formation processes during sintering of silicon carbide based materials with AlN-Y2O3, AlN-Yb2O3, and AlN-La2O3 sintering additives were investigated. Densification of the materials occurred by liquid-phase sintering mechanism. Proportion of alpha- and beta-SiC powders in the initial mixtures was a variable parameter, while the molar ratio of AlN/RE2O3, and the total amount of additives (10 vol. % were kept constant. Shrinkage behavior during sintering in interrelation with the starting composition of the material and the sintering atmosphere was investigated by high temperature dilatometry. Kinetics of b-SiC to a-SiC phase transformation during post-sintering heat treatment at temperatures 1900-1950 °C was studied, the degree of phase transformation being determined by quantitative x-ray analysis using internal standard technique. Evolution of microstructure resulting from beta-SiC to alpha-SiC transformation was followed up by scanning electron microscopy on polished and chemically etched samples. Transformation-controlled grain growth mechanism similar to the one observed for silicon nitride based ceramics was established. Possibility of in-situ platelet reinforced dense SiC-based ceramics fabrication with improved mechanical properties by means of sintering was shown.

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

Science.gov (United States)

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

2018-01-01

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

Sintering behavior of porous wall tile bodies during fast single-firing process

Directory of Open Access Journals (Sweden)

Sidnei José Gomes Sousa

2005-06-01

Full Text Available In ceramic wall tile processing, fast single-firing cycles have been widely used. In this investigation a fast single-firing porous wall tile mixture was prepared using raw materials from the North Fluminense region.Specimens were obtained by uniaxial pressing and sintered in air at various temperatures (1080 - 1200 °C using a fast-firing cycle (60 minutes. Evolution of the microstructure was followed by XRD and SEM. The results revealed that the main phases formed during the sintering step are anorthite, gehlenite and hematite. It appears that the sintering process is characterized by the presence of a small amount of a liquid phase below 1140 °C. As a result, the microstructure of the ceramic bodies showed a network of small dense zones interconnected with a porous phase. In addition, the strength of the material below 1140 °C appeared to be related to the type and quantity of crystalline phases in the sintered bodies.

Preparation and Characterization of TiB2-(Supra-Nano-Dual-Phase High-Entropy Alloy Cermet by Spark Plasma Sintering

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Shulei Zhang

2018-01-01

Full Text Available This paper introduces the preparation method and characterization results of TiB2 ceramics with CoCrFeNiAl high-entropy alloy (HEA as a sintering aid by Spark Plasma Sintering (SPS. Good wettability between HEA and TiB2 was proved by the sessile drop method, indicating promising prospects for this composite. The sintering results showed that the addition of HEA could dramatically promote the sinterability of TiB2. TiB2-5 wt. % HEA dense ceramics prepared at the optimal temperature of 1650 °C showed fine morphology without formation of brittle phases. The liquid phase in the ceramics was highly consistent with the so-called “supra-nano-dual-phase materials (SNDPM”, with near-ideal strength. This study represents the first time that a ceramic-SNDPM composite has been fabricated since the invention of such structures.

Basic study of Eu.sup.2+./sup.-doped garnet ceramic scintillator produced by spark plasma sintering

Czech Academy of Sciences Publication Activity Database

Sugiyama, K.; Yanagida, T.; Fujimoto, Y.; Yokota, Y.; Ito, A.; Nikl, Martin; Goto, T.; Yoshikawa, A.

2012-01-01

Roč. 35, č. 2 (2012), s. 222-226 ISSN 0925-3467 R&D Projects: GA MŠk LH12150 Institutional research plan: CEZ:AV0Z10100521 Keywords : Eu 2+ 5d–4f transition * scintillator * spark plasma sintering Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.918, year: 2012

Processing and properties of mechanically alloyed sintered steels with hard inclusions

International Nuclear Information System (INIS)

Gutsfeld, C.

1991-10-01

The aim of this work was the development of mechanically alloyed sintered steels with inert hard inclusions and their characterisation concerning the mechanical properties and the sliding wear behaviour. For this material concept the hard materials NbC, TiC, TiN and Al 2 O 3 were chosen with volume contents upto 20%. Mechanical alloying of the raw powders is a necessary prerequisit for an extreme fine and homogeneous microstructure and good mechanical and wear properties. Through a connecting powder annealing a conventional powder metallurgical processing with cold pressing and sintering is possible. For the consolidation pressureless liquid phase sintering initiated through phosphorus contents of 0,6% is suitable. Because of the strong hampering of grain growth through the included hard particles sintering densities upto 99% TD are possible with extreme fine microstructures. The mechanical properties can be varied in wide ranges. So tensile strengths of 1150 MPa, elongations at fracture of 17%, hardness of over 800 HV and fatigue strengths of 370 MPa have been reached. Throughout HIP or sinter forging the mechanical properties can be improved furthermore. (orig.) [de

Effect of process parameters on surface oxides on chromium-alloyed steel powder during sintering

International Nuclear Information System (INIS)

Chasoglou, D.; Hryha, E.; Nyborg, L.

2013-01-01

The use of chromium in the PM steel industry today puts high demands on the choice and control of the atmosphere during the sintering process due to its high affinity to oxygen. Particular attention is required in order to control the surface chemistry of the powder which in turn is the key factor for the successful sintering and production of PM parts. Different atmosphere compositions, heating rates and green densities were employed while performing sintering trials on water atomized steel powder pre-alloyed with 3 wt.% Cr in order to evaluate the effect on surface chemical reactions. Fracture surfaces of sintered samples were examined using high resolution scanning electron microscopy combined with X-ray microanalysis. The investigation was complemented with thermogravimetric (TG) studies. Reaction products in particulate form containing strong-oxide forming elements such as Cr, Si and Mn were formed during sintering for all conditions. Processing in vacuum results in intensive inter-particle neck development during the heating stage and consequently in the excessive enclosure of surface oxide which is reflected in less good final mechanical properties. Enhanced oxide reduction was observed in samples processed in hydrogen-containing atmospheres independent of the actual content in the range of 3–10 vol.%. An optimum heating rate was required for balancing reduction/oxidation processes. A simple model for the enclosure and growth of oxide inclusions during the sinter-neck development is proposed. The obtained results show that significant reduction of the oxygen content can be achieved by adjusting the atmosphere purity/composition. - Highlights: ► A local atmosphere microclimate is very important for sintering of PM steels. ► High risk of surface oxide enclosure between 800 and 1000 °C. ► Coalescence and agglomeration of enclosed oxides take place during sintering. ► The effect of different process parameters on the oxide reduction is examined. ► A

The influence of green microstructure and sintering parameters on precipitation process during copper-nickel-zinc ferrites sintering

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Barba, Antonio

2014-04-01

Full Text Available Microstructural changes that occur during heat treatment of copper-nickel-zinc ferrites have been studied. The process of precipitation of the two types of crystals that occur during the sintering process has been analyzed. It is found that this process depends on dry relative density of the press specimens and on the following sintering parameters: sintering temperature, sintering time and cooling rate of the thermal cycle. Crystal precipitates characterization have been done by scanning electron microscopy (SEM, energy-dispersive X-ray (EDX analysis, X-ray diffraction (XRD, and X-ray photoelectron spectroscopy (XPS. These techniques have allowed to determine the nature of these crystals, which in this case correspond to zinc and copper oxides. It has been used two chemical reactions to explain the bulk precipitation and subsequent re-dissolution of these crystal precipitates during sintering.En este trabajo se han estudiado los cambios microestructurales que se producen durante el tratamiento térmico de las ferritas de cobre-níquel-cinc y se ha analizado el proceso de precipitación de los dos tipos de cristales que aparecen durante el proceso de sinterización. Se ha encontrado que este proceso depende de la densidad relativa en seco de las muestras compactadas y de las siguientes variables de la etapa de sinterización: temperatura y tiempo de sinterización y velocidad de enfriamiento. La caracterización de los cristales precipitados se ha realizado por microscopía electrónica de barrido (MEB, microanálisis por dispersión de energía de rayos X (EDX, difracción de rayos X (DRX, y espectroscopía de fotoelectrones de rayos X (XPS. Estas técnicas han permitido determinar la naturaleza de estos cristales, que en este caso corresponden a los óxidos de cinc y de cobre. Se han propuesto dos reacciones químicas que permiten explicar el proceso de precipitación y la posterior re-disolución de estos cristales precipitados durante la

Material Evaluation and Process Optimization of CNT-Coated Polymer Powders for Selective Laser Sintering

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Shangqin Yuan

2016-10-01

Full Text Available Multi-walled carbon nanotubes (CNTs as nano-reinforcements were introduced to facilitate the laser sintering process and enhance the thermal and mechanical properties of polymeric composites. A dual experimental-theoretical method was proposed to evaluate the processability and predict the process parameters of newly developed CNT-coated polyamide 12 (CNTs/PA12 powders. The thermal conductivity, melt viscosity, phase transition and temperature-dependent density and heat capacity of PA12 and CNTs/PA12 powders were characterized for material evaluation. The composite powders exhibited improved heat conduction and heat absorption compared with virgin polymer powders, and the stable sintering range of composite powders was extended and found to be favourable for the sintering process. The microstructures of sintered composites revealed that the CNTs remained at the powder boundaries and formed network architectures, which instantaneously induced the significant enhancements in tensile strength, elongation at break and toughness without sacrificing tensile modulus.

Study of distribution of Carbon nanotube in Al-CNT nanocomposite synthesized via Spark-Plasma sintering

Science.gov (United States)

Maiti, A.; Laha, T.

2018-03-01

In the present study, first ever attempt has been made to develop physically functionalized multiwalled carbon nanotube (MWCNT) reinforced Al-11 5Si alloy nanocomposites synthesized via novel consolidation technique viz spark plasma sintering (SPS). There is a recent trend in employing carbon nanotubes (CNTs), an allotrope of carbon, as reinforcement for high strength structural metallic composite materials, as these cylindrical nano-fibers poses extremely unique mechanical properties such as very high elastic modulus (~ 300 GPa to 1.5 TPa) as well as tensile strength (~150 GPa). However, it has remained as an ever-existing problem to achieve a porosity-free nanocrystalline matrix with homogenously dispersed CNTs, owing to the very high coagulation tendency of CNTs. The gas-atomized, spherical Al-11.5Si alloy powders (1-8 μm) were subjected to high energy ball milling for the purpose of achieving nanocrystallinity in the powders. The improvement in MWCNT dispersion was effort by treating the MWCNTs with a physical surfactant, sodium dodecyl sulfate (SDS). The nano-grained ball-milled Al-Si powders with varying MWCNT content (0.5 and 1 wt%) were consolidated via spark plasma sintering in order to retain the nano-sized grains in the Al-Si matrix, attributed to the faster and highly effective sintering kinetics of the sintering techniques. FESEM study shows problem of MWCNT agglomeration persists by addition of non-SDS treated as pristine MWCNT in the composite. After treated with SDS, MWCNTs are well separated out from each other and as a result of that good morphological and mechanical property such as high hardness value obtained after analysis. Detailed TEM study of the 0.5wt% MWCNT reinforced SPS nanocomposite revealed that the distribution of CNTs in the matrix. Mechanical analysis study of the nanocomposite attributes higher hardness in case of SDS treated CNT reinforced nanocomposite owing to less agglomeration problem of the CNT in the matrix. Nano

Science of sintering

International Nuclear Information System (INIS)

Kuczynski, G.

1977-01-01

Although the methods of integration of materials by sintering, have been used since the early history of humanity, the actual understanding of the process involved came only in the last three decades. As in the most human endeavors, the art preceded theory. The comprehension of the elementary processes occuring during sintering comes from the studies of model system. Although the elementary processes occuring during sintering are today quite well understood, the problem of shrinkage of a powder compact which was at the origin of Sintering Science is still far from solved. This is due to the complexity of the internal geometry of the compacts. The recent attempts to apply statistics to this problem, seem to offer some promise

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

Science.gov (United States)

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

2017-04-01

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

Nanocrystalline Al7075+1 wt % Zr Alloy Prepared Using Mechanical Milling and Spark Plasma Sintering.

Czech Academy of Sciences Publication Activity Database

Molnárová, O.; Málek, P.; Veselý, J.; Šlapáková, M.; Minárik, P.; Lukáč, František; Chráska, Tomáš; Novák, P.; Průša, F.

2017-01-01

Roč. 10, č. 9 (2017), č. článku 1105. ISSN 1996-1944 R&D Projects: GA ČR(CZ) GA15-15609S Institutional support: RVO:61389021 Keywords : gas atomization * mechanical milling * spark plasma sintering * microstructure * microhardness * recrystallization Subject RIV: JG - Metallurgy OBOR OECD: Materials engineering Impact factor: 2.654, year: 2016 http://www.readcube.com/articles/10.3390/ma10091105

In situ process monitoring in selective laser sintering using optical coherence tomography

Science.gov (United States)

Gardner, Michael R.; Lewis, Adam; Park, Jongwan; McElroy, Austin B.; Estrada, Arnold D.; Fish, Scott; Beaman, Joseph J.; Milner, Thomas E.

2018-04-01

Selective laser sintering (SLS) is an efficient process in additive manufacturing that enables rapid part production from computer-based designs. However, SLS is limited by its notable lack of in situ process monitoring when compared with other manufacturing processes. We report the incorporation of optical coherence tomography (OCT) into an SLS system in detail and demonstrate access to surface and subsurface features. Video frame rate cross-sectional imaging reveals areas of sintering uniformity and areas of excessive heat error with high temporal resolution. We propose a set of image processing techniques for SLS process monitoring with OCT and report the limitations and obstacles for further OCT integration with SLS systems.

Spark-plasma-sintering magnetic field assisted compaction of Co{sub 80}Ni{sub 20} nanowires for anisotropic ferromagnetic bulk materials

Energy Technology Data Exchange (ETDEWEB)

Ouar, Nassima; Schoenstein, Frédéric; Mercone, Silvana; Farhat, Samir; Jouini, Noureddine [Laboratoire des Sciences des Procédés et des Matériaux, CNRS, LSPM—UPR 3407, Université Paris 13, Sorbonne-Paris-Cité, 99 Avenue J.-B. Clément, 93430 Villetaneuse (France); Villeroy, Benjamin [Institut de Chimie et des Matériaux Paris Est, CNRS, ICMPE—UMR 7182, Equipe de Chimie Métallurgique des Terres Rares, 2-8 rue Henri Dunant, 94320 Thiais Cedex (France); Leridon, Brigitte [Laboratoire de Physique et d’Étude des Matériaux, LPEM, ESPCI-ParisTech, CNRS, UPMC, 10 rue Vauquelin, F-75231 Paris Cedex 5 (France)

2013-10-28

We developed a two-step process showing the way for sintering anisotropic nanostructured bulk ferromagnetic materials. A new reactor has been optimized allowing the synthesis of several grams per batch of nanopowders via a polyol soft chemistry route. The feasibility of the scale-up has been successfully demonstrated for Co{sub 80}Ni{sub 20} nanowires and a massic yield of ∼97% was obtained. The thus obtained nanowires show an average diameter of ∼6 nm and a length of ∼270 nm. A new bottom-up strategy allowed us to compact the powder into a bulk nanostructured system. We used a spark-plasma-sintering technique under uniaxial compression and low temperature assisted by a permanent magnetic field of 1 T. A macroscopic pellet of partially aligned nanowire arrays has been easily obtained. This showed optimized coercive properties along the direction of the magnetic field applied during compaction (i.e., the nanowires' direction)

Spark plasma sintering and mechanical properties of $ZrO_{2} (Y_{2}O_{3})-Al_{2}O_{3}$ composites

CERN Document Server

Jin Sheng H; Dalla Torre, S; Miyamoto, H; Miyamoto, K

2000-01-01

Spark plasma sintering (SPS) was conducted on nanocrystalline ZrO/sub 2/(Y/sub 2/O/sub 3/)-20 mol% Al/sub 2/O/sub 3/ powder at a heat rate of 600 degrees C/min with a short holding time. Full density was obtained at sintering temperatures >1300 degrees C. Considerable grain growth occurred relative to the initial powder particles, but smaller grain size and higher density can be obtained as compared to hot-pressing. High flexural strength and fracture toughness were also achieved for the SPS-resulted composite. (8 refs).

The Influence of Sintering Temperature of Reactive Sintered (Ti, MoC-Ni Cermets

Directory of Open Access Journals (Sweden)

Marek Jõeleht

2015-09-01

Full Text Available Titanium-molybdenum carbide nickel cermets ((Ti, MoC-Ni were produced using high energy milling and reactive sintering process. Compared to conventional TiC-NiMo cermet sintering the parameters for reactive sintered cermets vary since additional processes are present such as carbide synthesis. Therefore, it is essential to acquire information about the suitable sintering regime for reactive sintered cermets. One of the key parameters is the final sintering temperature when the liquid binder Ni forms the final matrix and vacancies inside the material are removed. The influence of the final sintering temperature is analyzed by scanning electron microscopy. Mechanical properties of the material are characterized by transverse rupture strength, hardness and fracture toughness.DOI: http://dx.doi.org/10.5755/j01.ms.21.3.7179

Temperature dependence of magnetic behaviour in very fine grained, spark plasma sintered NiCuZn ferrites

Energy Technology Data Exchange (ETDEWEB)

Ahmadi, Behzad; Zehani, Karim; LoBue, Martino; Loyau, Vincent; Mazaleyrat, Frederic [SATIE, ENS Cachan, CNRS, UniverSud 61, avenue du President Wilson, F-94230 Cachan (France)

2012-04-01

Recently, using spark plasma sintering technique, a family of very fine grained, fully dense NiCuZn ferrites have been produced, which show constant permeability up to several 10 MHz. These ferrites can be used for filtering purposes in high frequency applications where a wide frequency band is required. In this paper, we study the magnetization processes taking place in these nano grained materials, in the frequency interval of 100 kHz to 5 MHz. Using a fluxmetric hysteresis graph, permeability, loss, and BH loops are measured at different temperatures, from -5 deg. C to 110 deg. C. Results are compared to the behavior of micrometric grain size ferrites, which are commonly used for power electronic and high frequency applications.

Temperature dependence of magnetic behaviour in very fine grained, spark plasma sintered NiCuZn ferrites

International Nuclear Information System (INIS)

Ahmadi, Behzad; Zehani, Karim; LoBue, Martino; Loyau, Vincent; Mazaleyrat, Frederic

2012-01-01

Recently, using spark plasma sintering technique, a family of very fine grained, fully dense NiCuZn ferrites have been produced, which show constant permeability up to several 10 MHz. These ferrites can be used for filtering purposes in high frequency applications where a wide frequency band is required. In this paper, we study the magnetization processes taking place in these nano grained materials, in the frequency interval of 100 kHz to 5 MHz. Using a fluxmetric hysteresis graph, permeability, loss, and BH loops are measured at different temperatures, from -5 deg. C to 110 deg. C. Results are compared to the behavior of micrometric grain size ferrites, which are commonly used for power electronic and high frequency applications.

A study of emission property and microstructure of rare earth oxide-molybdenum cermet cathode materials made by spark plasma sintering

International Nuclear Information System (INIS)

Wang Jinshu; Li Hongyi; Yang Sa; Cui Ying; Zhou Meiling

2004-01-01

A fast sintering method, spark plasma sintering (SPS) was used for the synthesis of rare earth oxide-molybdenum cathode material. The secondary emission property, microstructure, and phase constitution of materials have been studied in this paper. The experimental results show that the maximum secondary emission coefficient of this material can be high to 3.84, much higher than that of rare earth oxide-molybdenum cathode made by traditional sintering method. The grain size is less than 1 μm and rare earth distributed evenly in the material. After the material was activated at 1600 deg. C, a 4 μm layer of rare earth oxide which leads to the high secondary emission coefficient of the material, is formed on the surface of the cathode

ZrB₂-CNTs Nanocomposites Fabricated by Spark Plasma Sintering.

Science.gov (United States)

Jin, Hua; Meng, Songhe; Xie, Weihua; Xu, Chenghai; Niu, Jiahong

2016-11-29

ZrB₂-based nanocomposites with and without carbon nanotubes (CNTs) as reinforcement were prepared at 1600 °C by spark plasma sintering. The effects of CNTs on the microstructure and mechanical properties of nano-ZrB₂ matrix composites were studied. The results indicated that adding CNTs can inhibit the abnormal grain growth of ZrB₂ grains and improve the fracture toughness of the composites. The toughness mechanisms were crack deflection, crack bridging, debonding, and pull-out of CNTs. The experimental results of the nanograined ZrB₂-CNTs composites were compared with those of the micro-grained ZrB₂-CNTs composites. Due to the small size and surface effects, the nanograined ZrB₂-CNTs composites exhibited stronger mechanical properties: the hardness, flexural strength and fracture toughness were 18.7 ± 0.2 GPa, 1016 ± 75 MPa, and 8.5 ± 0.4 MPa·m 1/2 , respectively.

Kinetics of UO2 sintering

International Nuclear Information System (INIS)

Ristic, M.M.

1962-01-01

Detailed conclusions related to the UO 2 sintering can be drawn from investigating the kinetics of the sintering process. This report gives an thorough analysis of the the data concerned with sintering available in the literature taking into account the Jander and Arrhenius laws. This analysis completes the study of influence of the O/U ratio and the atmosphere on the sintering. Results presented are fundamentals of future theoretical and experimental work related to characterisation of the UO 2 sintering process

Plasma synthesis of nanostructures for improved thermoelectric properties

International Nuclear Information System (INIS)

Petermann, Nils; Hecht, Christian; Schulz, Christof; Wiggers, Hartmut; Stein, Niklas; Schierning, Gabi; Theissmann, Ralf; Stoib, Benedikt; Brandt, Martin S

2011-01-01

The utilization of silicon-based materials for thermoelectrics is studied with respect to the synthesis and processing of doped silicon nanoparticles from gas phase plasma synthesis. It is found that plasma synthesis enables the formation of spherical, highly crystalline and soft-agglomerated materials. We discuss the requirements for the formation of dense sintered bodies, while keeping the crystallite size small. Small particles a few tens of nanometres and below that are easily achievable from plasma synthesis, and a weak surface oxidation, both lead to a pronounced sinter activity about 350 K below the temperature usually needed for the successful densification of silicon. The thermoelectric properties of our sintered materials are comparable to the best results found for nanocrystalline silicon prepared by methods other than plasma synthesis.

Sintering Theory and Practice

Science.gov (United States)

German, Randall M.

1996-01-01

Although sintering is an essential process in the manufacture of ceramics and certain metals, as well as several other industrial operations, until now, no single book has treated both the background theory and the practical application of this complex and often delicate procedure. In Sintering Theory and Practice, leading researcher and materials engineer Randall M. German presents a comprehensive treatment of this subject that will be of great use to manufacturers and scientists alike. This practical guide to sintering considers the fact that while the bonding process improves strength and other engineering properties of the compacted material, inappropriate methods of control may lead to cracking, distortion, and other defects. It provides a working knowledge of sintering, and shows how to avoid problems while accounting for variables such as particle size, maximum temperature, time at that temperature, and other problems that may cause changes in processing. The book describes the fundamental atomic events that govern the transformation from particles to solid, covers all forms of the sintering process, and provides a summary of many actual production cycles. Building from the ground up, it begins with definitions and progresses to measurement techniques, easing the transition, especially for students, into advanced topics such as single-phase solid-state sintering, microstructure changes, the complications of mixed particles, and pressure-assisted sintering. German draws on some six thousand references to provide a coherent and lucid treatment of the subject, making scientific principles and practical applications accessible to both students and professionals. In the process, he also points out and avoids the pitfalls found in various competing theories, concepts, and mathematical disputes within the field. A unique opportunity to discover what sintering is all about--both in theory and in practice What is sintering? We see the end product of this thermal

Production of dispersed nanometer sized YAG powders from alkoxide, nitrate and chloride precursors and spark plasma sintering to transparency

International Nuclear Information System (INIS)

Suarez, M.; Fernandez, A.; Menendez, J.L.; Torrecillas, R.

2010-01-01

Yttrium aluminum garnet (YAG) was synthesized from different starting materials, i.e., alkoxide, nitrate and chloride precursors. The conversion steps from the precursors to crystalline YAG were studied by Raman spectroscopy. Dispersed YAG powders were formed at a relatively low temperature, around 800 o C by the chlorides route, whereas alkoxide precursors needed firing over 900 o C and nitrates even over 1100 o C. Lyophilized YAG gel was sintered to transparency by the spark plasma sintering method at 1500 o C with in-line transmittances close to 60% at 680 nm and over 80% in the infrared range.

Effect of two-stage sintering process on microstructure and mechanical properties of ODS tungsten heavy alloy

Energy Technology Data Exchange (ETDEWEB)

Lee, Kyong H. [Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology, 373-1 Kusong-dong, Yusong-gu, Taejon 305-701 (Korea, Republic of); Cha, Seung I. [International Center for Young Scientists, National Institute for Materials Science 1-1, Namiki, Tsukuba 305-0044 (Japan); Ryu, Ho J. [DUPIC, Korea Atomic Energy Research Institute, 150 Deokjin-dong, Yusong-gu, Taejon 305-353 (Korea, Republic of); Hong, Soon H. [Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology, 373-1 Kusong-dong, Yusong-gu, Taejon 305-701 (Korea, Republic of)], E-mail: shhong@kaist.ac.kr

2007-06-15

Oxide dispersion strengthened (ODS) tungsten heavy alloys have been considered as promising candidates for advanced kinetic energy penetrator due to their characteristic fracture mode compared to conventional tungsten heavy alloy. In order to obtain high relative density, the ODS tungsten heavy alloy needs to be sintered at higher temperature for longer time, however, induces growth of tungsten grains. Therefore, it is very difficult to obtain controlled microstructure of ODS tungsten heavy alloy having fine tungsten grains with full densification. In this study, two-stage sintering process, consisted of primary solid-state sintering and followed by secondary liquid phase sintering, was introduced for ODS tungsten heavy alloys. The mechanically alloyed 94W-4.56Ni-1.14Fe-0.3Y{sub 2}O{sub 3} powders are solid-state sintered at 1300-1450 deg. C for 1 h in hydrogen atmosphere, and followed by liquid phase sintering temperature at 1465-1485 deg. C for 0-60 min. The microstructure of ODS tungsten heavy alloys showed high relative density above 97%, with contiguous tungsten grains after primary solid-state sintering. The microstructure of solid-state sintered ODS tungsten heavy alloy was changed into spherical tungsten grains embedded in W-Ni-Fe matrix during secondary liquid phase sintering. The two-stage sintered ODS tungsten heavy alloy from mechanically alloyed powders showed finer microstructure and higher mechanical properties than conventional liquid phase sintered alloy. The mechanical properties of ODS tungsten heavy alloys are dependent on the microstructural parameters such as tungsten grain size, matrix volume fraction and tungsten/tungsten contiguity, which can be controlled through the two-stage sintering process.

Boric oxide or boric acid sintering aid for sintering ceramics

International Nuclear Information System (INIS)

Lawler, H.A.

1979-01-01

The invention described relates to the use of liquid sintering aid in processes involving sintering of ceramic materials to produce dense, hard articles having industrial uses. Although the invention is specifically discussed in regard to compositions containing silicon carbide as the ceramic material, other sinterable carbides, for example, titanium carbide, may be utilized as the ceramic material. A liquid sintering aid for densifying ceramic material is selected from solutions of H 3 BO 3 , B 2 O 3 and mixtures of these solutions. In sintering ceramic articles, e.g. silicon carbide, a shaped green body is formed from a particulate ceramic material and a resin binder, and the green body is baked at a temperature of 500 to 1000 0 C to form a porous body. The liquid sintering aid of B 2 O 3 and/or H 3 BO 3 is then dispersed through the porous body and the treated body is sintered at a temperature of 1900 to 2200 0 C to produce the sintered ceramic article. (U.K.)

Effect of microstructure changes on magnetic properties of spark plasma sintered Nd-Fe-B powders

Directory of Open Access Journals (Sweden)

Michalski B.

2013-01-01

Full Text Available In this study the SPS method was applied for low RE content (8,5% at. and high RE content (13,5 % at. MQ powders. The powders were sintered in a wide range of temperature, for 5 min., under pressure of 35 MPa. The low RE content grade, densified reluctantly and gained the density close to the theoretical value only for 850 °C. The coercivity decreased gradually with increasing sintering temperature. On the other hand, the densification of the higher RE content grade powder occurred much easier and the coercivity, close to the theoretical value, was achieved already at 650 °C. The coercivity of this material also decreased with increasing sintering temperature. Microstructural studies revealed that the SPS sintering process leads to partial decomposition of the Nd2Fe14B phase. The proportion of the RE-rich and iron phases increases parallel to the increasing sintering temperature. On the basis of the current results one can conclude that fabrication of high density MQ powders based magnets by the SPS method is possible, however the powders having higher RE content should be used for this purpose and the sintering temperature as low as possible, related to density, should be kept.

The influence of milling and spark plasma sintering on the microstructure and properties of the Al7075 alloy

Czech Academy of Sciences Publication Activity Database

Molnárová, O.; Málek, P.; Veselý, J.; Minárik, P.; Lukáč, František; Chráska, Tomáš; Novák, P.; Průša, F.

2018-01-01

Roč. 11, č. 4 (2018), č. článku 547. ISSN 1996-1944 R&D Projects: GA ČR(CZ) GA15-15609S Institutional support: RVO:61389021 Keywords : gas atomized Al7075 alloy * mechanical milling * spark plasma sintering * microstructure * microhardness Subject RIV: JG - Metallurgy Impact factor: 2.654, year: 2016

Structure and mechanical properties of Al-Si-Fe alloys prepared by short-term mechanical alloying and Spark Plasma Sintering

Czech Academy of Sciences Publication Activity Database

Průša, J.; Vojtěch, D.; Bláhová, M.; Michalcová, A.; Kubatík, Tomáš František; Čížek, J.

2015-01-01

Roč. 75, June (2015), s. 65-75 ISSN 0261-3069 Institutional support: RVO:61389021 Keywords : Aluminium alloy s * Mechanical Properties * Microstructure * Mechanical alloy ing * Spark-Plasma Sintering Subject RIV: JG - Metallurgy Impact factor: 3.997, year: 2015 http://www.sciencedirect.com/science/article/pii/S0261306915000990#

Microstructure and superconducting properties of Bi-2223/Ag tapes fabricated in the two-step sintering process

International Nuclear Information System (INIS)

Lu, X.Y.; Nagata, A.; Sugawara, K.

2008-01-01

The microstructure and superconducting properties of Bi-2223/Ag tapes fabricated in the two-step sintering process were investigated. The tapes were then subjected to two heat treatments with an intermediate rolling. All the tapes were sintered at 835 deg. C for 24 h at initial sintering stage. A two-step sintering procedure was then used in the final sintering stage. In the first step, the tapes are sintered at 840-865 deg. C for 1 h. In the second step, they were sintered at 835 deg. C for 120 h. The results show that the first step sintering temperature has significant influence on the microstructure and the critical current density J c . The observed microstructures are consistent well with the different J c performances of the tapes first-step-sintered at different temperatures. The tape first-step-sintered at 850 deg. C, which has small secondary phases, stronger c-axis grain alignment, higher proportion of Bi-2223 phase, and no cracks, exhibits the highest J c value

Isotropic and anisotropic nanocrystalline NdFeB-based magnets prepared by spark plasma sintering and hot deformation

International Nuclear Information System (INIS)

Liu, Z.W.; Huang, Y.L.; Huang, H.Y.; Zhong, X.C.; Yu, Y.H.; Zeng, D.C.

2011-01-01

Isotropic and anisotropic NdFeB permanent magnets were prepared by Spark Plasma Sintering (SPS) and SPS followed hot deformation (HD), respectively, using melt spun NdFeB ribbons with various compositions as starting materials. It is found that, based on RE-rich composition, SPSed magnets sintered at low temperatures (<700 C) almost maintained the uniform fine grain structure inherited from rapid quenching. At higher temperatures, a distinct two-zone (coarse grain and fine grain zones) structure was formed in the SPSed magnets. The SPS temperature and pressure have important effects on the grain structure, which led to the variations in the magnetic properties. By employing low SPS temperature and high pressure, high-density magnets with negligible coarse grain zone and an excellent combination of magnetic properties can be obtained. For single phase NdFeB alloy, because of the deficiency of Nd-rich phases, it is relatively difficult to consolidate micro-sized melt spun powders into high density bulk magnet, but generally a larger particle size is beneficial to achieve better magnetic properties. Anisotropic magnets with a maximum energy product of approx. equal to 38 MGOe were produced by the SPS+HD process. HD did not lead to obvious grain growth and the two-zone structure still existed in the hot deformed magnets. The results indicated that nanocrystalline NdFeB magnets without significant grain growth and with excellent properties could be obtained by SPS and HD processes. (author)

Influence of electric current on microstructure evolution in Ti/Al and Ti/TiAl{sub 3} during spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Sun, Y. [Department of Materials Science and Engineering, Institute of Materials Science, University of Connecticut, Storrs, CT 06269-3136 (United States); Haley, J. [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616-5294 (United States); Kulkarni, K. [Department of Materials Science and Engineering, Indian Institute of Technology, Kanpur 208016, UP (India); Aindow, M. [Department of Materials Science and Engineering, Institute of Materials Science, University of Connecticut, Storrs, CT 06269-3136 (United States); Lavernia, E.J., E-mail: lavernia@ucdavis.edu [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616-5294 (United States); Department of Chemical Engineering and Materials Science, University of California, Irvine, CA 92697-2575 (United States)

2015-11-05

The synthesis of γ-TiAl from elemental metals via solid-state reactive diffusion processing routes involves multiple reaction steps with the formation of various intermediate intermetallic compounds, starting with TiAl{sub 3} because this phase is favored kinetically. To understand the processes by which the TiAl{sub 3} intermediate is eliminated during synthesis of γ-TiAl alloy via spark plasma sintering (SPS), the reaction between Ti and TiAl{sub 3} during SPS was studied with emphasis on the effects of the applied electric current and starting TiAl{sub 3} microstructure on the reaction kinetics and the underlying diffusion mechanisms. The intermediate intermetallic phases Ti{sub 3}Al, TiAl and TiAl{sub 2} were formed between the Ti and TiAl{sub 3} upon SPS processing at 900 °C. The applied electric current did not alter the character of the phases formation in the Ti/TiAl{sub 3} system, but thermodynamic calculations suggest that the activation energy for the nucleation of TiAl{sub 2} is reduced significantly with an electric current flowing. Moreover, the kinetics of the reactions between Ti and TiAl{sub 3} were enhanced when the starting TiAl{sub 3} microstructure was refined. The electric field also had a more significant influence on the grain growth kinetics for TiAl{sub 2} and TiAl in powder blend compacts with refined microstructures. - Highlights: • Reaction between Ti and TiAl{sub 3} during spark plasma sintering was studied. • Refined starting TiAl{sub 3} microstructure enhanced the reactions kinetics. • The nucleation barrier of TiAl{sub 2} was reduced by the applied electric field. • The applied electric field restrained the grain growth of TiAl and TiAl{sub 2}.

Effect of cryogenic milling on Al7075 prepared by spark plasma sintering method.

Czech Academy of Sciences Publication Activity Database

Lukáč, František; Chráska, Tomáš; Molnárová, O.; Málek, P.; Cinert, Jakub

2017-01-01

Roč. 32, S1 (2017), S221-S224 ISSN 0885-7156. [European Powder Diffraction Conference (EPDIC) /15./. Bari, 12.06.2016-15.06.2016] R&D Projects: GA ČR(CZ) GA15-15609S Institutional support: RVO:61389021 Keywords : Intermetallic precipitates * cryogenic milling * powder metallurgy * ultrafine-grained materials * Al7075 alloy Subject RIV: JG - Metallurgy OBOR OECD: Materials engineering Impact factor: 0.674, year: 2016 https://www.cambridge.org/core/journals/powder-diffraction/ article /effect-of-cryogenic-milling-on-al7075-prepared-by-spark-plasma-sintering-method/17E9F722BAFD428BA7310194FEE551C6

Study of nano-metric silicon carbide powder sintering. Application to fibers processing

International Nuclear Information System (INIS)

Malinge, A.

2011-01-01

Silicon carbide ceramic matrix composites (SiCf/SiCm) are of interest for high temperature applications in aerospace or nuclear components for their relatively high thermal conductivity and low activation under neutron irradiation. While most of silicon carbide fibers are obtained through the pyrolysis of a poly-carbo-silane precursor, sintering of silicon carbide nano-powders seems to be a promising route to explore. For this reason, pressureless sintering of SiC has been studied. Following the identification of appropriate sintering aids for the densification, optimization of the microstructure has been achieved through (i) the analysis of the influence of operating parameters and (ii) the control of the SiC β a SiC α phase transition. Green fibers have been obtained by two different processes involving the extrusion of SiC powder dispersion in polymer solution or the coagulation of a water-soluble polymer containing ceramic particles. Sintering of these green fibers led to fibers of around fifty microns in diameter. (author) [fr

Porous copper template from partially spark plasma-sintered Cu–Zn ...

Indian Academy of Sciences (India)

Administrator

analysis. Keywords. Metal; corrosion; porous structure; sintering; powder metallurgy. 1. Introduction ... well as in the case, when the overall electrode potential of the final ... at 100 °C/min to reach sintering temperature and load was applied ...

Spark-plasma sintering of ZrB2 ultra-high-temperature ceramics

OpenAIRE

Zamora Rodríguez, Víctor

2013-01-01

This work was performed in the context of the research line entitled Processing and Sintering of Advanced Ceramic Materials in the Grupo Especializado de Materiales of the University of Extremadura, and was supported by the Ministerio de Ciencia y Tecnología (Government of Spain) and FEDER funds under the Grant Nº MAT 2007-61609.

Comparative evaluation of electrical conductivity of hydroxyapatite ceramics densified through ramp and hold, spark plasma and post sinter Hot Isostatic Pressing routes

Energy Technology Data Exchange (ETDEWEB)

Buchi Suresh, M., E-mail: suresh@arci.res.in; Biswas, P.; Mahender, V.; Johnson, Roy, E-mail: royjohnson@arci.res.in

2017-01-01

Hydroxyapatite ceramics synthesized through sonochemical route were processed and densified through ramp & hold (R&H) and Spark Plasma Sintering (SPS) routes. The effect of processing route on the relative density and electrical conductivity were studied. Further, the samples were Hot Isostatically Pressed (HIP) under argon pressure at elevated temperature to further densify the sample. All these samples processed under different conditions were characterized by X-ray diffraction, Scanning Electron Microscopy and AC Conductivity. The samples have exhibited hydroxyapatite phase; however, microstructures exhibited distinctly different grain morphologies and grain sizes. AC impedance spectroscopic measurement was carried out on hydroxyapatite samples processed through different routes and the corresponding spectra were analyzed by the analogy to equivalent circuit involving resistors and capacitors. SPS sintered sample after HIPing has exhibited the highest conductivity. This can be attributed to the higher density in combination with finer grain sizes. Activation energy based on Arrhenius equation is calculated and the prominent conduction mechanism is proposed. - Highlights: • Hot Isostatic Pressing (HIP) of SPS and R&H processed samples has resulted into densities near to theoretical densities • No change in the crystal structure is observed in SPS and R&H samples before and after HIP treatment • SPS processed and HIP treated samples resulted into higher conductivities with smaller grain sizes and grain boundary area.

Consolidation of mechanically alloyed nanocrystalline Cu-Nb-ZrO{sub 2} powder by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Eymann, K., E-mail: Konrad.Eymann@tu-dresden.de [Institute of Materials Science, Technische Universitaet Dresden, 01062 Dresden (Germany); Riedl, T.; Bram, A.; Ruhnow, M.; Boucher, R.; Kirchner, A.; Kieback, B. [Institute of Materials Science, Technische Universitaet Dresden, 01062 Dresden (Germany)

2012-09-15

Highlights: Black-Right-Pointing-Pointer Solid solution of Cu-Nb was achieved by mechanically alloying Cu, Nb and ZrO{sub 2}. Black-Right-Pointing-Pointer In as-milled state the Cu-Nb-ZrO{sub 2} powders show an average Cu grain size of 16 nm. Black-Right-Pointing-Pointer Mechanical and electrical properties are studied in dependence of thermal exposure. Black-Right-Pointing-Pointer Compaction at 1000 Degree-Sign C/1 min using SPS increases Cu grain size to 43 nm. Black-Right-Pointing-Pointer Bulk samples reach a maximum IACS of 16% and 98% relative density. - Abstract: This work presents the synthesis of ultra fine grained high-strength Cu-Nb-ZrO{sub 2} bulk samples via mechanical alloying and spark plasma sintering. Technologically relevant properties such as density, micro-hardness, and electrical conductivity were studied in terms of the compaction parameters, in particular the sintering temperature and holding time. An optimum process parameter combination has been found T = 950 Degree-Sign C, t = 1 min, and 65 MPa, which yield a micro-hardness of 325 HV, 97.5% relative density, and electrical conductivity of 10% IACS. The dependence of these properties on the compaction parameters is explained by analyzing the microstructure, i.e. grain size, presence and distribution of phases, and porosity, with X-ray diffraction, optical and electron microscopy as well as with an Archimedes densitometer.

Study of the sintering process and the formation of a (Th, U) O2 solid solution

International Nuclear Information System (INIS)

Tomasi, Roberto

1979-01-01

The effect of some variables in the (Th, U) O 2 sintering process and solid solution formation was studied. ThO 2 , U 3 O 8 and UO 2 powder were prepared. The ThO 2 powders were obtained by calcination of thorium at 500 and 750 deg C; the U 3 O 8 powders were derived from the calcination of ADU at 660 and 750 deg C; the UO 2 powder were prepared from ADU and from ATCU. The different characteristics of these materials were determined by measurements of surface area, by scanning electron microscopy, tap density tests, X-ray diffractometry and by measurements of the O/U ratios. The oxide mixtures were chosen in order to produce a final composition with 10 w/o of UO 2 . A mixture of thorium oxalate and ADU was also prepared by calcining these salts in air at 700 deg C, in order to obtain certain amount of solid solution prior to sintering. The sintering operations were developed in an argon atmosphere at temperatures between 1400 and 1700 deg C, during interval varying from 1 to 4 hours. The effect of the mixture characteristics on the sintering process and solid solution formation were studied considering the results of densification, microstructure development and X-ray diffractometry. The ThO 2 powder characteristics have a main effect on the mixtures compactability and sinterability, the higher calcining temperatures increasing the green density, but decreasing the final density of the sintered pellets. In the sintering of mixtures containing U 3 O 3 , this oxide is reduced to UO 2 and it is possible to obtain pellets with density and microstructures similar to those produced from mixtures containing UO 2 . But if oxygen in excess is present during sintering, the process is affected, occurring exaggerated grain growth. The densification results were related to the Coble's kinetics equation for second stage of sintering, valid for bulk diffusion, grain boundary acting as vacancy sinks. The sintering activation energy is independent from the powder starting

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

Science.gov (United States)

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

2017-08-01

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

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

Science.gov (United States)

Zhao, Yan; Gao, Yang

2017-12-01

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

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

Science.gov (United States)

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.

Microstructure, magnetic and Moessbauer studies on spark-plasma sintered Sm-Co-Fe/Fe(Co) nanocomposite magnets

Energy Technology Data Exchange (ETDEWEB)

Rao, N V Rama; Saravanan, P; Gopalan, R; Raja, M Manivel; Rao, D V Sreedhara; Chandrasekaran, V [Defence Metallurgical Research Laboratory, Hyderabad-500 058 (India); Sivaprahasam, D [International Advanced Research Centre for Powder Metallurgy and New Materials Hyderabad-500 005 (India); Ranganathan, R [Saha Institute of Nuclear Physics, Kolkata-700 064 (India)], E-mail: rg_gopy@yahoo.com

2008-03-21

Nanocomposite powders comprising Sm-Co-Fe intermetallic phases and Fe(Co) were synthesized by high-energy ball milling and were consolidated into bulk magnets by the spark-plasma sintering (SPS) technique. While the microstructure of the SPS samples was characterized by transmission electron microscopy (TEM), the solubility of Fe in different phases was investigated using Moessbauer spectroscopy. TEM studies revealed that the spark-plasma sintered sample has Sm(Co,Fe){sub 5} as a major phase with Sm{sub 2}(Co,Fe){sub 17}, Sm(Co,Fe){sub 2} and Fe(Co) as secondary phases. The size of the nanocrystalline grains of all these phases was found to be in the range 50-100 nm. The Moessbauer spectra of the as-milled powders exhibited two different subspectra: a sextet corresponding to the Fe phase and a broad sextet associated with the Fe(Co) phase; while that of the SPS sample showed four different subspectra: a sextet corresponding to Fe and other three sextets corresponding to the Fe(Co), Sm(Co,Fe){sub 5} and Sm{sub 2}(Co,Fe){sub 17} phases; these results are in accordance with the TEM observation. Recoil magnetization and reversible susceptibility measurements revealed magnetically single phase behaviour of the SPS magnets.

Spark Plasma Sintering of Ultracapacitors

Energy Technology Data Exchange (ETDEWEB)

Hill, Curtis W. [CK Technologies, Camirillo, CA (United States); Boatner, Lynn A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Tucker, Dennis [NASA Johnson Space Center, Houston, TX (United States); Kolopus, James A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Cheng, Zhongyang [Auburn Univ., AL (United States)

2016-01-01

A solid-state ultracapacitor module to replace standard electrochemical batteries would achieve major performance gains and mass/volume reduction. This report summarizes a project to evaluate an alternative sintering process to produce a solid-state ultracapacitor to overcome the limitations of both the electrochemical batteries presently in use on spacecraft and of currently available electrochemical ultracapacitors. It will provide a robust energy storage device with higher reliability, wider working temperature range, longer lifetime, and less weight and volume than electrochemical batteries. As modern electronics decrease in size, more efficient and robust remote power is needed. Current state-of-the-art rechargeable batteries cannot be rapidly charged, contain harmful chemicals, and suffer from early wear-out mechanisms. Solid-state ultracapacitors are recyclable energy storage devices that offer the promise of higher power and a greater number of charge/discharge cycles than current rechargeable batteries. In addition, the theoretical energy density when compared to current electrochemical batteries indicates that a significant weight savings is possible. This is a project to develop a very high density solid-state ultracapacitor with giant permittivity and acceptable dielectric loss to overcome the energy-density barrier such that it will be a suitable replacement for batteries.

In vitro cell-biological performance and structural characterization of selective laser sintered and plasma surface functionalized polycaprolactone scaffolds for bone regeneration

Energy Technology Data Exchange (ETDEWEB)

Van Bael, Simon, E-mail: simon.vanbael@mech.kuleuven.be [Department of Mechanical Engineering, Division of Production Engineering, Machine Design and Automation, Katholieke Universiteit Leuven, Celestijnenlaan 300b, 3001 Leuven (Belgium); Department of Mechanical Engineering, Division of Biomechanics and Engineering Design, Katholieke Universiteit Leuven, Celestijnenlaan 300c, bus 2419, 3001 Heverlee (Belgium); Prometheus, Division of Skeletal Tissue Engineering, Katholieke Universiteit Leuven, O and N 1, Herestraat 49, bus 813, 3000 Leuven (Belgium); Desmet, Tim [Polymer Chemistry and Biomaterials Research Group, Ghent University, Krijgslaan 281 S4 Bis, Ghent, 9000 (Belgium); Research Unit Plasma Technology (RUPT), Department of Applied Physics, Faculty of Engineering, Ghent University, Jozef Plateaustraat 22, 9000 Ghent (Belgium); Chai, Yoke Chin [Prometheus, Division of Skeletal Tissue Engineering, Katholieke Universiteit Leuven, O and N 1, Herestraat 49, bus 813, 3000 Leuven (Belgium); Pyka, Gregory [Prometheus, Division of Skeletal Tissue Engineering, Katholieke Universiteit Leuven, O and N 1, Herestraat 49, bus 813, 3000 Leuven (Belgium); Department of Metallurgy and Materials Engineering, Katholieke Universiteit Leuven, Kasteelpark Arenberg 44, bus 2450, 3001 Leuven (Belgium); Dubruel, Peter [Polymer Chemistry and Biomaterials Research Group, Ghent University, Krijgslaan 281 S4 Bis, Ghent, 9000 (Belgium); Research Unit Plasma Technology (RUPT), Department of Applied Physics, Faculty of Engineering, Ghent University, Jozef Plateaustraat 22, 9000 Ghent (Belgium); Kruth, Jean-Pierre [Department of Mechanical Engineering, Division of Production Engineering, Machine Design and Automation, Katholieke Universiteit Leuven, Celestijnenlaan 300b, 3001 Leuven (Belgium); Schrooten, Jan [Prometheus, Division of Skeletal Tissue Engineering, Katholieke Universiteit Leuven, O and N 1, Herestraat 49, bus 813, 3000 Leuven (Belgium)

2013-08-01

In the present study a structural characterization and in vitro cell-biological evaluation was performed on polycaprolactone (PCL) scaffolds that were produced by the additive manufacturing technique selective laser sintering (SLS), followed by a plasma-based surface modification technique, either non-thermal oxygen plasma or double protein coating, to functionalize the PCL scaffold surfaces. In the first part of this study pore morphology by means of 2D optical microscopy, surface chemistry by means of hydrophilicity measurement and X-ray photoelectron spectroscopy, strut surface roughness by means of 3D micro-computed tomography (CT) imaging and scaffold mechanical properties by means of compression testing were evaluated before and after the surface modifications. The results showed that both surface modifications increased the PCL scaffold hydrophilicity without altering the morphological and mechanical properties. In the second part of this study the in vitro cell proliferation and differentiation of human osteoprogenitor cells, over 14 days of culture in osteogenic and growth medium were investigated. The O{sub 2} plasma modification gave rise to a significant lower in vitro cell proliferation compared to the untreated and double protein coated scaffolds. Furthermore the double protein coating increased in vitro cell metabolic activity and cell differentiation compared to the untreated and O{sub 2} plasma PCL scaffolds when OM was used. - Highlights: • Polycaprolactone scaffolds are produced with selective laser sintering. • 2 types of plasma based surface functionalization were applied. • Plasma had no significant effect on strut roughness and pore morphology. • Plasma improved surface hydrophilicity. • In vitro cell differentiation increased with plasma protein coated functionalization.

In vitro cell-biological performance and structural characterization of selective laser sintered and plasma surface functionalized polycaprolactone scaffolds for bone regeneration

International Nuclear Information System (INIS)

Van Bael, Simon; Desmet, Tim; Chai, Yoke Chin; Pyka, Gregory; Dubruel, Peter; Kruth, Jean-Pierre; Schrooten, Jan

2013-01-01

In the present study a structural characterization and in vitro cell-biological evaluation was performed on polycaprolactone (PCL) scaffolds that were produced by the additive manufacturing technique selective laser sintering (SLS), followed by a plasma-based surface modification technique, either non-thermal oxygen plasma or double protein coating, to functionalize the PCL scaffold surfaces. In the first part of this study pore morphology by means of 2D optical microscopy, surface chemistry by means of hydrophilicity measurement and X-ray photoelectron spectroscopy, strut surface roughness by means of 3D micro-computed tomography (CT) imaging and scaffold mechanical properties by means of compression testing were evaluated before and after the surface modifications. The results showed that both surface modifications increased the PCL scaffold hydrophilicity without altering the morphological and mechanical properties. In the second part of this study the in vitro cell proliferation and differentiation of human osteoprogenitor cells, over 14 days of culture in osteogenic and growth medium were investigated. The O 2 plasma modification gave rise to a significant lower in vitro cell proliferation compared to the untreated and double protein coated scaffolds. Furthermore the double protein coating increased in vitro cell metabolic activity and cell differentiation compared to the untreated and O 2 plasma PCL scaffolds when OM was used. - Highlights: • Polycaprolactone scaffolds are produced with selective laser sintering. • 2 types of plasma based surface functionalization were applied. • Plasma had no significant effect on strut roughness and pore morphology. • Plasma improved surface hydrophilicity. • In vitro cell differentiation increased with plasma protein coated functionalization

Development of a Sinter/HIP process for the superalloy Udimet 700 with investigations of the influence of the sinteratmosphere

International Nuclear Information System (INIS)

Wenning, L.

1991-03-01

The oxidation free treatment of reactive metalpowders like the nickel base alloy Udimet 700 demands sufficient oxygen free sinteratmospheres in nowadays sinter-HIP plants are not reachable. The reported work deals with the development of a sinter-HIP process which enables a sufficient low partial pressure of oxygen by scavenging the Udimet 700 powder packings with argon during vacuum sintering. By this the sinter hindering oxidation is avoided. Intensive investigations of the sinteratmosphere with a mass spectrometer and a zirconium oxide probe verify the reduction of the oxygen content of the residual gas atmosphere reached with different processes. In a second part the applicability of the scavenging gas process during the capsule free sinter-HIP treatment of metall injection moulded (MIM) samples is shown. (orig.) [de

Sintering of ZrC by hot isostatic pressing (HIP) and spark plasma sintering (SPS). Effect of impurities

International Nuclear Information System (INIS)

Allemand, Alexandre; Le Flem - Dormeval, Marion; Guillard, Francois

2005-01-01

Carbides are generally used as structural materials for high temperature applications. Particularly, ZrC because of low activation, neutronic transparency, cubic structure (isotropic behaviour) and good thermal conductivity, is one of the candidates under consideration for structural materials in the core of new high temperature nuclear reactors (Generation IV). Just a few studies about densification of monolithic ZrC exist. They mainly involve natural sintering or hot pressing at high temperature (until 2700 deg. C). Unfortunately those processes induce grain growth and do not lead to fully densified ZrC. The aim of this study is to compare the characteristics and the properties of ZrC sintered by HIP and by SPS. Fully dense ZrC can be reached either by HIP or by SPS, grain size being more or less controlled. Microstructural observations and mechanical testing of several ZrC grades shows that powder impurities play an important role in the quality of the grain boundaries and consequently in the mechanical properties. In particular, the porosity falls from 17% to 3 % just by reducing the free carbon content in starting ZrC powder. The densification process of dense monolithic ZrC was improved by combining a HIP at 1600 deg. C (titanium canning) followed by a post-HIP at 1900 deg. C (no canning required). Four-point bending tests are in progress to confirm the improvement of fracture strength. (authors)

Microstructural stability of spark-plasma-sintered W f /W composite with zirconia interface coating under high-heat-flux hydrogen beam irradiation.

Czech Academy of Sciences Publication Activity Database

Avello de Lama, M.; Balden, M.; Greuner, H.; Höschen, T.; Matějíček, Jiří; You, J.H.

2017-01-01

Roč. 13, December (2017), s. 74-80 ISSN 2352-1791 R&D Projects: GA ČR GB14-36566G EU Projects: European Commission(XE) 633053 - EUROfusion Institutional support: RVO:61389021 Keywords : tungsten-fibre/tungsten composites * plasma-facing components * spark plasma sintering Subject RIV: JI - Composite Materials OBOR OECD: Composites (including laminates, reinforced plastics, cermets, combined natural and synthetic fibre fabrics https://www.sciencedirect.com/science/article/pii/S2352179117300273

Alternative sintering methods compared to conventional thermal sintering for inkjet printed silver nanoparticle ink

NARCIS (Netherlands)

Niittynen, J.; Abbel, R.; Mäntysalo, M.; Perelaer, J.; Schubert, U.S.; Lupo, D.

2014-01-01

In this contribution several alternative sintering methods are compared to traditional thermal sintering as high temperature and long process time of thermal sintering are increasing the costs of inkjet-printing and preventing the use of this technology in large scale manufacturing. Alternative

Sintering Process and Mechanical Property of MWCNTs/HDPE Bulk Composite.

Science.gov (United States)

Ming-Wen, Wang; Tze-Chi, Hsu; Jie-Ren, Zheng

2009-08-01

Studies have proved that increasing polymer matrices by carbon nanotubes to form structural reinforcement and electrical conductivity have significantly improved mechanical and electrical properties at very low carbon nanotubes loading. In other words, increasing polymer matrices by carbon nanotubes to form structural reinforcement can reduce friction coefficient and enhance anti-wear property. However, producing traditional MWCNTs in polymeric materix is an extremely complicated process. Using melt-mixing process or in situ polymerization leads to better dispersion effect on composite materials. In this study, therefore, to simplify MWCNTs /HDPE composite process and increase dispersion, powder was used directly to replace pellet to mix and sinter with MWCNTs. The composite bulks with 0, 0.5, 1, 2 and 4% nanotube content by weight was analyzed under SEM to observe nanotubes dispersion. At this rate, a MWCNTs/HDPE composite bulk with uniformly dispersed MWCNTs was achieved, and through the wear bench (Pin-on-Disk), the wear experiment has accomplished. Accordingly, the result suggests the sintered MWCNTs/HDPE composites amplify the hardness and wear-resist property.

Characterization and Sintering of Armstrong Process Titanium Powder

Science.gov (United States)

Xu, Xiaoyan; Nash, Philip; Mangabhai, Damien

2017-04-01

Titanium and titanium alloys have a high strength to weight ratio and good corrosion resistance but also need longer time and have a higher cost on machining. Powder metallurgy offers a viable approach to produce near net-shape complex components with little or no machining. The Armstrong titanium powders are produced by direct reduction of TiCl4 vapor with liquid sodium, a process which has a relatively low cost. This paper presents a systematic research on powder characterization, mechanical properties, and sintering behavior and of Armstrong process powder metallurgy, and also discusses the sodium issue, and the advantages and disadvantages of Armstrong process powders.

Conductivity study of dense BaZr0.9Y0.1O(3 − δ) obtained by spark plasma sintering

DEFF Research Database (Denmark)

Ricote, Sandrine; Bonanos, Nikolaos; Wang, Hsiang-Jen

2012-01-01

10% yttrium doped barium zirconate (BZY10) was synthesized by solid state reaction and a 99.8% dense and transparent sample was prepared by spark plasma sintering (SPS) at 1700 °C for 5 minutes. A single phase compound was obtained, with no evaporation of barium. High-Resolution Transmission...

Comparative studies on mechanical properties of WC-Co composites sintered by SPS and conventional techniques

Directory of Open Access Journals (Sweden)

Pristinskiy Yuri

2017-01-01

Full Text Available Spark plasma sintering (SPS is an extremely fast solidification technique for compounds that are difficult to sinter within the material group metals, ceramics, or composites thereof, SPS uses a uniaxial pressure and a very rapid heating cycle to consolidate these materials. With SPS the main benefit is the ability to control the WC grain size due to the short sintering times at high temperature. Additionally, its allows to avoid negative reactions between WC and cobalt and to minimize the formation of undesirable phases in sintered composites. The WC-6wt.% Co cermet prepared by SPS processing achieves the enhanced mechanical properties with the hardness of 18.3 GPa and the fracture toughness of 15.5 MPa·m1/2 in comparison to standard reference tungsten carbide/cobalt material.

Mechanical characteristics under monotonic and cyclic simple shear of spark plasma sintered ultrafine-grained nickel

International Nuclear Information System (INIS)

Dirras, G.; Bouvier, S.; Gubicza, J.; Hasni, B.; Szilagyi, T.

2009-01-01

The present work focuses on understanding the mechanical behavior of bulk ultrafine-grained nickel specimens processed by spark plasma sintering of high purity nickel nanopowder and subsequently deformed under large amplitude monotonic simple shear tests and strain-controlled cyclic simple shear tests at room temperature. During cyclic tests, the samples were deformed up to an accumulated von Mises strain of about ε VM = 0.75 (the flow stress was in the 650-700 MPa range), which is extremely high in comparison with the low tensile/compression ductility of this class of materials at quasi-static conditions. The underlying physical mechanisms were investigated by electron microscopy and X-ray diffraction profile analysis. Lattice dislocation-based plasticity leading to cell formation and dislocation interactions with twin boundaries contributed to the work-hardening of these materials. The large amount of plastic strain that has been reached during the shear tests highlights intrinsic mechanical characteristics of the ultrafine-grained nickel studied here.

Mechanical characteristics under monotonic and cyclic simple shear of spark plasma sintered ultrafine-grained nickel

Energy Technology Data Exchange (ETDEWEB)

Dirras, G., E-mail: dirras@univ-paris13.fr [LPMTM - CNRS, Institut Galilee, Universite Paris 13, 99 Avenue J.B. Clement, 93430 Villetaneuse (France); Bouvier, S. [LPMTM - CNRS, Institut Galilee, Universite Paris 13, 99 Avenue J.B. Clement, 93430 Villetaneuse (France); Gubicza, J. [Department of Materials Physics, Eoetvoes Lorand University, P.O.B. 32, Budapest H-1518 (Hungary); Hasni, B. [LPMTM - CNRS, Institut Galilee, Universite Paris 13, 99 Avenue J.B. Clement, 93430 Villetaneuse (France); Szilagyi, T. [Department of Materials Physics, Eoetvoes Lorand University, P.O.B. 32, Budapest H-1518 (Hungary)

2009-11-25

The present work focuses on understanding the mechanical behavior of bulk ultrafine-grained nickel specimens processed by spark plasma sintering of high purity nickel nanopowder and subsequently deformed under large amplitude monotonic simple shear tests and strain-controlled cyclic simple shear tests at room temperature. During cyclic tests, the samples were deformed up to an accumulated von Mises strain of about {epsilon}{sub VM} = 0.75 (the flow stress was in the 650-700 MPa range), which is extremely high in comparison with the low tensile/compression ductility of this class of materials at quasi-static conditions. The underlying physical mechanisms were investigated by electron microscopy and X-ray diffraction profile analysis. Lattice dislocation-based plasticity leading to cell formation and dislocation interactions with twin boundaries contributed to the work-hardening of these materials. The large amount of plastic strain that has been reached during the shear tests highlights intrinsic mechanical characteristics of the ultrafine-grained nickel studied here.

Microstructure and mechanical properties of air atomized aluminum powder consolidated via spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Sweet, G.A. [Dalhousie University, Department of Process Engineering and Applied Science, 1360 Barrington Street, Halifax, Nova Scotia, Canada B3J 1Z1 (Canada); Brochu, M. [McGill University, Mining and Materials Engineering Department, 3610 University Street, Montreal, Quebec, Canada H3A 0C5 (Canada); Hexemer, R.L.; Donaldson, I.W. [GKN Sinter Metals LLC, 3300 University Drive, Auburn Hills 48326 (United States); Bishop, D.P., E-mail: Paul.Bishop@dal.ca [Dalhousie University, Department of Process Engineering and Applied Science, 1360 Barrington Street, Halifax, Nova Scotia, Canada B3J 1Z1 (Canada)

2014-07-01

Two air atomized aluminum powders, one of commercial purity and the other magnesium-doped (0.4 wt%), were processed by SPS and conventional PM means. An investigation of SPS processing parameters and their effect on sinter quality were investigated. A comparison with conventionally processed PM counterparts was also conducted. Applied pressure and ultimate processing temperature bore the greatest influence on processing, while heating rate and hold time showed a minor effect. Full density specimens were achieved for both powders under select processing conditions. To compliment this, large (80 mm) and small (20 mm) diameter samples were made to observe possible up-scaling effects, as well as tensile properties. Large samples were successfully processed, albeit with somewhat inferior densities to the smaller counterparts presumably due to the temperature inhomogeneity during processing. An investigation of tensile properties for SPS samples exhibited extensive ductility (∼30%) at high sintering temperatures, while lower temperature SPS samples as well as all PM processed samples exhibited a brittle nature. The measurement of residual oxygen and hydrogen contents showed a significant elimination of both species in SPS samples under certain processing parameters when compared to conventional PM equivalents.

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

Science.gov (United States)

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.

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

Directory of Open Access Journals (Sweden)

Dimos Paraskevas

2014-08-01

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

Investigation of microstructure and irradiation behavior of W–Nb/Ti composites prepared by spark plasma sintering

International Nuclear Information System (INIS)

Chen, Jing-Bo; Luo, Lai-Ma; Zhao, Mei-Ling; Xu, Qiu; Zan, Xiang; Wu, Yu-Cheng

2016-01-01

W–Nb/Ti composites were prepared by machine milling and spark plasma sintering. Field–emission scanning electron microscopy, high–resolution transmission electron microscopy, and X-ray diffraction analyses were used to characterize the samples. Thermal desorption spectroscopy (TDS) was used to measure the deuterium retention after only deuterium irradiation. The deuterium retention in W–4wt%Ti–wt1%Nb was lower than that in pure W (D_2"+ flux ∼10"2"2 ions/(m"2 s), ion energy ∼5 keV), Nb and Ti will improve the deuterium irradiation resistance of tungsten composite. In addition, transgranular and intergranular fractures were observed on the surface of the W–4 wt% Ti–1 wt% Nb composite. A Ti_(_X_)W_(_1_−_X_) solid solution was formed during sintering. The maximum tensile strength (410.53 MPa) was detected in the W–4wt%Ti–1wt%Nb composite at 600 °C.

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

Science.gov (United States)

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.

Phenomenological analysis of densification mechanism during spark plasma sintering of MgAl2O4

Science.gov (United States)

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.

Hydrogen Decrepitation Press-Less Process Recycling of NdFeB sintered magnets

DEFF Research Database (Denmark)

Xia, Manlong; Abrahamsen, Asger Bech; Bahl, Christian

2017-01-01

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...

Strengthening mechanism in graphene nanoplatelets reinforced aluminum composite fabricated through spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Bisht, Ankita [Biomaterials and Multiscale Mechanics Laboratory, Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Uttarakhand 247667 (India); Srivastava, Mukul [Biomaterials and Multiscale Mechanics Laboratory, Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Uttarakhand 247667 (India); Nanomaterials and Applications Laboratory, Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Uttarakhand 247667 (India); Kumar, R. Manoj [Biomaterials and Multiscale Mechanics Laboratory, Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Uttarakhand 247667 (India); Lahiri, Indranil [Nanomaterials and Applications Laboratory, Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Uttarakhand 247667 (India); Lahiri, Debrupa, E-mail: dlahifmt@iitr.ac.in [Biomaterials and Multiscale Mechanics Laboratory, Department of Metallurgical and Materials Engineering, Indian Institute of Technology Roorkee, Uttarakhand 247667 (India)

2017-05-17

Graphene nanoplatelets (GNP) reinforced aluminum matrix composites, with ≤5 wt% GNP content, were synthesized by spark plasma sintering (SPS). GNPs were found to withstand severe conditions of high pressure and temperature during processing. Strength of composite was observed to be depending on the content and uniform dispersion of GNP in aluminum matrix, as verified by scanning electron micrographs. X-ray diffraction analysis confirmed that no reaction products exist at Al-GNP interface in significant amount. Instrumented indentation studies revealed improvement in hardness by 21.4% with 1 wt% GNP. This is due to the presence of stronger reinforcement, which provides high resistance to matrix against deformation. Improvement in yield strength and tensile strength was 84.5% and 54.8%, respectively, with 1 wt% GNP reinforcement. Properties deteriorated at higher concentration due to agglomeration of GNP. Reinforcing effect of GNPs, in terms of strengthening of composite, is found to be dominated by Orowan strengthening mechanism. Pinning of grains boundaries by GNPs led to uniform grain size distribution in the composites structure. Overall, graphene reinforcement has offered 86% improvement in specific strength of aluminum matrix.

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

Science.gov (United States)

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

2018-02-01

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

Mechanical properties of thermoelectric n-type magnesium silicide synthesized employing in situ spark plasma reaction sintering

Science.gov (United States)

Muthiah, Saravanan; Singh, R. C.; Pathak, B. D.; Dhar, Ajay

2017-07-01

Thermoelectric devices employing magnesium silicide (Mg2Si) offer an inexpensive and non-toxic solution for green energy generation compared to other existing conventional thermoelectric materials in the mid-temperature range. However, apart from the thermoelectric performance, their mechanical properties are equally important in order to avoid the catastrophic failure of their modules during actual operation. In the present study, we report the synthesis of Mg2Si co-doped with Bi and Sb employing in situ spark plasma reaction sintering and investigate its broad range of mechanical properties. The mechanical properties of the sintered co-doped Mg2Si suggest a significantly enhanced value of hardness ~5.4  ±  0.2 GPa and an elastic modulus ~142.5  ±  6 GPa with a fracture toughness of ~1.71  ±  0.1 MPa  √m. The thermal shock resistance, which is one of the most vital parameter for designing thermoelectric devices, was found to be ~300 W m-1, which is higher than most of the other existing state-of-the-art mid-temperature thermoelectric materials. The friction and wear characteristics of sintered co-doped Mg2Si have been reported for the first time, in order to realize the sustainability of their thermoelectric modules under actual hostile environmental conditions.

The effects of applied current on one-dimensional interdiffusion between copper and nickel in spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Rudinsky, S.; Gauvin, R.; Brochu, M., E-mail: mathieu.brochu@mcgill.ca [Department of Mining and Materials Engineering, McGill University, 3610 University Street, Montreal, Quebec H3A 0C5 (Canada)

2014-10-21

Spark plasma sintering (SPS) is a powder metallurgy technique that employs the use of fast sintering kinetics to produce final consolidated components in a matter of minutes. In order to use blended powders in SPS to obtain fully alloyed parts, diffusion during sintering must be understood. An investigation into the effects of current on the diffusion of copper and nickel was performed using SPS. Bulk specimens were used to generate diffusion couples in SPS in alternating orientations with respect to the direction of the current. Control samples were produced using a horizontal insertion vacuum furnace. Experiments were performed at temperatures between 850°C and 1000°C for 3 h. Concentration profiles were obtained by the use of both energy-dispersive spectroscopy and a Monte Carlo simulated correction curve. Diffusion coefficients and activation energies were calculated for samples produced by SPS and annealing without current. It was shown that, at temperatures near 0.9 T{sub m}, the application of current in SPS inhibits diffusion between copper and nickel due to the re-orientation of electrons caused by the loss of ferromagnetism in nickel. Activation energy for diffusion is, however, decreased due to the temperature gradients arising from the difference in resistivity between the two species.

Microstructure and thermal properties of Cu-SiC composite materials depending on the sintering technique

Directory of Open Access Journals (Sweden)

Chmielewski Marcin

2017-01-01

Full Text Available The presented paper investigates the relationship between the microstructure and thermal properties of copper-silicon carbide composites obtained through hot pressing (HP and spark plasma sintering (SPS techniques. The microstructural analysis showed a better densification in the case of composites sintered in the SPS process. TEM investigations revealed the presence of silicon in the area of metallic matrix in the region close to metal-ceramic boundary. It is the product of silicon dissolving process in copper occurring at an elevated temperature. The Cu-SiC interface is significantly defected in composites obtained through the hot pressing method, which has a major influence on the thermal conductivity of materials.

Hexagonal OsB2: Sintering, microstructure and mechanical properties

International Nuclear Information System (INIS)

Xie, Zhilin; Lugovy, Mykola; Orlovskaya, Nina; Graule, Thomas; Kuebler, Jakob; Mueller, Martin; Gao, Huili; Radovic, Miladin; Cullen, David A.

2015-01-01

Highlights: • ReB 2 -type hexagonal OsB 2 powder has been densified by spark plasma sintering. • The sintered OsB 2 contains ∼80 wt.% hexagonal and ∼20 wt.% orthorhombic phases. • The average grain size of the sintered OsB 2 sample was 0.56 ± 0.26 μm. • H = 31 ± 9 GPa and E = 574 ± 112 GPa measured by nanoindentation. - Abstract: The metastable high pressure ReB 2 -type hexagonal OsB 2 bulk ceramics was produced by spark plasma sintering. The phase composition, microstructure, and mechanical behavior of the sintered OsB 2 were studied by X-ray diffraction, optical microscopy, TEM, SEM, EDS, and nanoindentation. The produced ceramics was rather porous and contained a mixture of hexagonal (∼80 wt.%) and orthorhombic (∼20 wt.%) phases as identified by X-ray diffraction and EBSD analysis. Two boron-rich phases, which do not contain Os, were also identified by TEM and SEM/EDS analysis. Nanoindentation measurements yielded a hardness of 31 ± 9 GPa and Young’s modulus of 574 ± 112 GPa, indicating that the material is rather hard and very stiff; however, it is very prone to crack formation and propagation, which is indicative of a very brittle nature of this material. Improvements in the sintering regime are required in order to produce dense, homogeneous and single phase hexagonal OsB 2 bulk ceramics

Sintering studies on iron-carbon-copper compacts

Directory of Open Access Journals (Sweden)

Perianayagam Philomen-D-Anand Raj

2016-01-01

Full Text Available Sintered Iron-Carbon-Copper parts are among the most widely used powder metallurgy product in automobile. In this paper, studies have been carried out to find out the sintering characteristics of iron-carbon-copper compacts when sintered in nitrogen atmosphere. The effects of various processing parameters on the sintering characteristics were studied. The various processing parameters considered were compaction pressure, green density and sintering temperature. The sintering characteristics determined were sintered density, porosity, dimensional change, micro hardness and radial crush strength. The results obtained have been discussed on the basis of micro structural observations. The characteristics of SEM fractography were also used to determine the mechanism of fracture. The fracture energy is strongly dependent on density of the compact.

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

Energy Technology Data Exchange (ETDEWEB)

Oro, Raquel, E-mail: raqueld@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden); Hryha, Eduard, E-mail: hryha@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden); Campos, Mónica, E-mail: campos@ing.uc3m.es [Department of Materials Science and Engineering, IAAB, Universidad Carlos III de Madrid, Av. Universidad 30, 28911 Leganés, Madrid (Spain); Torralba, José M., E-mail: torralba@ing.uc3m.es [Department of Materials Science and Engineering, IAAB, Universidad Carlos III de Madrid, Av. Universidad 30, 28911 Leganés, Madrid (Spain); IMDEA Materials Institute, c/Eric Kandel, 2, 28906 Getafe, Madrid (Spain)

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-ray 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

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

International Nuclear Information System (INIS)

Oro, Raquel; Hryha, Eduard; Campos, Mónica; Torralba, José M.

2014-01-01

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-ray 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

Pressless process in route of obtaining sintered Nd–Fe–B magnets

Energy Technology Data Exchange (ETDEWEB)

Popov, A.G, E-mail: apopov@imp.uran.ru [Institute of Metal Physics, UB of the RAS, 18, S. Kovalevskoy, Street, 620990 Ekaterinburg (Russian Federation); Golovnia, O.A. [Institute of Metal Physics, UB of the RAS, 18, S. Kovalevskoy, Street, 620990 Ekaterinburg (Russian Federation); Bykov, V.A. [Institute of Metallurgy, UB of the RAS, 101, Amundsena, Street, 620016 Ekaterinburg (Russian Federation)

2015-06-01

A short review on the pressless process (PLP) involved in the manufacture of sintered Nd–Fe–B magnet is given. Two approaches to increasing the degree of powder alignment with a high filling density ρ{sub f} in PLP-containers are proposed. (1) An increase in the pulse duration of applied magnetic field from 3.6 to 6.5 ms enhances the magnetic alignment of magnets prepared from the powder with ρ{sub f}=2.5 g/cm{sup 3} and ρ{sub f}=3 g/cm{sup 3} by 3% and 11%, respectively. (2) Addition of internal lubricants such as zinc stearate or esters reduces friction forces between the powder particles and, when the concentration of lubricants is bellow a critical concentration C{sub cr}, increases B{sub r} and (BH){sub max} by 5–7%. Simulation of the magnetic alignment of uniaxial particles demonstrates that a decrease in the coefficient of friction between the powder particles from 0.9 to 0.6 caused by the lubricant addition enhances the alignment degree. Contact dilatometry was used to study the anisotropy of densification of PLP-powders upon sintering. It has been shown that the anisotropy of the powder shrinkage is formed at the first stage of sintering at the temperature about 800 °C and is caused by the capillary action in the Nd-rich liquid. - Highlights: • A review of the pressless process for NdFeB magnets in the world and Russia is given. • Enhancement of the alignment degree by application of pulsed magnetic field is studied. • Reduction of the friction forces via addition of internal lubricants is proposed. • The simulation of the magnetic alignment of Nd–Fe–B uniaxial particles is presented. • A reason of anisotropic shrinkage of the powder at sintering is suggested.

A comparative approach to synthesis and sintering of alumina/yttria nanocomposite powders using different precipitants

Energy Technology Data Exchange (ETDEWEB)

Kafili, G. [Department of Nanotechnology Engineering, Faculty of Advanced Sciences and Technologies, University of Isfahan, Isfahan, 81746-73441 (Iran, Islamic Republic of); Movahedi, B., E-mail: b.movahedi@ast.ui.ac.ir [Department of Nanotechnology Engineering, Faculty of Advanced Sciences and Technologies, University of Isfahan, Isfahan, 81746-73441 (Iran, Islamic Republic of); Milani, M. [Faculty of Advanced Materials and Renewable Energy Research Center, Tehran (Iran, Islamic Republic of)

2016-11-01

Alumina/yttria nanocomposite powder as an yttrium aluminum garnet (YAG) precursor was synthesized via partial wet route using urea and ammonium hydrogen carbonate (AHC) as precipitants, respectively. The products were characterized using X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and energy dispersive spectroscopy. The use of urea produced very tiny spherical Y-compounds with chemical composition of Y{sub 2}(CO{sub 3}){sub 3}·nH{sub 2}O, which were attracted to the surface of alumina nanoparticles and consequently, a core-shell structure was obtained. The use of ammonium hydrogen carbonate produced sheets of Y-compounds with chemical composition of Y(OH)CO{sub 3} covering the alumina nanoparticles. A fine-grained YAG ceramic (about 500 nm), presenting a non-negligible transparency (45% RIT at IR range) was obtained by the spark plasma sintering (SPS) of alumina-yttria nanocomposite synthesized in the urea system. This amount of transmission was obtained by only the sintering of the powder specimen without any colloidal forming process before sintering or adding any sintering aids or dopant elements. However, by spark plasma sintering of alumina-yttria nanocomposite powder synthesized in AHC system, an opaque YAG ceramic with an average grain size of 1.2 μm was obtained. - Highlights: • Urea proved to be an appropriate precipitant for obtaining a core-shell alumina/yttria nanocomposite. • Alumina/yttria nanocomposite powders with more appropriate morphology and highly sinterability. • A fine-grained YAG ceramic was obtained by SPS of alumina-yttria nanocomposite.

Production of Al2O3–SiC nano-composites by spark plasma sintering

International Nuclear Information System (INIS)

Mansour Razavi; Ali Reza Farajipour; Mohammad Zakeri; Mohammad Reza Rahimipour; Ali Reza Firouzbakht

2017-01-01

In this paper, Al2O3–SiC composites were produced by SPS at temperatures of 1600°C for 10min under vacuum atmosphere. For preparing samples, Al2O3 with the second phase including of micro and nano-sized SiC powder were milled for 5h. The milled powders were sintered in a SPS machine. After sintering process, phase studies, densification and mechanical properties of Al2O3–SiC composites were examined. Results showed that the specimens containing micro-sized SiC have an important effect on bulk density, hardness and strength. The highest relative density, hardness and strength were 99.7%, 324.6 HV and 2329MPa, respectively, in Al2O3–20wt% SiCmicro composite. Due to short time sintering, the growth was limited and grains still remained in nano-meter scale. [es

Monitoring Sintering Burn-Through Point Using Infrared Thermography

Directory of Open Access Journals (Sweden)

Francisco G. Bulnes

2013-08-01

Full Text Available Sintering is a complex industrial process that applies heat to fine particles of iron ore and other materials to produce sinter, a solidified porous material used in blast furnaces. The sintering process needs to be carefully adjusted, so that the combustion zone reaches the bottom of the material just before the discharge end. This is known as the burnthrough point. Many different parameters need to be finely tuned, including the speed and the quantities of the materials mixed. However, in order to achieve good results, sintering control requires precise feedback to adjust these parameters. This work presents a sensor to monitor the sintering burn-through point based on infrared thermography. The proposed procedure is based on the acquisition of infrared images at the end of the sintering process. At this position, infrared images contain the cross-section temperatures of the mixture. The objective of this work is to process this information to extract relevant features about the sintering process. The proposed procedure is based on four steps: key frame detection, region of interest detection, segmentation and feature extraction. The results indicate that the proposed procedure is very robust and reliable, providing features that can be used effectively to control the sintering process.

Laser sintering of copper nanoparticles

International Nuclear Information System (INIS)

Zenou, Michael; Saar, Amir; Ermak, Oleg; Kotler, Zvi

2014-01-01

Copper nanoparticle (NP) inks serve as an attractive potential replacement to silver NP inks in functional printing applications. However their tendency to rapidly oxidize has so far limited their wider use. In this work we have studied the conditions for laser sintering of Cu-NP inks in ambient conditions while avoiding oxidation. We have determined the regime for stable, low-resistivity copper (< ×3 bulk resistivity value) generation in terms of laser irradiance and exposure duration and have indicated the limits on fast processing. The role of pre-drying conditions on sintering outcome has also been studied. A method, based on spectral reflectivity measurements, was used for non-contact monitoring of the sintering process evolution. It also indicates preferred spectral regions for sintering. Finally, we illustrated how selective laser sintering can generate high-quality, fine line (<5 µm wide) and dense copper circuits. (paper)

Investigation of the Sintering Process Using Non-Contact Electromagnetic Acoustic Transducers

International Nuclear Information System (INIS)

James C. Foley; David K. Rehbein; Daniel J. Barnard

2001-01-01

In-situ characterizations of green state part density and sintering state have long been desired in the powder metal community. Recent advances in non-contact electromagnetic acoustic transducer (EMAT) technology have enabled in-situ monitoring of acoustic amplitude and velocity as sintering proceeds. Samples were made from elemental powders of Al (99.99%), Al (99.7%), Ag, (99.99%), Cu (99.99%) and Fe (99.9%). The powders were pressed in a uniaxial die and examined with acoustic waves for changes in velocity and amplitude during sintering for the samples containing Al, Ag, and Cu. The changes in acoustic properties were correlated with sample microstructures and mechanical properties. Evolution of a series of reverberating echoes during sintering is shown to provide information on the state of sintering, and changes in sintering kinetics as well as having the potential for detection of interior flaws

Microwave sintering of hydroxyapatite-based composites

International Nuclear Information System (INIS)

Fang, Y.; Roy, D.M.; Cheng, J.; Roy, R.; Agrawal, D.K.

1993-01-01

Composites of hydroxyapatite/partially stabilized zirconia (HAp/PSZ) and hydroxyapatite/silicon carbide whiskers (HAp/SiC) were sintered at 1100-1200 degrees C by microwave at 2.45 GHz. Characterization of the sintered composites was carried out by density, microstructure, phase composition, and fracture toughness measurements. The results show that although not yet fully densified, a much higher sintered density in the HAp/PSZ composite was achieved by microwave sintering than by conventional sintering at the same temperature. A relative density of 93% was achieved by 20 min. microwave processing at 1200 degrees C. Comparatively, 2 h conventional sintering of the same material at 1200 degrees C led to only 75.5% relative density. K IC of this microwave sintered HAp/PSZ of 93% density was found to be 3.88 MPa√m, which is 250% of the value for pure HAp of the same density. A further increase in K IC could be expected if full or nearly full densification was achieved. Sintering of PSZ particles in the HAp/PSZ composite was also observed in the microwave processed sample. Microwave sintering of HAp/SiC was not successful in the current study due to the oxidation of SiC in air at high temperature. 8 refs., 4 figs., 1 tab

Study on the process of sintering matrix metallic Fe-Cu-25%Nb and Fe-Cu-25%Co during hot pressing

International Nuclear Information System (INIS)

Batista, A.C.; Oliveira, H.C.P.; Souza, M.H.; Assis, P.S.

2016-01-01

The sintering process promotes densification and the evolution of the microstructure of the material, with consequent significant increase in hardness and mechanical strength. However, few studies show the influence of pressure and temperature during sintering by hot pressing. In this sense, this work aims to evaluate the microstructural changes and properties with the variation of pressure and temperature and the type suffered by sintering metal powders during sintering by hot pressing. For this, two samples were studied by changing the sintering parameters: 25% Fe-50% Cu-25% Nb and 25% Fe-50% Cu-25% Co. Samples were analyzed by SEM / EDS in order to check the morphology and the presence of pores, as well as the interaction between the metallic constituents of each sample by the EDS analysis in line. They also determined the relative density, porosity and Vickers hardness (HV5). At the end of the study it was concluded that niobium alloy composite element by sintering activated suffered together with the liquid phase sintering. For cobalt alloys were observed by liquid phase sintering. The increase in the severity of the sintering conditions (temperature and pressure) led to an improvement in physical and mechanical properties of the alloys, which indicates that these parameters are directly related to the mechanisms of diffusion in the sintering process, improving the properties and diffusivity between elements. (author)

Process for preparing sintered uranium dioxide nuclear fuel

International Nuclear Information System (INIS)

Carter, R.E.

1975-01-01

Uranium dioxide is prepared for use as fuel in nuclear reactors by sintering it to the desired density at a temperature less than 1300 0 C in a chemically controlled gas atmosphere comprised of at least two gases which in equilibrium provide an oxygen partial pressure sufficient to maintain the uranium dioxide composition at an oxygen/uranium ratio of at least 2.005 at the sintering temperature. 7 Claims, No Drawings

Preparation and Microstructure of Porous ZrB2 Ceramics Using Reactive Spark Plasma Sintering Method

Institute of Scientific and Technical Information of China (English)

YUAN Huiping; LI Junguo; SHEN Qiang; ZHANG Lianmeng

2015-01-01

Zirconium oxide (ZrO2) and boron carbide (B4C) were added to ZrB2 raw powders to prepare ZrB2 porous ceramics by reactive spark plasma sintering (RSPS). The reactions between ZrO2 and B4C which produce ZrB2 and gas (such as CO and B2O3) result in pore formation. X-Ray Diffraction results indicated that the products phase was ZrB2 and the reaction was completed after the RSPS process. The porosity could be controlled by changing the ratio of synthesized ZrB2 to raw ZrB2 powders. The porosity of porous ceramics with 20 wt% and 40 wt% synthsized ZrB2 are 0.185 and 0.222, respectivly. And dense ZrB2-SiC ceramic with a porosity of 0.057 was prepared under the same conditions for comparison. The pores were homogeneously distributed within the microstructure of the porous ceramics. The results indicate a promising method for preparing porous ZrB2-based ceramics.

Spark plasma sintering and porosity studies of uranium nitride

Energy Technology Data Exchange (ETDEWEB)

Johnson, Kyle D., E-mail: kylej@kth.se; Wallenius, Janne; Jolkkonen, Mikael; Claisse, Antoine

2016-05-15

In this study, a number of samples of UN sintered by the SPS method have been fabricated, and highly pure samples ranging in density from 68% to 99.8%TD – corresponding to an absolute density of 14.25 g/cm{sup 3} out of a theoretical density of 14.28 g/cm{sup 3} – have been fabricated. By careful adjustment of the sintering parameters of temperature and applied pressure, the production of pellets of specific porosity may now be achieved between these ranges. The pore closure behaviour of the material has also been documented and compared to previous studies of similar materials, which demonstrates that full pore closure using these methods occurs near 97.5% of relative density. - Highlights: • UN pellets are fabricated over a wide array of densities using the SPS method. • The sintereing parameters necessary to produce pellets over a wide array of density space are charted. • Pellets of extremely high density (99.9% of TD, absolute density of 14.25 g/cm{sup 3}) are fabricated. • Full-closure of the porosity in this material is obtained at around 2.5% of total porosity.

Titanium Metal Powder Production by the Plasma Quench Process

Energy Technology Data Exchange (ETDEWEB)

R. A. Cordes; A. Donaldson

2000-09-01

The goals of this project included the scale-up of the titanium hydride production process to a production rate of 50 kg/hr at a purity level of 99+%. This goal was to be achieved by incrementally increasing the production capability of a series of reactor systems. This methodic approach was designed to allow Idaho Titanium Technologies to systematically address the engineering issues associated with plasma system performance, and powder collection system design and performance. With quality powder available, actual fabrication with the titanium hydride was to be pursued. Finally, with a successful titanium production system in place, the production of titanium aluminide was to be pursued by the simultaneously injection of titanium and aluminum precursors into the reactor system. Some significant accomplishments of the project are: A unique and revolutionary torch/reactor capable of withstanding temperatures up to 5000 C with high thermal efficiency has been operated. The dissociation of titanium tetrachloride into titanium powder and HC1 has been demonstrated, and a one-megawatt reactor potentially capable of producing 100 pounds per hour has been built, but not yet operated at the powder level. The removal of residual subchlorides and adsorbed HC1 and the sintering of powder to form solid bodies have been demonstrated. The production system has been operated at production rates up to 40 pounds per hour. Subsequent to the end of the project, Idaho Titanium Technologies demonstrated that titanium hydride powder can indeed be sintered into solid titanium metal at 1500 C without sintering aids.

Formation of solid solution during mutual diffusion of tungsten and molybdenum in the process of sintering

International Nuclear Information System (INIS)

Timofeeva, A.A.; Bulat, I.B.; Voronin, Yu.V.; Fedoseev, G.K.; Karasev, V.M.

1984-01-01

A process of a solid solution homogenization during sintering of W-15Mo and W-5Mo alloys is studied by the methods of density measurements, analysis of the X-ray lines physical broadening and determination of crystalline lattice constant. Study of the process of solid solution formation under conditions of powder composite sintering is shown to be conducted with account of peculiarities of tungsten and molybdenum mutual diffusion in the investigated temperature range of concentrations

Production of Al2O3–SiC nano-composites by spark plasma sintering

Directory of Open Access Journals (Sweden)

Mansour Razavi

2017-07-01

Full Text Available In this paper, Al2O3–SiC composites were produced by SPS at temperatures of 1600 °C for 10 min under vacuum atmosphere. For preparing samples, Al2O3 with the second phase including of micro and nano-sized SiC powder were milled for 5 h. The milled powders were sintered in a SPS machine. After sintering process, phase studies, densification and mechanical properties of Al2O3–SiC composites were examined. Results showed that the specimens containing micro-sized SiC have an important effect on bulk density, hardness and strength. The highest relative density, hardness and strength were 99.7%, 324.6 HV and 2329 MPa, respectively, in Al2O3–20 wt% SiCmicro composite. Due to short time sintering, the growth was limited and grains still remained in nano-meter scale.

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

Science.gov (United States)

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.

Nanostructured Al/Al4C3 composites reinforced with graphite or fullerene and manufactured by mechanical milling and spark plasma sintering

International Nuclear Information System (INIS)

Robles Hernández, F.C.; Calderon, H.A.

2012-01-01

Highlights: ► Fullerene mix (C 60 + C 70 + soot) is effective to manufacture nanostructured Al/Al 4 C 3 . ► Carbon in the fullerene mix is more reactive with Al that that present in graphite. ► A complete transformation of carbon into Al 4 C 3 is observed in the Al/fullerene. ► Milling and sintering conditions preserve the nanostructured nature of the composites. ► Hardness improvement: 375% Al/graphite and 582% for Al/fullerene composites. - Abstract: Nanostructured Al matrix composites with reinforcements of graphite or fullerene (C 60 + C 70 + soot) have been produced by mechanical milling and spark plasma sintering (SPS). X-ray diffraction and transmission electron microscopy show that C 60 + C 70 withstand longer mechanical milling/alloying times than graphite. Fullerene is a good control agent during mechanical alloying resulting in a denser Al/fullerene composite when compared to the Al/graphite one. A refinement mechanism that takes place during mechanical alloying of fullerene and graphite is experimentally found and correspondingly discussed. Such a mechanism plays a major role in the amorphization of graphite. The larger surface area of the fullerene mix after milling promotes a better interaction with Al and hence allows its complete transformation into Al 4 C 3 during the SPS process. The sintered products show an increase in hardness for the Al/fullerene composite of 6 times and only 4 times for the Al/graphite composite. The SPS technique shows to be an excellent method to transform the fullerene into Al 4 C 3 while preserving its nanostructured nature.

Hexagonal OsB{sub 2}: Sintering, microstructure and mechanical properties

Energy Technology Data Exchange (ETDEWEB)

Xie, Zhilin [Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Lugovy, Mykola [Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Institute for Problems of Materials Science, 3 Krzhizhanivskii Str., Kyiv 03142 (Ukraine); Orlovskaya, Nina, E-mail: Nina.Orlovskaya@ucf.edu [Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Graule, Thomas; Kuebler, Jakob [Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for High Performance Ceramics, CH-8600 Dubendorf (Switzerland); Mueller, Martin [Laboratory of Mechanical Metallurgy, EPFL, CH-1015 Lausanne (Switzerland); Gao, Huili [Department of Mechanical Engineering, Texas A& M University, College Station, TX 77843 (United States); Radovic, Miladin [Department of Materials Science and Engineering, Texas A& M University, College Station, TX 77843 (United States); Cullen, David A. [Materials Science & Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States)

2015-06-15

Highlights: • ReB{sub 2}-type hexagonal OsB{sub 2} powder has been densified by spark plasma sintering. • The sintered OsB{sub 2} contains ∼80 wt.% hexagonal and ∼20 wt.% orthorhombic phases. • The average grain size of the sintered OsB{sub 2} sample was 0.56 ± 0.26 μm. • H = 31 ± 9 GPa and E = 574 ± 112 GPa measured by nanoindentation. - Abstract: The metastable high pressure ReB{sub 2}-type hexagonal OsB{sub 2} bulk ceramics was produced by spark plasma sintering. The phase composition, microstructure, and mechanical behavior of the sintered OsB{sub 2} were studied by X-ray diffraction, optical microscopy, TEM, SEM, EDS, and nanoindentation. The produced ceramics was rather porous and contained a mixture of hexagonal (∼80 wt.%) and orthorhombic (∼20 wt.%) phases as identified by X-ray diffraction and EBSD analysis. Two boron-rich phases, which do not contain Os, were also identified by TEM and SEM/EDS analysis. Nanoindentation measurements yielded a hardness of 31 ± 9 GPa and Young’s modulus of 574 ± 112 GPa, indicating that the material is rather hard and very stiff; however, it is very prone to crack formation and propagation, which is indicative of a very brittle nature of this material. Improvements in the sintering regime are required in order to produce dense, homogeneous and single phase hexagonal OsB{sub 2} bulk ceramics.

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

Science.gov (United States)

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

Processing of a novel nano-structured ferritic steel via spark plasma sintering and investigation of its mechanical and microstructural characteristics

International Nuclear Information System (INIS)

Pasebani, Somayeh; Charit, Indrajit; Wu, Yaqiao; Burns, Jatuporn; Allahar, Kerry N.; Butt, Darryl P.; Cole, James I.

2015-01-01

Nano-structured ferritic steels (NFSs) with 12-14 wt% Cr have attracted widespread interest for potential high temperature structural and fuel cladding applications in advanced nuclear reactors. They have excellent high temperature mechanical properties and high resistance to radiation-induced damage. The properties of the NFSs depend on the composition that mainly consists of Cr, Ti, W or Mo, and Y 2 O 3 as alloying constituents. In this study, a novel nano-structured ferritic steel (Fe-14Cr-1Ti-0.3Mo-0.5La 2 O 3 , wt%) termed as 14LMT was developed via high energy ball milling and spark plasma sintering. Vickers microhardness values were measured. Microstructural studies of the developed NFSs were performed by EBSD and TEM, which revealed a bimodal grain size distribution. A significant number density of nano-precipitates was observed in the microstructure. The diameter of the precipitates varied between 2-70 nm and the morphology from the spherical to faceted shape. The Cr-La-Ti-O-enriched nano-clusters were identified by APT studies. (authors)

Processing and microstructure characterisation of oxide dispersion strengthened Fe–14Cr–0.4Ti–0.25Y2O3 ferritic steels fabricated by spark plasma sintering

International Nuclear Information System (INIS)

Zhang, Hongtao; Huang, Yina; Ning, Huanpo; Williams, Ceri A.; London, Andrew J.; Dawson, Karl; Hong, Zuliang; Gorley, Michael J.; Grovenor, Chris R.M.; Tatlock, Gordon J.; Roberts, Steve G.; Reece, Michael J.; Yan, Haixue; Grant, Patrick S.

2015-01-01

Highlights: • Nanostructured ODS steels were successfully produced by SPS. • Presence of Y 2 Ti 2 O 7 nanoclusters was confirmed by synchrotron XRD and microscopy. • The chemistry of nanoclusters tested by ATP indicated they are Y–Ti–O oxides. - Abstract: Ferritic steels strengthened with Ti–Y–O nanoclusters are leading candidates for fission and fusion reactor components. A Fe–14Cr–0.4Ti + 0.25Y 2 O 3 (14YT) alloy was fabricated by mechanical alloying and subsequently consolidated by spark plasma sintering (SPS). The densification of the 14YT alloys significantly improved with an increase in the sintering temperature. Scanning electron microscopy and electron backscatter diffraction revealed that 14YT SPS-sintered at 1150 °C under 50 MPa for 5 min had a high density (99.6%), a random grain orientation and a bimodal grain size distribution (<500 nm and 1–20 μm). Synchrotron X-ray diffraction patterns showed bcc ferrite, Y 2 Ti 2 O 7 , FeO, and chromium carbides, while transmission electron microscopy and atom probe tomography showed uniformly dispersed Y 2 Ti 2 O 7 nanoclusters of <5 nm diameter and number density of 1.04 × 10 23 m −3 . Due to the very much shorter consolidation times and lower pressures used in SPS compared with the more usual hot isostatic pressing routes, SPS is shown to be a cost-effective technique for oxide dispersion strengthened (ODS) alloy manufacturing with microstructural features consistent with the best-performing ODS alloys

Synthesis of Ti3AlC2 by spark plasma sintering of mechanically milled 3Ti/xAl/2C powder mixtures

International Nuclear Information System (INIS)

Yang Chen; Jin Songzhe; Liang Baoyan; Liu Guojun; Duan Lianfeng; Jia Shusheng

2009-01-01

Elemental powders of Ti, Al and C were mechanically milled as starting materials for the fabrication of ternary carbide Ti 3 AlC 2 by spark plasma sintering (SPS) technique. The effect of Al content in the starting materials on the Ti 3 AlC 2 synthesis was investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were employed to determine the phase identification and observe the microstructure of the synthesized samples. With increasing proper Al content, it was found that the purity of Ti 3 AlC 2 increased and the sintering temperature reduced. The dense and high-purity Ti 3 AlC 2 could be successfully fabricated from 3Ti/1.2Al/2C powders at a lower sintering temperature of 1050 deg. C, holding for 10 min. In addition, the reaction path for the formation of Ti 3 AlC 2 in the present study was proposed

Effect Of Compaction Pressure And Sintering Temperature On The Liquid Phase Sintering Behavior Of Al-Cu-Zn Alloy

Directory of Open Access Journals (Sweden)

Lee S.H.

2015-06-01

Full Text Available The liquid phase sintering characteristics of Al-Cu-Zn alloy were investigated with respect to various powder metallurgy processing conditions. Powders of each alloying elements were blended to form Al-6Cu-5Zn composition and compacted with pressures of 200, 400, and 600 MPa. The sintering process was performed at various temperatures of 410, 560, and 615°C in N2 gas atmosphere. Density and micro-Vickers hardness measurements were conducted at different processing stages, and transverse rupture strength of sintered materials was examined for each condition, respectively. The microstructure was characterized using optical microscope and scanning electron microscopy. The effect of Zn addition on the liquid phase sintering behavior during P/M process of the Al-Cu-Zn alloy was also discussed in detail.

Relación entre los mecanismos de difusión atómica y las propiedades ópticas en la sinterización por Spark Plasma Sintering (SPS de la alúmina.

Directory of Open Access Journals (Sweden)

Torrecillas, R.

2009-12-01

Full Text Available The control of the sintering parameters during spark plasma sintering (SPS of polycrystalline alumina allows modifying the contribution due to the different atomic diffusion mechanisms. Thus, changing the heating rate as a function of the sintering stage allows tailoring sintering cycles that optimize the final density of the material with a minimal grain growth. It is shown in this work how by using two heating rates, 100 and 4ºC/min, allows obtaining a polycrystalline transparent alumina with a higher real in-line transmittance than that obtained with constant heating rates sintering cycles.

El control de los parámetros de sinterización de la alúmina policristalina por spark plasma sintering (SPS permite modificar la contribución de los diferentes mecanismos de difusión atómica. Así, variar la rampa de calentamiento en función de la etapa de sinterización permite diseñar ciclos de sinterización que optimizan la densidad final del material con un mínimo crecimiento de grano. En este trabajo se demuestra cómo empleando dos velocidades, 100 y 4ºC/min, es posible obtener una alúmina policristalina con una transmitancia real en línea superior a la obtenida en ciclos con rampas constantes.

Densification of LSGM electrolytes using activated microwave sintering

Science.gov (United States)

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).

Reaction behavior of SO2 in the sintering process with flue gas recirculation.

Science.gov (United States)

Yu, Zhi-Yuan; Fan, Xiao-Hui; Gan, Min; Chen, Xu-Ling; Chen, Qiang; Huang, Yun-Song

2016-07-01

The primary goal of this paper is to reveal the reaction behavior of SO2 in the sinter zone, combustion zone, drying-preheating zone, and over-wet zone during flue gas recirculation (FGR) technique. The results showed that SO2 retention in the sinter zone was associated with free-CaO in the form of CaSO3/CaSO4, and the SO2 adsorption reached a maximum under 900ºC. SO2 in the flue gas came almost from the combustion zone. One reaction behavior was the oxidation of sulfur in the sintering mix when the temperature was between 800 and 1000ºC; the other behavior was the decomposition of sulfite/sulfate when the temperature was over 1000ºC. However, the SO2 adsorption in the sintering bed mainly occurred in the drying-preheating zone, adsorbed by CaCO3, Ca(OH)2, and CaO. When the SO2 adsorption reaction in the drying-preheating zone reached equilibrium, the excess SO2 gas continued to migrate to the over-wet zone and was then absorbed by Ca(OH)2 and H2O. The emission rising point of SO2 moved forward in combustion zone, and the concentration of SO2 emissions significantly increased in the case of flue gas recirculation (FGR) technique. Aiming for the reuse of the sensible heat and a reduction in exhaust gas emission, the FGR technique is proposed in the iron ore sintering process. When using the FGR technique, SO2 emission in exhaust gas gets changed. In practice, the application of the FGR technique in a sinter plant should be cooperative with the flue gas desulfurization (FGD) technique. Thus, it is necessary to study the influence of the FGR technique on SO2 emissions because it will directly influence the demand and design of the FGD system.

The Influence of Milling and Spark Plasma Sintering on the Microstructure and Properties of the Al7075 Alloy

Science.gov (United States)

Málek, Přemysl; Minárik, Peter; Novák, Pavel; Průša, Filip

2018-01-01

The compact samples of an Al7075 alloy were prepared by a combination of gas atomization, high energy milling, and spark plasma sintering. The predominantly cellular morphology observed in gas atomized powder particles was completely changed by mechanical milling. The continuous-like intermetallic phases present along intercellular boundaries were destroyed; nevertheless, a small amount of Mg(Zn,Cu,Al)2 phase was observed also in the milled powder. Milling resulted in a severe plastic deformation of the material and led to a reduction of grain size from several µm into the nanocrystalline region. The combination of these microstructural characteristics resulted in abnormally high microhardness values exceeding 300 HV. Consolidation through spark plasma sintering (SPS) resulted in bulk samples with negligible porosity. The heat exposition during SPS led to precipitation of intermetallic phases from the non-equilibrium microstructure of both gas atomized and milled powders. SPS of the milled powder resulted in a recrystallization of the severely deformed structure. An ultra-fine grained structure (grain size close to 500 nm) with grains divided primarily by high-angle boundaries was formed. A simultaneous release of stored deformation energy and an increase in the grain size caused a drop of microhardness to values close to 150 HV. This value was retained even after annealing at 425 °C. PMID:29614046

The Influence of Milling and Spark Plasma Sintering on the Microstructure and Properties of the Al7075 Alloy

Directory of Open Access Journals (Sweden)

Orsolya Molnárová

2018-04-01

Full Text Available The compact samples of an Al7075 alloy were prepared by a combination of gas atomization, high energy milling, and spark plasma sintering. The predominantly cellular morphology observed in gas atomized powder particles was completely changed by mechanical milling. The continuous-like intermetallic phases present along intercellular boundaries were destroyed; nevertheless, a small amount of Mg(Zn,Cu,Al2 phase was observed also in the milled powder. Milling resulted in a severe plastic deformation of the material and led to a reduction of grain size from several µm into the nanocrystalline region. The combination of these microstructural characteristics resulted in abnormally high microhardness values exceeding 300 HV. Consolidation through spark plasma sintering (SPS resulted in bulk samples with negligible porosity. The heat exposition during SPS led to precipitation of intermetallic phases from the non-equilibrium microstructure of both gas atomized and milled powders. SPS of the milled powder resulted in a recrystallization of the severely deformed structure. An ultra-fine grained structure (grain size close to 500 nm with grains divided primarily by high-angle boundaries was formed. A simultaneous release of stored deformation energy and an increase in the grain size caused a drop of microhardness to values close to 150 HV. This value was retained even after annealing at 425 °C.

Sintering of beryllium oxide

International Nuclear Information System (INIS)

Caillat, R.; Pointud, R.

1955-01-01

This study had for origin to find a process permitting to manufacture bricks of beryllium oxide of pure nuclear grade, with a density as elevated as possible and with standardized shape. The sintering under load was the technique kept for the manufacture of the bricks. Because of the important toxicity of the beryllium oxide, the general features for the preliminary study of the sintering, have been determined while using alumina. The obtained results will be able to act as general indication for ulterior studies with sintering under load. (M.B.) [fr

Effects of V{sub 2}O{sub 5} addition on NiZn ferrite synthesized using two-step sintering process

Energy Technology Data Exchange (ETDEWEB)

Hu Jun [College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310032 (China); State Key Laboratory of Silicon Materials, Zhejiang University, Hangzhou 310027 (China); Shi Gang; Ni Zheming; Zheng Li [College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310032 (China); Chen Aimin, E-mail: hjzjut@zjut.edu.cn [College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310032 (China)

2012-06-15

The combined influence of a two-step sintering (TSS) process and addition of V{sub 2}O{sub 5} on the microstructure and magnetic properties of NiZn ferrite was investigated. As comparison, samples prepared by the conventional single-step sintering (SSS) procedure were also studied. It was found that with 0.3 wt% V{sub 2}O{sub 5} additive, the sample sintered by the two-step sintering process at a high temperature of 1250 Degree-Sign C for 30 min and a lower temperature of 1180 Degree-Sign C for 3 h exhibited more homogeneous microstructure and higher permeability with a high Q-factor. The results showed that the TSS method with suitable additive brought positive improvement of the microstructure and magnetic properties of NiZn ferrite.

Microstructure and mechanical strength of near- and sub-micrometre grain size copper prepared by spark plasma sintering

DEFF Research Database (Denmark)

Zhu, K. N.; Godfrey, A.; Hansen, Niels

2017-01-01

Spark plasma sintering (SPS) has been used to prepare fully dense samples of copper in a fully recrystallized condition with grain sizes in the near- and sub-micrometre regime. Two synthesis routes have been investigated to achieve grain size control: (i) SPS at different temperatures from 800...... transmission electron microscope, and on electron back-scatter diffraction studies, confirms the samples are in a nearly fully recrystallized condition, with grains that are dislocation-free, and have a random texture, with a high fraction of high angle boundaries. The mechanical strength of the samples has...

High temperature oxidation-sulfidation behavior of Cr-Al2O3 and Nb-Al2O3 composites densified by spark plasma sintering

International Nuclear Information System (INIS)

Saucedo-Acuna, R.A.; Monreal-Romero, H.; Martinez-Villafane, A.; Chacon-Nava, J.G.; Arce-Colunga, U.; Gaona-Tiburcio, C.; De la Torre, S.D.

2007-01-01

The high temperature oxidation-sulfidation behavior of Cr-Al 2 O 3 and Nb-Al 2 O 3 composites prepared by mechanical alloying (MA) and spark plasma sintering (SPS) has been studied. These composite powders have a particular metal-ceramic interpenetrating network and excellent mechanical properties. Oxidation-sulfidation tests were carried out at 900 deg. C, in a 2.5%SO 2 + 3.6%O 2 + N 2 (balance) atmosphere for 48 h. The results revealed the influence of the sintering conditions on the specimens corrosion resistance, i.e. the Cr-Al 2 O 3 and Nb-Al 2 O 3 composite sintered at 1310 deg. C/4 min showed better corrosion resistance (lower weight gains) compared with those found for the 1440 deg. C/5 min conditions. For the former composite, a protective Cr 2 O 3 layer immediately forms upon heating, whereas for the later pest disintegration was noted. Thus, under the same sintering conditions the Nb-Al 2 O 3 composites showed the highest weight gains. The oxidation products were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy

Bridge between fusion plasma and plasma processing

International Nuclear Information System (INIS)

Ohno, Noriyasu; Takamura, Shuichi

2008-01-01

In the present review, relationship between fusion plasma and processing plasma is discussed. From boundary-plasma studies in fusion devices new applications such as high-density plasma sources, erosion of graphite in a hydrogen plasma, formation of helium bubbles in high-melting-point metals and the use of toroidal plasmas for plasma processing are emerging. The authors would like to discuss a possibility of knowledge transfer from fusion plasmas to processing plasmas. (T. Ikehata)

Sintering process of Eu doped luminescent glass prepared from porous glass

International Nuclear Information System (INIS)

Akai, T; Murakami, M; Yamashita, M; Okajima, T; Umesaki, N

2011-01-01

Eu doped high silica glass prepared by sintering porous glass exhibits blue luminescence with high quantum efficiency. In this work, we studied effects of sintering temperature on valance state of europium ion. To investigate a change of valance state of Eu, X-ray absorption near edge structure (XANES) spectroscopy measurements were carried out. Intensity of blue emission at around 430nm drastically increases when the sintering temperature is above 1000 deg. C. From XANES spectra, it is found that almost all the Eu exist as Eu 3+ in a samples sintered below 900 deg. C, while more than 70% of Eu exist as Eu 2+ in the sample sintered at 1050 deg. C and 1100 deg. C. The drastic change of oxidation state of europium ion between 900 and 1050 deg. C is discussed in relation to the structural change probed by infrared (IR) spectroscopy.

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

Science.gov (United States)

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

2017-08-01

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

Sintering of a class F fly ash

Energy Technology Data Exchange (ETDEWEB)

Joseph J. Biernacki; Anil K. Vazrala; H. Wayne Leimer [Tennessee Technological University, Cookeville, TN (United States). Department of Chemical Engineering

2008-05-15

The sinterability of a class F fly ash was investigated as a function of processing conditions including sintering temperature (1050-1200{sup o}C) and sintering time (0-90 min). Density, shrinkage, splitting tensile strength, water absorption and residual loss on ignition (RLOI) were evaluated as measures of sintering efficiency. Scanning electron microscopy (SEM), X-ray microanalysis and X-ray diffraction was used to examine microstructure and phase development due to processing. The results show that premature densification can inhibit complete carbon removal and that carbon combustion is influenced by both internal and external mass transfer conditions. 18 refs., 10 figs., 1 tab.

The spatial distribution of temperature and oxygen deficiency in spark-plasma sintered superconducting Bi-based materials

International Nuclear Information System (INIS)

Govea-Alcaide, E.; Pérez-Fernández, J.E.; Machado, I.F.; Jardim, R.F.

2014-01-01

Pre-reacted powders of (Bi–Pb) 2 Sr 2 Ca 2 Cu 3 O 10+δ (Bi-2223) were consolidated by using the spark plasma sintering (SPS) technique under vacuum and at different consolidate temperatures T D . X-ray diffraction patterns revealed that the dominant phase in all SPS samples is the Bi-2223 phase, but traces of the Bi 2 Sr 2 CaCu 2 O 10+x (Bi-2212) phase were identified. We have found that the transport properties of SPS samples depend on their oxygen content because the SPS process is performed under vacuum. Simulations by using the finite element method (FEM) were performed for determining the actual temperature in which powders are consolidated. From these results we have inferred that SPS samples are oxygen deficient and such a deficiency is more marked near the grain boundaries, suggesting the occurrence of grains with core–shell morphology. We also argued that the width of the shell depends on the consolidation temperature, a feature corroborated by the FEM simulations

Strain-enhanced sintering of iron powders

Energy Technology Data Exchange (ETDEWEB)

Amador, D.R.; Torralba, J.M. [Universidad Carlos III de Madrid, Departamento de Ciencias de Materiales e Ingenieria Metalurgica, Leganes, Madrid (Spain); Monge, M.A.; Pareja, R. [Universidad Carlos III de Madrid, Departamento de Fisica, Madrid (Spain)

2005-02-01

Sintering of ball-milled and un-milled Fe powders has been investigated using dilatometry, X-ray, density, and positron annihilation techniques. A considerable sintering enhancement is found in milled powders showing apparent activation energies that range between 0.44 and 0.80 eV/at. The positron annihilation results, combined with the evolution of the shrinkage rate with sintering temperature, indicate generation of lattice defects during the sintering process of milled and un-milled powders. The sintering enhancement is attributed to pipe diffusion along the core of moving dislocations in the presence of the vacancy excess produced by plastic deformation. Positron annihilation results do not reveal the presence of sintering-induced defects in un-milled powders sintered above 1200 K, the apparent activation energy being in good agreement with that for grain-boundary diffusion in {gamma}-Fe. (orig.)

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

Science.gov (United States)

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 (uranium with small quantities of dissolved Si and Mo at the front of the reaction.

Low modulus and bioactive Ti/α-TCP/Ti-mesh composite prepared by spark plasma sintering.

Science.gov (United States)

Guo, Yu; Tan, Yanni; Liu, Yong; Liu, Shifeng; Zhou, Rui; Tang, Hanchun

2017-11-01

A titanium mesh scaffold composite filled with Ti/α-TCP particles was prepared by spark plasma sintering (SPS). The microstructures and interfacial reactions of the composites were investigated by scanning electron microscopy (SEM), Energy Dispersive Spectroscopy (EDS) and X-ray diffraction (XRD) analyses. The compressive strength and elastic modulus were also measured. In vitro bioactivity and biocompatibility was evaluated by using simulated body fluid and cells culture, respectively. After high temperature sintering, Ti oxides, Ti x P y and CaTiO 3 were formed. The formation of Ti oxides and Ti x P y were resulted from the diffusion of O and P elements from α-TCP to Ti. CaTiO 3 was the reaction product of Ti and α-TCP. The composite of 70Ti/α-TCP incorporated with Ti mesh showed a high compressive strength of 589MPa and a low compressive modulus of 30GPa. The bioactivity test showed the formation of a thick apatite layer on the composite and well-spread cells attachment. A good combination of mechanical properties and bioactivity indicated a high potential application of Ti/α-TCP/Ti-mesh composite for orthopedic implants. Copyright © 2017. Published by Elsevier B.V.

Sintering and densification; new techniques: sinter forging

International Nuclear Information System (INIS)

Winnubst, A.J.A.

1998-01-01

In this chapter pressure assisted sintering methods will be described. Attention will mainly be paid to sinter forging as a die-wall free uniaxial pressure sintering technique, where large creep strains are possible. Sinter forging is an effective tool to reduce sintering temperature and time and to obtain a nearly theoretically dense ceramic. In this way grain size in tetragonal zirconia ceramics can be reduced down to 100 nm. Another important phenomenon is the reduction of the number density and size of cracks and flaws resulting in higher strength and improved reliability, which is of utmost importance for engineering ceramics. The creep deformation during sinter forging causes a rearrangement of the grains resulting in a reduction of interatomic spaces between grains, while grain boundary (glassy) phases can be removed. The toughness and in some cases the wear resistance is enhanced after sinter forging as a result of the grain-boundary-morphology improvement. (orig.)

Preparation of (Bi, Pb)-2223/Ag tapes by high temperature sintering and post-annealing process

DEFF Research Database (Denmark)

Hua, L.; Grivel, Jean-Claude; Andersen, L.G.

2002-01-01

A novel heat treatment process was developed to fabricate (Bi, Pb)-2223/Ag tapes with high critical current density (J(c)). The process can be divided into two parts: reformation and post-annealing. Tapes were first heated to the maximum temperature (830-860 degreesC) followed by slow cooling...... (reformation). Then, tape, were annealed between 760 and 820 degreesC (post-annealing). Reformation is expected to produce a large amount of liquid phase which may heat microcracks, decrease porosity, and improve grain growth. However, since the sintering temperature is beyond the Bi-2223 single-phase region......-energy synchrotron XRD and SEM/EDX. Some process parameters e.g. sintering temperature. cooling rate. and post-annealing time were optimised. (C) 2002 Elsevier Science B.V. All rights reserved....

Phase and Microstructural Correlation of Spark Plasma Sintered HfB2-ZrB2 Based Ultra-High Temperature Ceramic Composites

Directory of Open Access Journals (Sweden)

Ambreen Nisar

2017-07-01

Full Text Available The refractory diborides (HfB2 and ZrB2 are considered as promising ultra-high temperature ceramic (UHTCs where low damage tolerance limits their application for the thermal protection system in re-entry vehicles. In this regard, SiC and CNT have been synergistically added as the sintering aids and toughening agents in the spark plasma sintered (SPS HfB2-ZrB2 system. Herein, a novel equimolar composition of HfB2 and ZrB2 has shown to form a solid-solution which then allows compositional tailoring of mechanical properties (such as hardness, elastic modulus, and fracture toughness. The hardness of the processed composite is higher than the individual phase hardness up to 1.5 times, insinuating the synergy of SiC and CNT reinforcement in HfB2-ZrB2 composites. The enhanced fracture toughness of CNT reinforced composite (up to a 196% increment surpassing that of the parent materials (ZrB2/HfB2-SiC is attributed to the synergy of solid solution formation and enhanced densification (~99.5%. In addition, the reduction in the analytically quantified interfacial residual tensile stress with SiC and CNT reinforcements contribute to the enhancement in the fracture toughness of HfB2-ZrB2-SiC-CNT composites, mandatory for aerospace applications.

Characterization and mechanical testing of alumina-based nanocomposites reinforced with niobium and/or carbon nanotubes fabricated by spark plasma sintering

International Nuclear Information System (INIS)

Thomson, K.E.; Jiang, D.; Yao, W.; Ritchie, R.O.; Mukherjee, A.K.

2012-01-01

Alumina-based nanocomposites reinforced with niobium and/or carbon nanotubes (CNT) were fabricated by advanced powder processing techniques and consolidated by spark plasma sintering. Raman spectroscopy revealed that single-walled carbon nanotubes (SWCNT) begin to break down at sintering temperatures >1150 °C. Nuclear magnetic resonance showed that, although thermodynamically unlikely, no Al 4 C 3 formed in the CNT–alumina nanocomposites, such that the nanocomposite can be considered as purely a physical mixture with no chemical bond formed between the nanotubes and ceramic matrix. In addition, in situ single-edge notched bend tests were conducted on niobium and/or CNT-reinforced alumina nanocomposites to assess their toughness. Despite the absence of subcritical crack growth, average fracture toughness values of 6.1 and 3.3 MPa m 1/2 were measured for 10 vol.% Nb and 10 vol.% Nb–5 vol.% SWCNT–alumina, respectively. Corresponding tests for the alumina nanocomposites containing 5 vol.% SWCNT, 10 vol.% SWCNT, 5 vol.% double-walled-CNT and 10 vol.% Nb yielded average fracture toughnesses of 3.0, 2.8, 3.3 and 4.0 MPa m 1/2 , respectively. It appears that the reason for not observing improvement in fracture toughness of CNT-reinforced samples is because of either damage to CNTs or possibly non-optimal interfacial bonding between CNT-alumina.

Pore Formation Process of Porous Ti3SiC2 Fabricated by Reactive Sintering

Directory of Open Access Journals (Sweden)

Huibin Zhang

2017-02-01

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

Functionalization of polymer powders for SLS-processes using an atmospheric plasma jet in a fluidized bed reactor

Energy Technology Data Exchange (ETDEWEB)

Sachs, Marius; Schmitt, Adeliene; Schmidt, Jochen; Peukert, Wolfgang; Wirth, Karl-Ernst [Institute of Particle Technology, Friedrich-Alexander-University Erlangen-Nuremberg (Germany)

2015-05-22

Recently additive manufacturing processes such as selective laser sintering (SLS) of polymers have gained more importance for industrial applications [1]. Tailor-made modification of polymers is essential in order to make these processes more efficient and to cover the industrial demands. The so far used polymer materials show weak performance regarding the mechanical stability of processed parts. To overcome this limitation, a new route to functionalize the surface of commercially available polymer particles (PA12; PE-HD; PP) using an atmospheric plasma jet in combination with a fluidized bed reactor has been investigated. Consequently, an improvement of adhesion and wettability [2] of the polymer surface without restraining the bulk properties of the powder is achieved. The atmospheric plasma jet process can provide reactive species at moderate temperatures which are suitable for polymer material. The functionalization of the polymer powders improves the quality of the devices build in a SLS-process.

Modeling of sintering of functionally gradated materials

International Nuclear Information System (INIS)

Gasik, M.; Zhang, B.

2001-01-01

The functionally gradated materials (FGMs) are distinguished from isotropic materials by gradients of composition, phase distribution, porosity, and related properties. For FGMs made by powder metallurgy, sintering control is one of the most important factors. In this study sintering process of FGMs is modeled and simulated with a computer. A new modeling approach was used to formulate equation systems and the model for sintering of gradated hard metals, coupled with heat transfer and grain growth. A FEM module was developed to simulate FGM sintering in conventional, microwave and hybrid conditions, to calculate density, stress and temperature distribution. Behavior of gradated WC-Co hardmetal plate and cone specimens was simulated for various conditions, such as mean particle size, green density distribution and cobalt gradation parameter. The results show that the deformation behavior and stress history of graded powder compacts during heating, sintering and cooling could be predicted for optimization of sintering process. (author)

Mechanical and magnetic properties of semi-Heusler/light-metal composites consolidated by spark plasma sintering

Czech Academy of Sciences Publication Activity Database

Koller, M.; Chráska, Tomáš; Cinert, Jakub; Heczko, Oleg; Kopeček, Jaromír; Landa, Michal; Mušálek, Radek; Rameš, Michal; Seiner, Hanuš; Stráský, J.; Janeček, M.

2017-01-01

Roč. 126, July (2017), s. 351-357 ISSN 0264-1275 R&D Projects: GA ČR GB14-36566G Institutional support: RVO:61389021 ; RVO:68378271 ; RVO:61388998 Keywords : Metal–metal composites * Spark plasma sintering * Light metals * Ferromagnetic alloys * Mechanical properties Subject RIV: JI - Composite Materials; JI - Composite Materials (FZU-D); JI - Composite Materials (UT-L) OBOR OECD: Composites (including laminates, reinforced plastics, cermets, combined natural and synthetic fibre fabrics; Composites (including laminates, reinforced plastics, cermets, combined natural and synthetic fibre fabrics (FZU-D); Composites (including laminates, reinforced plastics, cermets, combined natural and synthetic fibre fabrics (UT-L) Impact factor: 4.364, year: 2016 https://www.sciencedirect.com/science/ article /pii/S0264127517303842?via%3Dih

Faceted shell structure in grain boundary diffusion-processed sintered Nd–Fe–B magnets

International Nuclear Information System (INIS)

Seelam, U.M.R.; Ohkubo, T.; Abe, T.; Hirosawa, S.; Hono, K.

2014-01-01

Graphical abstract: The grain boundary diffusion process (GBDP) using a heavy rare earth elements (HRE) such as Dy and Tb is known as an effective method to enhance the coercivity of Nd–Fe–B sintered magnets without reducing remanence. This process has been industrially implemented to manufacture Nd–Fe–B based sintered magnets with high coercivity and high remanence. In this process, Dy is considered to diffuse through grain boundaries (GBs) to form (Nd 1−x Dy x ) 2 Fe 14 B shells surrounding the Nd 2 Fe 14 B grains and the higher anisotropy field of the Dy-rich shell is considered to suppress the nucleation of reverse domains at low magnetic field. Although there are several investigations on the microstructure of HRE GBDP Nd–Fe–B magnets, no paper addressed the origin of the asymmetric formation of HRE rich shells. Based on detailed analysis of facet planes of core/shell interfaces, we propose a mechanism of the faceted core/shell microstructure formation in the GBDP sintered magnets. We believe that this gives new insights on understanding the coercivity enhancement by the GBDP. - Highlights: • Faceting was observed at the interfaces of cores and shells. • The core/shell interfaces are sharp with an abrupt change in Dy concentration. • Meting occurs at the interfaces of metalic Nd-rich/Nd 2 Fe 14 B phases above 685 °C due to eutectic reaction. • Solidification of Dy-enriched liquid phase from 900 °C can result in the shell formation. - Abstract: Dysprosium enriched shell structure formed by the grain boundary diffusion process (GBDP) of a sintered Nd–Fe–B magnet was characterized by using scanning electron microscopy, electron back-scattered diffraction and transmission electron microscopy. Faceted core–shell interfaces with an abrupt change in Dy concentration suggest the Dy-rich shells are formed by the solidification of the liquid phase during cooling from the GBDP temperature. The Nd-rich phases are almost free from Dy, and

Hydrothermal Cold Sintering

Science.gov (United States)

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 �

Influence of spark plasma sintering parameters on the mechanical properties of Cu{sub 50}Zr{sub 45}Al{sub 5} bulk metallic glass obtained using metallic glass powder

Energy Technology Data Exchange (ETDEWEB)

Cardinal, S. [Université de Lyon, CNRS (France); INSA-Lyon, MATEIS UMR5510, F-69621 Villeurbanne (France); Pelletier, J.M., E-mail: jean-marc.pelletier@insa-lyon.fr [Université de Lyon, CNRS (France); INSA-Lyon, MATEIS UMR5510, F-69621 Villeurbanne (France); Qiao, J.C. [School of Mechanics, Civil Engineering and Architecture, Northwestern Polytechnical University, Xi’an 710072 (China); Bonnefont, G. [Université de Lyon, CNRS (France); INSA-Lyon, MATEIS UMR5510, F-69621 Villeurbanne (France); Xie, G. [Institute for Materials Research, Tohoku University, Sendai (Japan)

2016-11-20

Gas atomized Cu{sub 50}Zr{sub 45}Al{sub 5} amorphous powder was densified by spark plasma sintering, in order to obtain bulk metallic glasses with larger size than that obtained by the conventional casting strategy. The influence of different parameters was investigated: sintering temperature, isothermal holding time as well as size of the specimens. After optimization of the processing parameters, dense and amorphous specimens were elaborated with a diameter up to 30 mm. Thermal stability and mechanical properties of consolidated samples are similar to those of Cu{sub 50}Zr{sub 45} Al{sub 5} cast alloy. A hardness of 535 HV and a compressive strength of 1600 MPa have been obtained. Fractographic investigation indicated an intergranular rupture mode which leads to lower toughness compared to as the cast material, but for these samples the size is limited to 3 mm. However an increase in applied pressure (from 90 MPa to 1 GPa) induces a significant improvement in bonding between powder particles.

Hot pressing of nanocrystalline tantalum using high frequency induction heating and pulse plasma sintering

Science.gov (United States)

Jakubowicz, J.; Adamek, G.; Sopata, M.; Koper, J. K.; Siwak, P.

2017-12-01

The paper presents the results of nanocrystalline powder tantalum consolidation using hot pressing. The authors used two different heating techniques during hot pressing: high-frequency induction heating (HFIH) and pulse plasma sintering (PPS). A comparison of the structure, microstructure, mechanical properties and corrosion resistance of the bulk nanocrystalline tantalum obtained in both techniques was performed. The nanocrystalline powder was made to start from the microcrystalline one using the high-energy ball milling process. The nanocrystalline powder was hot-pressed at 1000 °C, whereas, for comparison, the microcrystalline powder was hot pressed up to 1500 °C for proper consolidation. The authors found that during hot pressing, the powder partially reacts with the graphite die covered by boron nitride, which facilitated punches and powder displacement in the die during densification. Tantalum carbide and boride in the nanocrystalline material was found, which can improve the mechanical properties. The hardness of the HFIH and PPS nanocrystalline tantalum was as high as 625 and 615 HV, respectively. The microstructure was more uniform in the PPS nanomaterial. The corrosion resistance in both cases deteriorated, in comparison to the microcrystalline material, while the PPS material corrosion resistance was slightly better than that of the HFIH one.

Sintering behavior and thermal conductivity of nickel-coated graphite flake/copper composites fabricated by spark plasma sintering

Science.gov (United States)

Xu, Hui; Chen, Jian-hao; Ren, Shu-bin; He, Xin-bo; Qu, Xuan-hui

2018-04-01

Nickel-coated graphite flakes/copper (GN/Cu) composites were fabricated by spark plasma sintering with the surface of graphite flakes (GFs) being modified by Ni-P electroless plating. The effects of the phase transition of the amorphous Ni-P plating and of Ni diffusion into the Cu matrix on the densification behavior, interfacial microstructure, and thermal conductivity (TC) of the GN/Cu composites were systematically investigated. The introduction of Ni-P electroless plating efficiently reduced the densification temperature of uncoated GF/Cu composites from 850 to 650°C and slightly increased the TC of the X-Y basal plane of the GF/Cu composites with 20vol%-30vol% graphite flakes. However, when the graphite flake content was greater than 30vol%, the TC of the GF/Cu composites decreased with the introduction of Ni-P plating as a result of the combined effect of the improved heat-transfer interface with the transition layer, P generated at the interface, and the diffusion of Ni into the matrix. Given the effect of the Ni content on the TC of the Cu matrix and on the interface thermal resistance, a modified effective medium approximation model was used to predict the TC of the prepared GF/Cu composites.

End Uses Mechanical Properties Settled By The Modified Sintering Conditions Of The Metal Injection Molding Process

International Nuclear Information System (INIS)

Marray, Tarek; Jaccquet, Philippe; Moinard-Checot, Delphine; Fabre, Agnes; Barrallier, Laurent

2011-01-01

Most common mechanical applications require parts with specific properties as hard faced features. It is well known that treating parts under suitable atmospheres may improve hardness and strength yield of steels. Heat treatment process and more particularly thermo-chemical diffusion processes (such as carburizing or its variation: carbonitriding) can be performed to reach the industrial hardness profile requirements. In this work, a low-alloyed steel feedstock based on water soluble binder system is submitted to the MIM process steps (including injection molding, debinding and sintering). As-sintered parts are then treated under a low pressure carbonitriding treatment. This contribution focuses on preliminary results such as microstructural analyses and mechanical properties which are established at each stage of the process to determine and monitor changes.

Fabrication of Li_2TiO_3 pebbles by a selective laser sintering process

International Nuclear Information System (INIS)

Zhou, Qilai; Gao, Yue; Liu, Kai; Xue, Lihong; Yan, Youwei

2015-01-01

Highlights: • Selective laser sintering (SLS) is employed to fabricate ceramic pebbles. • Quantities and diameter of the pebbles could be easily controlled by adjusting the model of pebbles. • All the pebbles could be prepared at a time within several minutes. • The Li_2TiO_3 pebbles sintered at 1100 °C show a notable crush load of 43 N. - Abstract: Lithium titanate, Li_2TiO_3, is an important tritium breeding material for deuterium (D)–tritium (T) fusion reactor. In test blanket module (TBM) design of China, Li_2TiO_3 is considered as one candidate material of tritium breeders. In this study, selective laser sintering (SLS) technology was introduced to fabricate Li_2TiO_3 ceramic pebbles. This fabrication process is computer assisted and has a high level of flexibility. Li_2TiO_3 powder with a particle size of 1–3 μm was used as the raw material, whilst epoxy resin E06 was adopted as a binder. Green Li_2TiO_3 pebbles with certain strengths were successfully prepared via SLS. Density of the green pebbles was subsequently increased by cold isostatic pressing (CIP) process. Li_2TiO_3 pebbles with a diameter of about 2 mm were obtained after high temperature sintering. Density of the pebbles reaches 80% of theoretical density (TD) with a comparable crush load of 43 N. This computer assisted approach provides a new efficient route for the production of Li_2TiO_3 ceramic pebbles.

Investigation of the sintering mechanisms for (U,Am)O{sub 2} pellets obtained by CRMP process

Energy Technology Data Exchange (ETDEWEB)

Caisso, M. [CEA, Centre de Marcoule, DEN, DTEC/SECA/LFC, F-30207 Bagnols-sur-Ceze (France); CEA, Centre de Marcole, DEN, DRCP/SERA/LCAR, F-30207 Bagnols-sur-Ceze (France); Institut Europeen des Membranes, UMR 5635 CNRS-ENSCM-UM, CC047, Campus Triolet, Universite de Montpellier, F-34095 Montpellier Cedex 5 (France); Boulesteix, R.; Maitre, A. [SPCTS, UMR 7315 CNRS-Universite de Limoges-ENSCI, Centre Europeen de la Ceramique, 12 Rue Atlantis, F-87068 Limoges (France); Picart, S.; Delahaye, T. [CEA, Centre de Marcole, DEN, DRCP/SERA/LCAR, F-30207 Bagnols-sur-Ceze Cedex (France); Ayral, A. [Institut Europeen des Membranes, UMR 5635 CNRS-ENSCM-UM, CC047, Campus Triolet Universite de Montpellier, F-34095 Montpellier Cedex 5 (France)

2016-07-01

The use of CRMP (Calcined Resin Microsphere Pelletization) process for AmBB (Americium Bearing Blankets) fabrication is today a key research axis in americium transmutation domain, where its very high activity requires minimization of powder dissemination. In this aim, the use of oxide microspheres as compaction precursors is a promising clean alternative to powder metallurgy. Understanding the different steps of densification during CRMP pellet sintering thus appears as fundamental to obtain final materials with the specific features required for AmBB. The densification curve recorded in dynamic conditions shows different sintering steps. A first decrease of shrinkage rate happens at low temperature, around 1100 K. This phenomenon is not normally observed in the sintering of conventional powders. Chemical and microstructural studies were performed on (U,Am)O{sub 2} and also on (Ce,Gd)O{sub 2} surrogate compound to highlight the causes of this low-temperature sintering step. Multi-scale reorganization finally appears as the sole explanation, through the sintering of nano-metric aggregate present in the green pellet and related to the morphology of the starting microspheres employed as pelletization precursors. (authors)

Fabrication of Tungsten-Rhenium Cladding materials via Spark Plasma Sintering for Ultra High Temperature Reactor Applications

Energy Technology Data Exchange (ETDEWEB)

Charit, Indrajit; Butt, Darryl; Frary, Megan; Carroll, Mark

2012-11-05

This research will develop an optimized, cost-effective method for producing high-purity tungsten-rhenium alloyed fuel clad forms that are crucial for the development of a very high-temperature nuclear reactor. The study will provide critical insight into the fundamental behavior (processing-microstructure- property correlations) of W-Re alloys made using this new fabrication process comprising high-energy ball milling (HEBM) and spark plasma sintering (SPS). A broader goal is to re-establish the U.S. lead in the research field of refractory alloys, such as W-Re systems, with potential applications in very high-temperature nuclear reactors. An essential long-term goal for nuclear power is to develop the capability of operating nuclear reactors at temperatures in excess of 1,000K. This capability has applications in space exploration and some special terrestrial uses where high temperatures are needed in certain chemical or reforming processes. Refractory alloys have been identified as being capable of withstanding temperatures in excess of 1,000K and are considered critical for the development of ultra hightemperature reactors. Tungsten alloys are known to possess extraordinary properties, such as excellent high-temperature capability, including the ability to resist leakage of fissile materials when used as a fuel clad. However, there are difficulties with the development of refractory alloys: 1) lack of basic experimental data on thermodynamics and mechanical and physical properties, and 2) challenges associated with processing these alloys.

High-Strength Ultra-Fine-Grained Hypereutectic Al-Si-Fe-X (X = Cr,Mn) Alloys Prepared by Short-Term Mechanical Alloying and Spark Plasma Sintering

Czech Academy of Sciences Publication Activity Database

Průša, F.; Bláhová, M.; Vojtěch, D.; Kučera, V.; Bernatiková, A.; Kubatík, Tomáš František; Michalcová, A.

2016-01-01

Roč. 9, č. 12 (2016), č. článku 973. ISSN 1996-1944 Institutional support: RVO:61389021 Keywords : mechanical alloying * spark plasma sintering * microstructure * mechanical properties Subject RIV: JK - Corrosion ; Surface Treatment of Materials Impact factor: 2.654, year: 2016 http://www.mdpi.com/1996-1944/9/12/973

The Structure and Mechanical Properties of High-Strength Bulk Ultrafine-Grained Cobalt Prepared Using High-Energy Ball Milling in Combination with Spark Plasma Sintering

Czech Academy of Sciences Publication Activity Database

Marek, I.; Vojtěch, D.; Michalcová, A.; Kubatík, Tomáš František

2016-01-01

Roč. 9, č. 5 (2016), č. článku 391. ISSN 1996-1944 Institutional support: RVO:61389021 Keywords : ultrafine-grained material * cobalt * ball milling * spark plasma sintering * mechanical properties Subject RIV: JG - Metallurgy Impact factor: 2.654, year: 2016 www.mdpi.com/1996-1944/9/5/391/pdf

Plutonium Immobilization Project Binder Burnout and Sintering Studies (Milestone 6.6a)

International Nuclear Information System (INIS)

Chandler, G.

1999-01-01

The Plutonium Immobilization Team has developed an integrated test program to understand and optimize the controlling variables for the sintering step of the plutonium immobilization process. Sintering is the key process step that controls the product mineralogy. It is expected that the sintering will be the limiting process step that controls the throughput of the production line. The goal of the current sintering test program is to better understand factors that affect the sintering process

Plutonium Immobilization Project Binder Burnout and Sintering Studies (Milestone 6.6a)

Energy Technology Data Exchange (ETDEWEB)

Chandler, G.

1999-10-28

The Plutonium Immobilization Team has developed an integrated test program to understand and optimize the controlling variables for the sintering step of the plutonium immobilization process. Sintering is the key process step that controls the product minerology. It is expected that the sintering will be the limiting process step that controls the throughput of the production line. The goal of the current sintering test program is to better understand factors that affect the sintering process.

Influences of spark plasma sintering temperature on the microstructures and thermoelectric properties of (Sr0.95Gd0.05)TiO3 ceramics

Science.gov (United States)

Li, Liang-Liang; Qin, Xiao-Ying; Liu, Yong-Fei; Liu, Quan-Zhen

2015-06-01

(Sr0.95Gd0.05)TiO3 (SGTO) ceramics are successfully prepared via spark plasma sintering (SPS) respectively at 1548, 1648, and 1748 K by using submicron-sized SGTO powders synthesized from a sol-gel method. The densities, microstructures, and thermoelectric properties of the SGTO ceramics are studied. Though the Seebeck coefficient shows no obvious difference in the case that SPS temperatures range from 1548 K to 1648 K, the electrical conductivity and the thermal conductivity increase remarkably due to the increase in grain size and density. The sample has a density higher than 98% theoretical density as the sintering temperature increases up to 1648 K and shows average grain sizes increasing from ˜ 0.7 μm to 7 μm until 1748 K. As a result, the maximum of the dimensionless figure of merit of ˜ 0.24 is achieved at ˜ 1000 K for the samples sintered at 1648 K and 1748 K, which was ˜ 71% larger than that (0.14 at ˜ 1000 K) for the sample sintered at 1548 K due to the enhancement of the power factor. Project supported by the National Natural Science Foundation of China (Grant Nos. 11174292, 51101150, and 11374306).

On the sintering kinetics in UO2

International Nuclear Information System (INIS)

Marajofsky, A.

1998-01-01

The fabrication process of UO 2 pellets from powders involve pressing and a sintering anneal at high temperature (1650 deg. C to 1750 deg. C) during two or more hours in a hydrogen atmosphere. An alternative method is the oxidative sintering, made at lower temperature (1000 deg. C to 1300 deg. C) in a CO 2 or CO/CO 2 atmosphere. The sintering phenomena consist in the densification of the material by a thermal treatment below the fusion point. For a compact made by pressing a powder, sintering is the process of annulation of the porosity present in the compact or pellet. Several theories describe the sintering phenomena dividing it in three stages, initial, intermediate and final: in all of them the densification is a continuous growing function of time. Nevertheless it has been experimentally reported that a reduction of the density occurs in the third step of the sintering. The phenomena has been called solarization. Solarization has been attributed to the effect of the evolved gases from additives or to the CO 2 atmosphere in oxidative sintering. Thus, it is convenient to distinguish between solarization in oxidative or reducing conditions. Reducing solarization is a consequence of the tendency towards equilibrium of intergranular pores. In oxidative sintering it occurs in the reducing anneal after the sintering and is due to the change in the lattice parameter. This work shows examples of both types of solarization and qualitative interpretation of this phenomena. Both situations show the need of strict control of the sintering and powder production conditions. (author)

Effect of B2O3 and P2O5 on fluorosilicic mica glass-ceramic sintering process

Directory of Open Access Journals (Sweden)

Wu S.

2010-01-01

Full Text Available To study the effect of B2O3 and P2O5 on fluorosilicic mica glass-ceramic sintering process, six sets of K2O-MgO-SiO2-F glasses were prepared by using B2O3 and P2O5 as sintering aid, respectively. Green bodies of the glass powder were formed by gel casting and sintered at 800, 850, 900, 950, 1000oC for 6 hours, resectively. The sintering and crystallization behavior were studied by thermal shrinkage , X-ray diffraction and SEM. The results showed that the shrinkage rate of the glass with 2wt% B2O3 and P2O5 was highest, while the rate of the glass with 5wt% P2O5 was lowest. An additional crystal other than fluorosilicic mica was precipitated in the glass ceramics generated by sintering of glass powder. The present results confirmed that the glass powder of pure K2O-MgO-SiO2-Fsystem had poor sinterability, while glass powder with minor addition of P2O5 and/or B2O3 showed good sinterability. This result was also verified by SEM.

Sintered-to-size FBR fuel

International Nuclear Information System (INIS)

Rasmussen, D.E.; Schaus, P.S.

1984-04-01

Fabrication of sintered-to-size PuO 2 -UO 2 fuel pellets was completed for testing of proposed FBR product specifications. Approximately 6000 pellets were fabricated to two nominal diameters and two densities by cold pressing and sintering to size. Process control and correlation between test and production batches are discussed

Sintering of nano crystalline o silicon carbide doping with

Indian Academy of Sciences (India)

Sinterable silicon carbide powders were prepared by attrition milling and chemical processing of an acheson type -SiC. Pressureless sintering of these powders was achieved by addition of aluminium nitride together with carbon. Nearly 99% sintered density was obtained. The mechanism of sintering was studied by ...

Influence of Various Process Parameters on the Density of Sintered Aluminium Alloys

Directory of Open Access Journals (Sweden)

Mateusz Laska

2012-01-01

Full Text Available This paper presents the results of density measurements carried out on Alumix sintered parts. ECKA Alumix aluminium powders were used because of their wide application in the powder metallurgy industry. The compacts were produced using a wide range of compaction pressures for three different chemical compositions. The compacts were then sintered under a pure dry nitrogen atmosphere at three different temperatures. The heating and cooling rates were the same throughout the entire test. The results showed that the green density increases with compaction pressure, but that sintered density is independent of green density (compaction pressure for each sintering temperature.

Development of AUC-based process at BARC for production of free-flowing and sinterable UO2 powder

International Nuclear Information System (INIS)

Keni, V.S.; Ghosh, S.K.; Ganguly, C.; Majumdar, S.

1994-01-01

Ammonium uranium carbonate (AUC) process has been developed and industrially used in Germany for preparation of free-flowing and sinterable UO 2 powder for fabrication of UO 2 fuel pellets for light water reactors (LWR). Efforts are underway at Bhabha Atomic Research Centre (BARC) for developing AUC-based process which would yield free-flowing UO 2 powder suitable for direct pelletisation and sintering to very high density (> 96% T.D.) UO 2 fuel pellets for pressurised heavy water reactors (PHWRs) in India. The first phase of this work has been completed jointly by Chemical Engineering Division (ChED) and Radiometallurgy Division (RMD) in batches of 1.5 kg. It was possible to fabricate UO 2 pellets of density 93-95% T.D. on a reproducible basis. At ChED, process parameters have been optimised for fabrication of AUC with suitable physical properties in batches of 1.5 kg (U), starting with nuclear pure uranyl nitrate solution. At RMD calcination parameters of AUC was optimised in batches of 500 g for obtaining free-flowing UO 2 powder, suitable for direct pelletisation and sintering. The pelletisation and sintering have been carried out at Radiometallurgy Division in batches of 1-1.5 kg. The maximum achievable density of UO 2 pellets has been in the range of 95.5-96% T.D. (author). 11 refs

One step sintering of homogenized bauxite raw material and kinetic study

Science.gov (United States)

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.

Sintering equation: determination of its coefficients by experiments - using multiple regression

International Nuclear Information System (INIS)

Windelberg, D.

1999-01-01

Sintering is a method for volume-compression (or volume-contraction) of powdered or grained material applying high temperature (less than the melting point of the material). Maekipirtti tried to find an equation which describes the process of sintering by its main parameters sintering time, sintering temperature and volume contracting. Such equation is called a sintering equation. It also contains some coefficients which characterise the behaviour of the material during the process of sintering. These coefficients have to be determined by experiments. Here we show that some linear regressions will produce wrong coefficients, but multiple regression results in an useful sintering equation. (orig.)

Nanoporous gold synthesized by plasma-assisted inert gas condensation: room temperature sintering, nanoscale mechanical properties and stability against high energy electron irradiation

Science.gov (United States)

Weyrauch, S.; Wagner, C.; Suckfuell, C.; Lotnyk, A.; Knolle, W.; Gerlach, J. W.; Mayr, S. G.

2018-02-01

With a plasma assisted gas condensation system it is possible to achieve high-purity nanoporous Au (np-Au) structures with minimal contaminations and impurities. The structures consist of single Au-nanoparticles, which partially sintered together due to their high surface to volume ratio. Through electron microscopy investigations a porosity  >50% with ligament sizes between 20-30 nm was revealed. The elastic modulus of the np-Au was determined via peak force quantitative nanomechanical mapping and resulted in values of 7.5  ±  1.5 GPa. The presented structures partially sintered at room temperature, but proved to be stable to electron irradiation with energies of 7 MeV up to doses of 100 MGy. The electron irradiation stability opens the venue for electron assisted functionalization with biomolecules.

Current state of the Uranium dioxide sintering theory

International Nuclear Information System (INIS)

Baranov, V.; Devyatko, Y.; Tenishev, A.; Khlunov, A.; Khomyakov, O.

2011-01-01

The basic approaches to the description of the ceramics sintering phenomenon are considered. It is established that diffusive sintering models incorrectly describe an intermediate stage of this process. The physical model of sintering, considering the substance plastic flow of pressing under the influence of internal stress forces and capillary forces, as the basic mechanism defining the shrinkage of sintering oxide nuclear fuel, is offered. (authors)

Synthesis, Sintering, and Electrical Properties of BaCe0.9−xZrxY0.1O3−δ

DEFF Research Database (Denmark)

Ricote, S.; Caboche, G.; Estournes, C.

2008-01-01

BaCe0.9-xZrxY0.1O3-delta powders were synthesized by a solid-state reaction. Different contents of cerium and zirconium were studied. Pellets were sintered using either conventional sintering in air at 1700 degrees C or the Spark Plasma Sintering (SPS) technique. The density of the samples sintered...

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

Directory of Open Access Journals (Sweden)

Xiaoyong Ren

2014-01-01

Full Text Available 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.

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

Energy Technology Data Exchange (ETDEWEB)

Lester, Brian T. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

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 products like wash-basins. To understand the sintering process, a variety of modeling approaches have been pursued at different scales.

Thermal Mechanical Processing Effects on Microstructure Evolution and Mechanical Properties of the Sintered Ti-22Al-25Nb Alloy.

Science.gov (United States)

Wang, Yuanxin; Lu, Zhen; Zhang, Kaifeng; Zhang, Dalin

2016-03-11

This work illustrates the effect of thermal mechanical processing parameters on the microstructure and mechanical properties of the Ti-22Al-25Nb alloy prepared by reactive sintering with element powders, consisting of O, B2 and Ti₃Al phases. Tensile and plane strain fracture toughness tests were carried out at room temperature to understand the mechanical behavior of the alloys and its correlation with the microstructural features characterized by scanning and transmission electron microscopy. The results show that the increased tensile strength (from 340 to 500 MPa) and elongation (from 3.6% to 4.2%) is due to the presence of lamellar O/B2 colony and needle-like O phase in B2 matrix in the as-processed Ti-22Al-25Nb alloys, as compared to the coarse lath O adjacent to B2 in the sintered alloys. Changes in morphologies of O phase improve the fracture toughness ( K IC ) of the sintered alloys from 7 to 15 MPa·m -1/2 . Additionally, the fracture mechanism shifts from cleavage fracture in the as-sintered alloys to quasi-cleavage fracture in the as-processed alloys.

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

Science.gov (United States)

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.

Faceted shell structure in grain boundary diffusion-processed sintered Nd–Fe–B magnets

Energy Technology Data Exchange (ETDEWEB)

Seelam, U.M.R.; Ohkubo, T.; Abe, T.; Hirosawa, S.; Hono, K., E-mail: kazuhiro.hono@nims.go.jp

2014-12-25

Graphical abstract: The grain boundary diffusion process (GBDP) using a heavy rare earth elements (HRE) such as Dy and Tb is known as an effective method to enhance the coercivity of Nd–Fe–B sintered magnets without reducing remanence. This process has been industrially implemented to manufacture Nd–Fe–B based sintered magnets with high coercivity and high remanence. In this process, Dy is considered to diffuse through grain boundaries (GBs) to form (Nd{sub 1−x}Dy{sub x}){sub 2}Fe{sub 14}B shells surrounding the Nd{sub 2}Fe{sub 14}B grains and the higher anisotropy field of the Dy-rich shell is considered to suppress the nucleation of reverse domains at low magnetic field. Although there are several investigations on the microstructure of HRE GBDP Nd–Fe–B magnets, no paper addressed the origin of the asymmetric formation of HRE rich shells. Based on detailed analysis of facet planes of core/shell interfaces, we propose a mechanism of the faceted core/shell microstructure formation in the GBDP sintered magnets. We believe that this gives new insights on understanding the coercivity enhancement by the GBDP. - Highlights: • Faceting was observed at the interfaces of cores and shells. • The core/shell interfaces are sharp with an abrupt change in Dy concentration. • Meting occurs at the interfaces of metalic Nd-rich/Nd{sub 2}Fe{sub 14}B phases above 685 °C due to eutectic reaction. • Solidification of Dy-enriched liquid phase from 900 °C can result in the shell formation. - Abstract: Dysprosium enriched shell structure formed by the grain boundary diffusion process (GBDP) of a sintered Nd–Fe–B magnet was characterized by using scanning electron microscopy, electron back-scattered diffraction and transmission electron microscopy. Faceted core–shell interfaces with an abrupt change in Dy concentration suggest the Dy-rich shells are formed by the solidification of the liquid phase during cooling from the GBDP temperature. The Nd-rich phases

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

International Nuclear Information System (INIS)

Zhang, Zhikun; Zhang, Lei; Li, Aimin

2015-01-01

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. 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 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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-04-15

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. 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

Fast plasma sintering delivers functional graded materials components with macroporous structures and osseointegration properties.

Science.gov (United States)

Godoy, R F; Coathup, M J; Blunn, G W; Alves, A L; Robotti, P; Goodship, A E

2016-04-13

We explored the osseointegration potential of two macroporous titanium surfaces obtained using fast plasma sintering (FPS): Ti macroporous structures with 400-600 µmØ pores (TiMac400) and 850-1000 µmØ pores (TiMac850). They were compared against two surfaces currently in clinical use: Ti-Growth® and air plasma spray (Ti-Y367). Each surface was tested, once placed over a Ti-alloy and once onto a CoCr bulk substrate. Implants were placed in medial femoral condyles in 24 sheep. Samples were explanted at four and eight weeks after surgery. Push-out loads were measured using a material-testing system. Bone contact and ingrowth were assessed by histomorphometry and SEM and EDX analyses. Histology showed early osseointegration for all the surfaces tested. At 8 weeks, TiMac400, TiMac850 and Ti-Growth® showed deep bone ingrowth and extended colonisation with newly formed bone. The mechanical push-out force was equal in all tested surfaces. Plasma spray surfaces showed greater bone-implant contact and higher level of pores colonisation with new bone than FPS produced surfaces. However, the void pore area in FPS specimens was significantly higher, yet the FPS porous surfaces allowed a deeper osseointegration of bone to implant. FPS manufactured specimens showed similar osseointegration potential to the plasma spray surfaces for orthopaedic implants. FPS is a useful technology for manufacturing macroporous titanium surfaces. Furthermore, its capability to combine two implantable materials, using bulk CoCr with macroporous titanium surfaces, could be of interest as it enables designers to conceive and manufacture innovative components. FPS delivers functional graded materials components with macroporous structures optimised for osseointegration.

Laser sintering of metal powders on top of sintered layers under multiple-line laser scanning

International Nuclear Information System (INIS)

Xiao Bin; Zhang Yuwen

2007-01-01

A three-dimensional numerical model for multiple-line sintering of loose powders on top of multiple sintered layers under the irradiation of a moving Gaussian laser beam is carried out. The overlaps between vertically deposited layers and adjacent lines which strengthen bonding are taken into account. The energy equation is formulated using the temperature transforming model and solved by the finite volume method. The effects of the number of the existing sintered layers, porosity and initial temperature coupled with the optimal combination laser intensity and scanning velocity are presented. The results show that the liquid pool moves slightly towards the negative scanning direction and the shape of the liquid pool becomes shallower with higher scanning velocity. A higher laser intensity is needed to achieve the required overlaps when the number of the existing sintered layers increases. Increasing porosity or initial temperature enhances the sintering process and thus less intensity is needed for the overlap requirement

Porous Nb-Ti based alloy produced from plasma spheroidized powder

Directory of Open Access Journals (Sweden)

Qijun Li

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

Morphological analysis and modelling of sintering and of sintered materials

International Nuclear Information System (INIS)

Jernot, Jean-Paul

1982-01-01

This research thesis addresses the study of solid phase sintering of metallic powders, and aims at describing as precisely as possible the different involved matter transport mechanisms, first by using a thermodynamic approach to sintering. Sintering diagrams are also used to determine prevailing mechanisms. The microstructure of sintered materials has been studied by using image quantitative analysis, thus by using a morphological approach to sintering. Morphological parameters allow, on the one hand, the evolution of powders during sintering to be followed, and, on the other hand, sintered products to be correctly characterised. Moreover, the author reports the study of the evolution of some physical properties of sintered materials with respect to their microstructure parameters. This leads to the development of a modelling of the behaviour of these materials [fr

A study of pressureless microwave sintering, microwave-assisted hot press sintering and conventional hot pressing on properties of aluminium/alumina nanocomposite

Energy Technology Data Exchange (ETDEWEB)

Abedinzadeh, Reza; Safavi, Seyed Mohsen; Karimzadeh, Fathallah [Isfahan University, Isfahan (Iran, Islamic Republic of)

2016-05-15

Bulk Al/4wt-%Al{sub 2}O{sub 3} nanocomposites were prepared by consolidating nanocomposite powders using pressureless microwave sintering, microwave-assisted hot press sintering and conventional hot pressing techniques. Microstructural observations revealed that the microwave-assisted hot press sintering at different sintering temperatures of 400.deg.C and 500.deg.C resulted in more densification and smaller grain size for Al/Al{sub 2}O{sub 3} nanocomposite as compared with the conventional hot pressing. Moreover, the application of pressure in microwave sintering process led to more densification and grain growth. Mechanical properties resulting from microhardness and nanoindentation tests were also compared between three-method processed samples. It was found that the microwave-assisted hot-pressed sample exhibited higher hardness and elastic modulus in comparison with microwave-sintered and conventional hot-pressed samples. The improvement in the mechanical properties can be ascribed to lower porosity of microwave-assisted hot-pressed sample.

Processing of W-Cu functionally graded materials (FGM) through the powder metallurgy route: application as plasma facing components for ITER-like thermonuclear fusion reactor

International Nuclear Information System (INIS)

Raharijaona, J.J.

2009-11-01

The aim of this study was to study and optimize the sintering of W-Cu graded composition materials, for first wall of ITER-like thermonuclear reactor application. The graded composition in the material generates graded functional properties (Functionally Graded Materials - FGM). Rough thermomechanical calculations have shown the interest of W-Cu FGM to improve the lifetime of Plasma Facing Components (PFC). To process W-Cu FGM, powder metallurgy route was analyzed and optimized from W-CuO powder mixtures. The influence of oxide reduction on the sintering of powder mixtures was highlighted. An optimal heating treatment under He/H 2 atmosphere was determined. The sintering mechanisms were deduced from the analysis of the effect of the Cu-content. Sintering of W-Cu materials with a graded composition and grain size has revealed two liquid migration steps: i) capillary migration, after the Cu-melting and, ii) expulsion of liquid, at the end of sintering, from the dense part to the porous part, due to the continuation of W-skeleton sintering. These two steps were confirmed by a model based on capillary pressure calculation. In addition, thermal conductivity measurements were conducted on sintered parts and showed values which gradually increase with the Cu-content. Hardness tests on a polished cross-section in the bulk are consistent with the composition profiles obtained and the differential grain size. (author)

Development of a manufacturing process of (Th,U)O2 sintered pellets to be used as nuclear fuel

International Nuclear Information System (INIS)

Neto Ferreira, R.A.; Santos, A.M. dos; Lameiras, F.S.; Cardoso, P.E.

1989-01-01

The R and D result of a reliable manufacturing process of sintered (Th,U)O 2 pellets meeting the operational requirements of pressurized light water nuclear reactors is presented. Available technologies were used as much as possible. The R and D effort was directed to perform the required adaptations. The gel precipitation process was adapted successfully to the specific requirements of direct pressing and sintering. This was done mainly by adjusting the composition of the feed solution. The direct pressing and sintering parameters could be kept almost unchanged in relation to the manufacturing of UO 2 pellets. The design criteria of the (Th,U)O 2 nuclear fuel for pressurized light water reactors were identified and settled in the specification for this fuel. This R and D work was made jointly with the Kernforschungsanlage - Juelich, NUKEM and SIEMENS, Group KWU [pt

Effects of sintering temperature on the density and porosity

African Journals Online (AJOL)

2013-03-01

bonding) between the salt beads at all the temperatures in which sintering was performed. .... and the sintering of some covalent solids and low- stability ceramics. The entire sintering process is gen- erally considered to occur in ...

Master sintering curve: A practical approach to its construction

Directory of Open Access Journals (Sweden)

Pouchly V.

2010-01-01

Full Text Available The concept of a Master Sintering Curve (MSC is a strong tool for optimizing the sintering process. However, constructing the MSC from sintering data involves complicated and time-consuming calculations. A practical method for the construction of a MSC is presented in the paper. With the help of a few dilatometric sintering experiments the newly developed software calculates the MSC and finds the optimal activation energy of a given material. The software, which also enables sintering prediction, was verified by sintering tetragonal and cubic zirconia, and alumina of two different particle sizes.

Titanium and zirconium metal powder spheroidization by thermal plasma processes

OpenAIRE

Bissett, H.; van der Walt, I.J.; Havenga, J.L.; Nel, J.T.

2015-01-01

New technologies used to manufacture high-quality components, such as direct laser sintering, require spherical powders of a narrow particle size distribution as this affects the packing density and sintering mechanism. The powder also has to be chemically pure as impurities such as H, O, C, N, and S causes brittleness, influence metal properties such as tensile strength, hardness, and ductility, and also increase surface tension during processing. Two new metal powder processes have been dev...

Kinetics of UO{sub 2} sintering; Kinetika sinterovanja UO{sub 2}

Energy Technology Data Exchange (ETDEWEB)

Ristic, M M [Institute of Nuclear Sciences Vinca, Laboratorija za reaktorske materijale, Beograd (Serbia and Montenegro)

1962-10-15

Detailed conclusions related to the UO{sub 2} sintering can be drawn from investigating the kinetics of the sintering process. This report gives an thorough analysis of the the data concerned with sintering available in the literature taking into account the Jander and Arrhenius laws. This analysis completes the study of influence of the O/U ratio and the atmosphere on the sintering. Results presented are fundamentals of future theoretical and experimental work related to characterisation of the UO{sub 2} sintering process.

Effect of the sintering method on microstructure and thermal and mechanical properties of zirconium oxophosphate ceramics Zr2O(PO4)2

Science.gov (United States)

Bregiroux, Damien; Cedelle, Julie; Ranc, Isabelle; Barreteau, Céline; Mata Osoro, Gustavo; Wallez, Gilles

2017-12-01

Due to an ultra-low thermal expansion, Zr2O(PO4)2 could find many applications as a thermal shock resistant material. To this end, ceramic processing is a key step in order to reach best properties. In this work, Zr2O(PO4)2 was sintered by conventional sintering and by the spark plasma sintering technique (SPS) with and without additive. Samples made by conventional sintering with ZnO as sintering aid have a maximum relative density of around 92%. Microstructure is composed of large grains and microcracks can be observed. When doped with 5 wt. % of MgO, samples can be densified by SPS up to 99.6% of the relative density and the grain size maintained between 0.5 and 1.5 μm. Thermal conductivity and Vickers microhardness were investigated as a function of the microstructure. Best values were obtained for the ceramic doped with 5 wt.% MgO and sintered by SPS, thanks to a fine microstructure and a small amount of residual microcracks.

Si-substituted hydroxyapatite nanopowders: Synthesis, thermal stability and sinterability

International Nuclear Information System (INIS)

Bianco, Alessandra; Cacciotti, Ilaria; Lombardi, Mariangela; Montanaro, Laura

2009-01-01

Synthetic hydroxyapatites incorporating small amounts of Si have shown improved biological performances in terms of enhanced bone apposition, bone in-growth and cell-mediated degradation. This paper reports a systematic investigation on Si-substituted hydroxyapatite (Si 1.40 wt%) nanopowders produced following two different conventional wet methodologies: (a) precipitation of Ca(NO 3 ) 2 .4H 2 O and (b) titration of Ca(OH) 2 . The influence of the synthesis process on composition, thermal behaviour and sinterability of the resulting nanopowders is studied. Samples were characterised by electron microscopy, induced coupled plasma atomic emission spectroscopy, thermal analysis, infrared spectroscopy, N 2 adsorption measurements, X-ray diffraction and dilatometry. Semicrystalline Si-substituted hydroxyapatite powders made up of needle-like nanoparticles were obtained, the specific surface area ranged between 84 and 110 m 2 /g. Pure and Si-substituted hydroxyapatite nanopowders derived from Ca(NO 3 ) 2 .4H 2 O decomposed around 1000 deg. C. Si-substituted hydroxyapatite nanopowders obtained from Ca(OH) 2 were thermally stable up to 1200 deg. C and showed a distinct decreased thermal stability with respect to the homologous pure sample. Si-substituted hydroxyapatites exhibited higher sintering temperature and increased total shrinkage with respect to pure powders. Nanostructured dense ceramics were obtained by sintering at 1100 deg. C Si-substituted hydroxyapatites derived from Ca(OH) 2

Coercivity of Nd-Fe-B hot-deformed magnets produced by the spark plasma sintering method

Directory of Open Access Journals (Sweden)

Tetsuji Saito

2017-05-01

Full Text Available The effects of Nd-Cu alloy powder addition on the microstructures and magnetic properties of Nd-Fe-B hot-deformed magnets produced by the spark plasma sintering (SPS method were investigated. The addition of a small amount of Nd-Cu alloy powder, up to 2%, significantly increased the coercivity of the Nd-Fe-B hot-deformed magnets without deteriorating the crystallographic alignment of the Nd2Fe14B phase. The Nd-Fe-B hot-deformed magnet with 2% Nd-Cu alloy powder had the same remanence value as the Nd-Fe-B hot-deformed magnet without Nd-Cu alloy powder addition, but the magnet with 2% Nd-Cu alloy powder exhibited higher coercivity and a higher maximum energy product than the magnet without Nd-Cu alloy powder addition.

Process-generated nanoparticles from ceramic tile sintering: Emissions, exposure and environmental release.

Science.gov (United States)

Fonseca, A S; Maragkidou, A; Viana, M; Querol, X; Hämeri, K; de Francisco, I; Estepa, C; Borrell, C; Lennikov, V; de la Fuente, G F

2016-09-15

The ceramic industry is an industrial sector in need of significant process changes, which may benefit from innovative technologies such as laser sintering of ceramic tiles. Such innovations result in a considerable research gap within exposure assessment studies for process-generated ultrafine and nanoparticles. This study addresses this issue aiming to characterise particle formation, release mechanisms and their impact on personal exposure during a tile sintering activity in an industrial-scale pilot plant, as a follow-up of a previous study in a laboratory-scale plant. In addition, possible particle transformations in the exhaust system, the potential for particle release to the outdoor environment, and the effectiveness of the filtration system were also assessed. For this purpose, a tiered measurement strategy was conducted. The main findings evidence that nanoparticle emission patterns were strongly linked to temperature and tile chemical composition, and mainly independent of the laser treatment. Also, new particle formation (from gaseous precursors) events were detected, with nanoparticles efficiency of the filtration system was successfully tested and evidenced a >87% efficiency in particle number concentrations removal. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Sintering characteristics of nano-ceramic coatings

NARCIS (Netherlands)

de Hosson, J.T.M.; Popma, R.

2003-01-01

This paper concentrates on sintering characteristics of nano-sized ceramic SiO2 particles. The sintering process is studied as a function of temperature using a conventional furnace and using a laser beam. The underlying idea is to combine the nanoceramic sol-gel concept with inkjet technology and

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

Science.gov (United States)

Cariapa, Vikram

1993-01-01

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

Effect of sintering time at low temperature on the properties of IGZO TFTs fabricated by using the sol-gel process

International Nuclear Information System (INIS)

Choi, Jun Hyuk; Shim, Jong Hyun; Hwang, Soo Min

2010-01-01

We explored the application of the sol-gel process technique to the fabrication of InGaZnO (IGZO) thin film transistors (TFTs). We fabricated IGZO TFTs by using the sol-gel method and evaluated the effect of the sintering time on the electrical properties of the IGZO system with an atomic ratio of In:Ga:Zn = 2:1:1. In the process, IGZO precursor solutions were prepared by mixing In nitrate, Ga nitrate, and Zn acetate and were then deposited on a p-type Si-wafer covered with a thermally grown SiO 2 layer by spin-coating. The sintering process was performed for 3 h, 6 h or 12 h at 300 .deg. C in the ambient atmosphere. The source/drain electrodes of the TFT devices were fabricated using Al thermal evaporation. For all of the samples, a low off current (∼10 -1 1 A) and on-to-off current ratio (∼ 5 x 10 4 ) were obtained in their transfer curves. The saturation mobility increased with increasing sintering time: for the samples sintered for 3 h, 6 h and 12 h, the saturation mobilities were calculated to be 0.825 cm 2 /Vs, 1.65 cm 2 /Vs, and 2.06 cm 2 /Vs, respectively. Based on the XPS and TEM analyses, the enhancement of the mobility was attributed to the increase in the number of oxygen vacancies and the nanocrystalline structure in the amorphous matrix with increasing sintering time. These results demonstrate for the potential application of sol-gel processed IGZO devices on flexible polymer substrates.

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

Science.gov (United States)

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.

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

Science.gov (United States)

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.

Effects of sintering processes on mechanical properties and microstructure of TiB2–TiC + 8 wt% nano-Ni composite ceramic cutting tool material

International Nuclear Information System (INIS)

Zou Bin; Huang Chuanzhen; Song Jinpeng; Liu Ziye; Liu Lin; Zhao Yan

2012-01-01

Highlights: ► TiB 2 –TiC + 8 wt% nano-Ni ceramic tool material was sintered by six processes. ► The properties of material depended mainly on the holding stages and duration. ► SP1 process was involved with the multiple holding stages and longer duration. ► SP1 process led to many pores, and coarsening and brittle rupture of grains. ► Tool material sintered by SP6 process exhibited the optimum mechanical properties. - Abstract: TiB 2 –TiC composite powder was prepared by ball-milled with ethanol and vacuum dry, and TiB 2 –TiC + 8 wt% nano-Ni composite ceramic cutting tool material was sintered using vacuum hot-pressed sintering technique by six processes which included the different holding stages and times. The effects of sintering processes on the mechanical properties and microstructure were investigated. The polished surface and fracture surface of TiB 2 –TiC + 8 wt% nano-Ni ceramics sintered by the different sintering processes were observed by scanning electron microscope (SEM), X-ray diffraction (XRD) and energy-dispersive spectrometry (EDS), and the relationships between mechanical properties and microstructure were discussed. The mechanical properties and microstructure depended mainly on the total holding time and the different holding stages. The longer holding time and multiple holding stages led to coarsening of TiB 2 and TiC grains, formation of pores and the brittle rupture of grains, which deteriorated the mechanical properties of TiB 2 –TiC + 8 wt% nano-Ni ceramic. TiB 2 –TiC + 8 wt% nano-Ni composite ceramic cutting tool material sintered by SP6 process exhibited the optimum resultant mechanical properties because of its finer microstructure and higher relative density, and its flexural strength, fracture toughness and hardness were 916.8 MPa, 7.80 MPa m 1/2 and 22.54 GPa, respectively.

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

Science.gov (United States)

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.

Influence of sintering atmospheres on the aluminium sintering characteristics

International Nuclear Information System (INIS)

Mintzer, S.; Bermudez Belkys, S.

1993-01-01

This paper describes the aluminium powder (Al) cool compacted (at 95% from theoretical density) which was sintered at 903 K during 4 hours at different atmospheres; oxidizing (air), inert Argon (Ar), Nitrogen (N) and high vacuum. The results obtained show: a) porosity measurements; greater porosity when sintering in Ar and air. b) Metallographic and Scanning observations: many fine pores (< 1 μm) and pore lines distributed at random, at air sintering and greater pores distributed preferentially near the surface, in Ar and N atmospheres. c) Dimensional changes: tendency to contraction of the samples at N and vacuum sintering and expansion in Ar or air. d) Mechanical properties: greater strength and fluence stresses at air and N sintering. The analysis of the results is performed considering sintering modes in presence of an oxide layer and dropped inert gases. (Author)

HAp physical investigation - the effect of sintering temperature

International Nuclear Information System (INIS)

Mohd Reusmaazran Yusof; Idris Besar; Rusnah Mustaffa; Cik Rohaida Che Hak

2004-01-01

The paper presents the effect of sintering temperature on the physical properties of porous hydroxyapatite (HAp). In this study, the HAp was prepared using polymeric sponge techniques with different binder concentration. The sintering process was carried out in air for temperature ranging from 1200 degree C to 1600 degree C. Different physical properties namely density and porosity were observed at different sintering temperatures. The HAp prepared with higher PVP binder showed a slightly decreased in apparent density with increasing sintering temperature, while those HAp prepared with lower PVP showed a slightly increase in apparent density with increasing sintering temperature. The total porosity was found to be approximately constant in the whole sintering temperature range. However, closed porosity decreases with increasing sintering temperature for HAp prepared by lower binder concentration. On the other hand, the HAp prepared by higher binder concentration HAp showed increasing closed porosity with increasing sintering temperature. Other features such as the influence of sintering temperatures on grain and strut also be presented in this paper. (Author)

Microwave sintering of Ag-nanoparticle thin films on a polyimide substrate

Energy Technology Data Exchange (ETDEWEB)

Fujii, S., E-mail: fujii.s.ap@m.titech.ac.jp [Department of Applied Chemistry, Tokyo Institute of Technology, Tokyo 152-8522 (Japan); Department of Information and Communication System Engineering, National Institute of Technology, Okinawa College, Nago, Okinawa 905-2192 (Japan); Kawamura, S.; Maitani, M. M.; Suzuki, E.; Wada, Y. [Department of Applied Chemistry, Tokyo Institute of Technology, Tokyo 152-8522 (Japan); Mochizuki, D. [Interdisciplinary Cluster for Cutting Edge Research, Center for Energy and Environmental Science, Shinshu University, Ueda, Nagano 386-8567 (Japan)

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. The 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.

Microwave sintering of Ag-nanoparticle thin films on a polyimide substrate

Directory of Open Access Journals (Sweden)

S. Fujii

2015-12-01

Full Text Available 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. The 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.

Multiple recycling of NdFeB-type sintered magnets

Energy Technology Data Exchange (ETDEWEB)

Zakotnik, M. [Department of Metallurgy and Materials, University of Birmingham, Edgbaston, Birmingham B15 2TT (United Kingdom)], E-mail: miha.zakotnik@gmail.com; Harris, I.R.; Williams, A.J. [Department of Metallurgy and Materials, University of Birmingham, Edgbaston, Birmingham B15 2TT (United Kingdom)

2009-02-05

Some fully dense, sintered NdFeB-type magnets (employed in VCM disc drives) have been subjected to a recycling process using the hydrogen decrepitation (HD) process. After a brief milling treatment, the powder was aligned, pressed and re-sintered and this procedure was repeated four times with a progressive fall in the density and in the magnetic properties. The chemical analysis indicated that this was due to the progressive oxidation of the Nd-rich material and to some Nd loss by evaporation. The procedure was then repeated but with the addition (blending) of a fine powder of neodymium hydride after the first cycle. It was found that the addition of 1 at.% of neodymium at each stage was sufficient to maintain the density and the magnetic properties of the recycled magnets up to and including the 4th cycle. Inductively coupled plasma (ICP) and metallographic analysis indicated that the neodymium hydride additions compensated for the neodymium loss due to evaporation and to oxidation so that the proportion of Nd-rich material remained approximately constant. The additional amount of Nd{sub 2}O{sub 3} in the blended recycled magnets appeared to inhibit grain growth on the 3rd and 4th cycles when compared to that of the unblended magnets. The next challenge is to see if the process can be scaled-up to an industrial scale.

Sintering and Microstructures of SUS 316L Powder Produced by 3D Printing Process

Directory of Open Access Journals (Sweden)

Kim W.J.

2017-06-01

Full Text Available Selective laser sintering (SLS is a type of laminating sintering technique, using CO2 laser with (metal, polymer, and ceramic powders. In this result, the flake SUS 316L was used to achieve a high porous product, and compare to spherical type. After SLS, the porosity of flake-type sample with 34% was quite higher than that of the spherical-type one that had only 11%. The surface roughness of the flake SLS sample were also investigated in both inner and surface parts. The results show that the deviation of the roughness of the surface part is about 64.40μm, while that of the internal one was about 117.65μm, which presents the containing of high porosity in the uneven surfaces. With the process using spherical powder, the sample was quite dense, however, some initial particles still remained as a result of less energy received at the beneath of the processing layer.

In vitro degradation and biocompatibility of Fe–Pd and Fe–Pt composites fabricated by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Huang, T. [State Key Laboratory for Turbulence and Complex System, College of Engineering, Peking University, Beijing 100871 (China); Department of Materials Science and Engineering, College of Engineering, Peking University, Beijing 100871 (China); Cheng, J. [Center for Biomedical Materials and Tissue Engineering, Academy for Advanced Interdisciplinary Studies, Peking University, Beijing 100871 (China); Zheng, Y.F., E-mail: yfzheng@pku.edu.cn [State Key Laboratory for Turbulence and Complex System, College of Engineering, Peking University, Beijing 100871 (China); Department of Materials Science and Engineering, College of Engineering, Peking University, Beijing 100871 (China); Center for Biomedical Materials and Tissue Engineering, Academy for Advanced Interdisciplinary Studies, Peking University, Beijing 100871 (China)

2014-02-01

In order to obtain biodegradable Fe-based materials with similar mechanical properties as 316L stainless steel and faster degradation rate than pure iron, Fe-5 wt.%Pd and Fe-5 wt.%Pt composites were prepared by spark plasma sintering with powders of pure Fe and Pd/Pt, respectively. The grain size of Fe-5 wt.%Pd and Fe-5 wt.%Pt composites was much smaller than that of as-cast pure iron. The metallic elements Pd and Pt were uniformly distributed in the matrix and the mechanical properties of these materials were improved. Uniform corrosion of Fe–Pd and Fe–Pt composites was observed in both electrochemical tests and immersion tests, and the degradation rates of Fe–Pd and Fe–Pt composites were much faster than that of pure iron. It was found that viabilities of mouse fibroblast L-929 cells and human umbilical vein endothelial cells (ECV304) cultured in extraction mediums of Fe–Pd and Fe–Pt composites were close to that of pure iron. After 4 days' culture, the viabilities of L-929 and ECV304 cells in extraction medium of experimental materials were about 80%. The result of direct contact cytotoxicity also indicated that experimental materials exhibited no inhibition on vascular endothelial process. Meanwhile, iron ions released from experimental materials could inhibit proliferation of vascular smooth muscle cells (VSMC), which may be beneficial for hindering vascular restenosis. Furthermore, compared with that of as-cast pure iron, the hemolysis rates of Fe–Pd and Fe–Pt composites were slightly higher, but still within the range of 5%, which is the criteria for good blood compatibility. The numbers of platelet adhered on the surface of Fe–Pd and Fe–Pt composites were lower than that of pure iron, and the morphology of platelets kept spherical. To sum up, the Fe-5wt.%Pd and Fe-5wt.%Pt composites exhibited good mechanical properties and degradation behavior, closely approaching the requirements for biodegradable metallic stents. - Highlights: �

Hydrogen Decrepitation Press-Less Process recycling of NdFeB sintered magnets

Science.gov (United States)

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. The coercivity reached Hci = 957 kA/m being 86% of the original N48M material without addition of rare earth elements.

Microstructure and mechanical properties of thermoelectric nanostructured n-type silicon-germanium alloys synthesized employing spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Bathula, Sivaiah [CSIR-Network of Institutes for Solar Energy, CSIR-National Physical Laboratory, Dr. K. S. Krishnan Marg, New Delhi 110012 (India); Department of Applied Physics, Delhi Technological University, Delhi (India); Gahtori, Bhasker; Tripathy, S. K.; Tyagi, Kriti; Srivastava, A. K.; Dhar, Ajay, E-mail: adhar@nplindia.org [CSIR-Network of Institutes for Solar Energy, CSIR-National Physical Laboratory, Dr. K. S. Krishnan Marg, New Delhi 110012 (India); Jayasimhadri, M. [Department of Applied Physics, Delhi Technological University, Delhi (India)

2014-08-11

Owing to their high thermoelectric (TE) figure-of-merit, nanostructured Si{sub 80}Ge{sub 20} alloys are evolving as a potential replacement for their bulk counterparts in designing efficient radio-isotope TE generators. However, as the mechanical properties of these alloys are equally important in order to avoid in-service catastrophic failure of their TE modules, we report the strength, hardness, fracture toughness, and thermal shock resistance of nanostructured n-type Si{sub 80}Ge{sub 20} alloys synthesized employing spark plasma sintering of mechanically alloyed nanopowders of its constituent elements. These mechanical properties show a significant enhancement, which has been correlated with the microstructural features at nano-scale, delineated by transmission electron microscopy.

Sintering of dioxide pellets in an oxidizing atmosphere (CO2)

International Nuclear Information System (INIS)

Santos, G.R.T.

1992-01-01

This work consists in the study of the sintering process of U O 2 pellets in an oxidizing atmosphere. Sintering tests were performed in an CO 2 atmosphere and the influence of temperature and time on the pellets density and microstructure were verified. The results obtained were compared to those from the conventional sintering process and its efficiency was confirmed. (author)

Electro sinter forging of titanium disks

DEFF Research Database (Denmark)

Cannella, Emanuele; Nielsen, Chris Valentin; Bay, Niels Oluf

by measuring the electrical resistance during the sintering process [5], since low electrical resistance corresponds to high density. It is, however, necessary to be aware that increased temperature, on the other hand, increases the resistance. SEM micrographs and Computed Tomography (CT) are carried out......Electro sinter forging (ESF) is a new sintering process based on the principle of electrical Joule heating. In the present work, middle frequency direct current (MFDC) was flowing through the powder compact, which was under mechanical pressure. The main parameters are the high electrical current......, up to 10 kA, and the low voltage, 1-2 V, resulting in heat generation in the powder. Figure 1 shows the experimental setup. The punches were made of a conductive material; namely a copper alloy. The die, which has to be electrically insulating, was made of alumina. The ESF process takes 3-4s...

Sintered ceramics having controlled density and porosity

International Nuclear Information System (INIS)

Brassfield, H.C.; DeHollander, W.R.; Nivas, Y.

1980-01-01

A new method was developed for sintering ceramic uranium dioxide powders, in which ammonium oxalate is admixed with the powder prior to being pressed into a cylindrical green body, so that the end-point density of the final nuclear-reactor fuel product can be controlled. When the green body is heated, the ammonium oxalate decomposes and leaves discrete porosity in the sintered body, which corresponds to the ammonium oxalate regions in the green body. Thus the end-point density of the sintered body is a function of the amount of ammonium oxalate added. The final density of the sintered product is about 90-97% of the theoretical. The addition of ammonium oxalate also allows control of the pore size and distribution throughout the fuel. The process leaves substantially no impurities in the sintered strucuture. (DN)

Two steps sintering alumina doped with niobia

International Nuclear Information System (INIS)

Gomes, L.B.; Hatzfeld, J.; Heck, M.; Pokorny, A.; Bergmann, C.P.

2014-01-01

In this work, high surface area commercial alumina was doped with niobia and sintered in two steps in order to obtain dense materials with lower processing temperatures. The powders were milled and uniaxially pressed (200 MPa). The first step of sintering took place at 1100°C for 3, 6, 9 and 12 hours, followed by the second step at 1350°C for 3 hours. The relative density, porosity and water absorption of the samples were determined by the Archimedes method. The crystalline phases were analyzed by X-ray Diffraction (XRD) and the morphology of the samples after sintering, evaluated by Scanning Electron Microscopy (SEM). The results indicate that the use of niobia combined with the two steps sintering promotes an increase in the density of the material, even at lower sintering temperatures. (author)

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

Energy Technology Data Exchange (ETDEWEB)

Antonov, E N; Krotova, L I; Minaev, N V; Minaeva, S A; Mironov, A V; Popov, V K [Institute on Laser and Information Technologies of the Russian Academy of Sciencies, Troitsk, Moscow (Russian Federation); Bagratashvili, V N [Department of Chemistry, M.V. Lomonosov Moscow State University, Moscow (Russian Federation)

2015-11-30

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

Influence of the starch content and sintering temperature on the processing of porous zirconia substrates

International Nuclear Information System (INIS)

Albano, Maria P; Garrido, Liliana B

2008-01-01

Porous ceramics are used as electrodes in fuel cells, separators in batteries, filters, etc. Thin porous substrates of zirconium stabilized with yttrium oxide (ZSY) are used as anodes in solid oxide fuel cells. One way to obtain a porous band is to mix starch particles during the preparation stage of the ZSY suspension. The starch burns during the removal of the binder and leaves stable pores that are not eliminated in the subsequent sintering stage. This work used the band pouring process to produce porous bands of ZSY with porosities of 29% to 53% using starch as a transitory additive. Concentrated aqueous suspensions of ZSY were prepared with different contents of starch and of an acrylic latex binder. The influence of the fraction of starch volume and of the temperature on the sintering behavior and on the final micro structure of the bands was studied. The total porosity of the bands was higher than the fractions in volume of added starch, due to the presence of closed porosity in the matrix. The deviations compared to the porosity predicted based on the fractions in the volume of starch, were greater as the starch content increased. The percentage of open porosity in the sintered bands depended on the fraction in the volume of added starch and on the sintering temperature. When the fraction in volume of starch increased from 17.6% to 37.8% a gradual increase occurred in the opening of the porous structure. The contraction of the bands during sintering at a given temperature correlated with the density of the packing of ZSY (au)

Spark plasma sintering of α-Si3N4 ceramics with Al2O3 and Y2O3 as additives and its morphology transformation

International Nuclear Information System (INIS)

Ceja-Cardenas, L.; Lemus-Ruiz, J.; Jaramillo-Vigueras, D.; Torre, S.D. de la

2010-01-01

The spark plasma sintering SPS technique has been used to densify pure α-Si 3 N 4 commercial powder, having Y 2 O 3 and Al 2 O 3 additions; from 0, 2.5 and 5.0 wt% to 0, 1.5 and 3 wt%, respectively. Such powder admixtures were previously spray-dried at 160 o C in such a way that powder was thoroughly homogenized. Set sintering treatment included: 0-20 min holding time and 38 MPa axial load, sintering temperature of 1500 o C and heating rate of 300 o C/min. The maximum relative density developed on studied specimens ranged from 99.4 to 99.8% and could only be attained once the β-phase nucleated from the α-silicon nitride matrix. Obtained Si 3 N 4 composites combine both α- and β-phases. The later phase becomes evident trough the rod-like geometry, which forms throughout the presence of a liquid face. The largest hardness value developed (1588 Hv (20kgf) ) on studied ceramics (3M-series - 3 min) matched close to the corresponding counterpart found in literature (1600 Hv), the former developed in much shorter sintering times. Using X-ray diffraction XRD and scanning electron microscope SEM analyses, the two major phases of Si 3 N 4 were identified in the resultant microstructures. The morphology evolution of Si 3 N 4 particles as occurred upon SPS-sintering is analyzed.

Processing of Syndiotactic Polystyrene to Microspheres for Part Manufacturing through Selective Laser Sintering

Directory of Open Access Journals (Sweden)

Nicolas Mys

2016-10-01

Full Text Available Syndiotactic polystyrene pellets were processed into powder form using mechanical (ball milling, rotor milling and physicochemical (spray drying techniques with the intention of using it as feed material for selective laser sintering. New materials are an important component in broadening the application window for selective laser sintering but must meet strict requirements to be used. Particles obtained were characterized in size and shape using SEM imaging, analyzed by software, and compared to the product obtained by conventional ball milling. Rotor milling and spray drying proved capable of making spherical powders, yet only rotor milling achieved particles with a mean diameter within the desired range of 45–97 µm. Subsequently, the obtained powders were examined for the effect each processing technique imparts on the intrinsic properties of the material. Differential scanning calorimetry analysis revealed amorphization for all methods and a reduction in crystallinity after processing, however, the reduction in crystallinity was acceptably low for the spray-dried and rotor-milled powders. Ball milling displayed an exceptional reduction in crystallinity, suggesting severe degradation. As a final test, the rotor-milled powder was subjected to single-layer test and displayed good coalescence and smooth morphology, albeit with a large amount of warpage.

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

Directory of Open Access Journals (Sweden)

Jiaqi Ni

2018-05-01

Full Text Available 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.

Emerging applications of spark plasma sintering in all solid-state lithium-ion batteries and beyond

Science.gov (United States)

Zhu, Hongzheng; Liu, Jian

2018-07-01

Solid-state batteries have received increasing attention due to their high safety aspect and high energy and power densities. However, the development of solid-state batteries is hindered by inferior solid-solid interfaces between the solid-state electrolyte and electrode, which cause high interfacial resistance, reduced Li-ion and electron transfer rate, and limited battery performance. Recently, spark plasma sintering (SPS) is emerging as a promising technique for fabricating solid-state electrolyte and electrode pellets with clean and intimate solid-solid interfaces. During the SPS process, the unique reaction mechanism through the combination of current, pressure and high heating rate allow the formation of desirable solid-solid interfaces between active material particles. Herein, this work focuses on the overview of the application of SPS for fabricating solid-state electrolyte and electrode in all solid-state Li-ion batteries, and beyond, such as solid-state Li-S and Na-ion batteries. The correlations among SPS parameters, interfacial resistance, and electrochemical properties of solid-state electrolytes and electrodes are discussed for different material systems. In the end, we point out future opportunities and challenges associated with SPS application in the hot area of solid-state batteries. It is expected that this timely review will stimulate more fundamental and applied research in the development of solid-state batteries by SPS.

Sintering of Multilayered Porous Structures: Part I-Constitutive Models

DEFF Research Database (Denmark)

Olevsky, Eugene; Tadesse Molla, Tesfaye; Frandsen, Henrik Lund

2013-01-01

Theoretical analyses of shrinkage and distortion kinetics during sintering of bilayered porous structures are carried out. The developed modeling framework is based on the continuum theory of sintering; it enables the direct assessment of the cofiring process outcomes and of the impact of process...

Continuum simulation of heat transfer and solidification behavior of AlSi10Mg in Direct Metal Laser Sintering Process

Science.gov (United States)

Ojha, Akash; Samantaray, Mihir; Nath Thatoi, Dhirendra; Sahoo, Seshadev

2018-03-01

Direct Metal Laser Sintering (DMLS) process is a laser based additive manufacturing process, which built complex structures from powder materials. Using high intensity laser beam, the process melts and fuse the powder particles makes dense structures. In this process, the laser beam in terms of heat flux strikes the powder bed and instantaneously melts and joins the powder particles. The partial solidification and temperature distribution on the powder bed endows a high cooling rate and rapid solidification which affects the microstructure of the build part. During the interaction of the laser beam with the powder bed, multiple modes of heat transfer takes place in this process, that make the process very complex. In the present research, a comprehensive heat transfer and solidification model of AlSi10Mg in direct metal laser sintering process has been developed on ANSYS 17.1.0 platform. The model helps to understand the flow phenomena, temperature distribution and densification mechanism on the powder bed. The numerical model takes into account the flow, heat transfer and solidification phenomena. Simulations were carried out for sintering of AlSi10Mg powders in the powder bed having dimension 3 mm × 1 mm × 0.08 mm. The solidification phenomena are incorporated by using enthalpy-porosity approach. The simulation results give the fundamental understanding of the densification of powder particles in DMLS process.

Immobilization of Uranium Silicides in Sintered Glass

International Nuclear Information System (INIS)

Mateos, P.; Russo, D.O.; Heredia, A.D.; Sanfilippo, M.

2003-01-01

High activity nuclear spent fuels vitrification by fusion is a well known technology which has industrial scale in France, England, Japan, EEUU. Borosilicates glasses are used in this process.Sintered glasses are an alternative to the immobilization task in which there is also a wide experience around the world.The available technics are: cold pressing and sintering , hot-pressing and hot isostatic pressing.This work compares Borosilicates and Iron silicates sintered glasses behaviour when different ammounts of nuclear simulated waste is added

Selective laser sintering: A qualitative and objective approach

Science.gov (United States)

Kumar, Sanjay

2003-10-01

This article presents an overview of selective laser sintering (SLS) work as reported in various journals and proceedings. Selective laser sintering was first done mainly on polymers and nylon to create prototypes for audio-visual help and fit-to-form tests. Gradually it was expanded to include metals and alloys to manufacture functional prototypes and develop rapid tooling. The growth gained momentum with the entry of commercial entities such as DTM Corporation and EOS GmbH Electro Optical Systems. Computational modeling has been used to understand the SLS process, optimize the process parameters, and enhance the efficiency of the sintering machine.

Process for obtaining sintered conglomerates with a high density of rare earth oxides and actinides

International Nuclear Information System (INIS)

Pasto, A.E.

1974-01-01

The invention concerns a method to produce agglomerates of actinide and rare earth oxides possessing a cubic-monoclinic transformation in order to obtain high densities close to the theoretical density, and the articles produced by the method. The process is based on the use of a rare earth or actinide oxide, in particular Eu 2 O 3 , with a cubic-monoclinic phase transformation, the oxide being sintered by hot compression at a temperature 50 deg C to 100 deg C above the transformation temperature. The sintered agglomerates obtained can have a purity of at least 99.9% and a density of practically 100%. These agglomerates are suitable in particular for the formation of nuclear reactor control rods [fr

Determination of optimum thermal debinding and sintering process parameters using Taguchi Method

CSIR Research Space (South Africa)

Seerane, M

2015-07-01

Full Text Available powder and a wax-based binder. The binder’s backbone component is a low density polyethylene (LDPE). Careful selection of thermal debinding parameters was guided by thermo- gravimetric analysis (TGA) results. The Taguchi method was used to determine... International Light Metals Technology Conference (LMT 2015), Port Elizabeth, South Africa, July 27-29 Determination of Optimum Process for Thermal Debinding and Sintering using Taguchi Method SEERANE Mandya,*, CHIKWANDA Hildab, MACHAKA Ronaldc CSIR...

Sintering process optimization for multi-layer CGO membranes by in situ techniques

DEFF Research Database (Denmark)

Kaiser, Andreas; Prasad, A.S.; Foghmoes, Søren Preben Vagn

2013-01-01

The sintering of asymmetric CGO bi-layers (thin dense membrane on a porous support; Ce0.9Gd0.1O1.95-delta = CGO) with Co3O4 as sintering additive has been optimized by combination of two in situ techniques. Optical dilatometry revealed that bi-layer shape and microstructure are dramatically...... changing in a narrow temperature range of less than 100 degrees C. Below 1030 degrees C, a higher densification rate in the dense membrane layer than in the porous support leads to concave shape, whereas the densification rate of the support is dominant above 1030 degrees C, leading to convex shape. A fiat...... bi-layer could be prepared at 1030 degrees C, when shrinkage rates were similar. In situ van der Pauw measurements on tape cast layers during sintering allowed following the conductivity during sintering. A strong increase in conductivity and in activation energy E-a for conduction was observed...

Comparative sinterability of combustion synthesized and commercial titanium carbides

International Nuclear Information System (INIS)

Manley, B.W.

1984-11-01

The influence of various parameters on the sinterability of combustion synthesized titanium carbide was investigaged. Titanium carbide powders, prepared by the combustion synthesis process, were sintered in the temperature range 1150 to 1600 0 C. Incomplete combustion and high oxygen contents were found to be the cause of reduced shrinkage during sintering of the combustion syntheized powders when compared to the shrinkage of commercial TiC. Free carbon was shown to inhibit shrinkage. The activation energy for sintering was found to depend on stoichiometry (C/Ti). With decreasing C/Ti, the rate of sintering increased. 29 references, 16 figures, 13 tables

Quality prediction modeling for sintered ores based on mechanism models of sintering and extreme learning machine based error compensation

Science.gov (United States)

Tiebin, Wu; Yunlian, Liu; Xinjun, Li; Yi, Yu; Bin, Zhang

2018-06-01

Aiming at the difficulty in quality prediction of sintered ores, a hybrid prediction model is established based on mechanism models of sintering and time-weighted error compensation on the basis of the extreme learning machine (ELM). At first, mechanism models of drum index, total iron, and alkalinity are constructed according to the chemical reaction mechanism and conservation of matter in the sintering process. As the process is simplified in the mechanism models, these models are not able to describe high nonlinearity. Therefore, errors are inevitable. For this reason, the time-weighted ELM based error compensation model is established. Simulation results verify that the hybrid model has a high accuracy and can meet the requirement for industrial applications.

Challenges in Laser Sintering of Melt-Processable Thermoset Imide Resin

Science.gov (United States)

Chuang, Kathy C.; Gornet, Timothy; Koerner, Hilmar

2016-01-01

Polymer Laser Sintering (LS) is an additive manufacturing technique that builds 3D models layer by layer using a laser to selectively melt cross sections in powdered polymeric materials, following sequential slices of the CAD model. LS generally uses thermoplastic polymeric powders, such as polyamides (i.e. Nylon), and the resultant 3D objects are often weaker in their strength compared to traditionally processed materials, due to the lack of polymer inter-chain connection in the z-direction. The objective of this project is to investigate the possibility of printing a melt-processable RTM370 imide resin powder terminated with reactive phenylethynyl groups by LS, followed by a postcure in order to promote additional crosslinking to achieve higher temperature (250-300 C) capability. A preliminary study to build tensile specimens by LS and the corresponding DSC and rheology study of RTM370 during LS process is presented.

The study of Ashby-type sintering diagrams for uranium dioxide

International Nuclear Information System (INIS)

Georgeoni, P.

1980-01-01

Computer modelling of binary and ternary Ashby-type sintering diagrams for stoechiometric and hyperstoechiometric uranium dioxide (in the range O/U = 2, 0-2, 10). Material data and mass transfer equations, selected from the literature, were used. Sintering isochronous curves were calculated and traced as well. Improvement of a modern dilatometric method by reading and processing experimental curves on a computer and by determining for them a criterion of proximity to the theoretical model equation. It was possible: to develop a reliable method of determination for the dominant mechanism, diffusion coefficient and real process activation energy; to draw up the real sintering diagram; to understand the quantitative and qualitative changes occuring during the actual sintering process of UO 2 , concerning massing and modification of pore shape; to recommend the technological parameters of the thermal regime concerning the elimination of lubricant and binder additives in order to obtain high quality sintered tablets. (author)

Green Compact Temperature Evolution during Current-Activated Tip-Based Sintering (CATS of Nickel

Directory of Open Access Journals (Sweden)

Khaled Morsi

2013-04-01

Full Text Available Current-activated tip-based sintering (CATS is a novel process where spark plasma sintering conditions are applied through an electrically conducting tip on a locally controlled area on a green powder compact/bed. The localization of electric current in CATS allows for unique temporal and spatial current and temperature distributions within the tip and powder compact. In this paper, special experimental setups were used to monitor the temperature profiles in the tip and at multiple locations on the surface of nickel powder compacts. A variation in the initial green density was found to have a significant effect on the maximum temperature in the tip as well as the temperature distribution across the powder compact. In general, the lowest green density specimens displayed the best conditions for localized densification. The concept of effective current density is introduced and results are discussed in relation to the densification parameter.

Plasma processing for VLSI

CERN Document Server

Einspruch, Norman G

1984-01-01

VLSI Electronics: Microstructure Science, Volume 8: Plasma Processing for VLSI (Very Large Scale Integration) discusses the utilization of plasmas for general semiconductor processing. It also includes expositions on advanced deposition of materials for metallization, lithographic methods that use plasmas as exposure sources and for multiple resist patterning, and device structures made possible by anisotropic etching.This volume is divided into four sections. It begins with the history of plasma processing, a discussion of some of the early developments and trends for VLSI. The second section

Plasma exposure of different tungsten grades with plasma accelerators under ITER-relevant conditions

International Nuclear Information System (INIS)

Makhlaj, Vadym A; Garkusha, Igor E; Aksenov, Nikolay N; Byrka, Oleg V; Bazylev, Boris; Landman, Igor; Linke, Jochen; Wirtz, Marius; Malykhin, Sergey V; Pugachov, Anatoliy T; Sadowski, Marek J; Skladnik-Sadowska, Elzbieta

2014-01-01

This paper presents the results of tungsten irradiation experiments performed with three plasma facilities: the QSPA Kh-50 quasi-steady-state plasma accelerator, the PPA pulsed plasma gun and the magneto-plasma compressor. Targets made of different kinds of tungsten (sintered, rolled and deformed) were irradiated with powerful plasma streams at heat fluxes relevant to edge-localized modes in ITER. The irradiated targets were analyzed and two different meshes of cracks were identified. It has been shown that the major cracks do not depend on the tungsten grade. This has been attributed to ductile-to-brittle transition effects. Meshes of inter-granular micro-cracks were detected for energy loads above the melting threshold and these were probably caused by the re-solidification process. The blister-like and cellular-like structures were observed on sample surfaces exposed to helium and hydrogen plasmas. (paper)

Effects of low energy helium plasma irradiation on potassium doped tungsten

Energy Technology Data Exchange (ETDEWEB)

Shu, Xiaoyan [Key Laboratory of Radiation Physics and Technology of Ministry of Education, Institute of Nuclear Science and Technology, Sichuan University, Chengdu (China); Key Subject Laboratory of National Defense for Radioactive Waste and Environmental Security, Southwest University of Science and Technology, Mianyang (China); Huang, Bo [Key Laboratory of Radiation Physics and Technology of Ministry of Education, Institute of Nuclear Science and Technology, Sichuan University, Chengdu (China); Liu, Dongping; Fan, Hongyu [School of Physics and Materials Engineering, Dalian Nationalities University, Dalian (China); Liu, Ning [Key Laboratory of Radiation Physics and Technology of Ministry of Education, Institute of Nuclear Science and Technology, Sichuan University, Chengdu (China); Tang, Jun, E-mail: tangjun@scu.edu.cn [Key Laboratory of Radiation Physics and Technology of Ministry of Education, Institute of Nuclear Science and Technology, Sichuan University, Chengdu (China)

2017-04-15

Effects of helium plasma irradiation on spark plasma sintering (SPS) W-K, pure W and traditionally sintered commercial W-K have been studied, concerning the density, grain size and potassium content as the influence factors. Pinholes are formed under 120 eV He ions at 600 °C and 1 × 10{sup 23} m{sup −2} fluence on the surface of all samples. It is found that SPS-sintered W-K shows the best irradiation resistance among the present samples, and SPS-sintered pure W exhibits higher irradiation tolerance than commercial W-K. Different He-plasma tolerance was observed among the SPS-sintered W-K samples due to varied potassium content and grain size. In addition, the microstructure evolution under helium irradiation, the growth-migration of helium bubbles and their interactions of potassium bubbles have also been discussed.

Sintered cobalt-rare earth intermetallic product

International Nuclear Information System (INIS)

Benz, M.C.

1975-01-01

A process is described for preparing novel sintered cobalt--rare earth intermetallic products which can be magnetized to form permanent magnets having stable improved magnetic properties. A cobalt--rare earth metal alloy is formed having a composition which at sintering temperature falls outside the composition covered by the single Co 5 R intermetallic phase on the rare earth richer side. The alloy contains a major amount of the Co 5 R intermetallic phase and a second solid CoR phase which is richer in rare earth metal content than the Co 5 R phase. The specific cobalt and rare earth metal content of the alloy is substantially the same as that desired in the sintered product. The alloy, in particulate form, is pressed into compacts and sintered to the desired density. The sintered product is comprised of a major amount of the Co 5 R solid intermetallic phase and up to about 35 percent of the product of the second solid CoR intermetallic phase which is richer in rare earth metal content than the Co 5 R phase

Synthesis and characterization of alumina-coated aluminum sponges manufactured by sintering and dissolution process as possible structured reactors

International Nuclear Information System (INIS)

Méndez, Franklin J.; Rivero-Prince, Sayidh; Escalante, Yelisbeth; Villasana, Yanet; Brito, Joaquín L.

2016-01-01

Al_2O_3–Al sponges were manufactured by sintering and dissolution process with the aim of using these materials as structured catalytic reactors. For this purpose, several synthesis conditions were examined for the design of the cellular material, such as: particle size of NaCl, weight fraction of Al, compaction pressure, and sintering temperature or time. An alumina layers was grown on top of the aluminum surfaces during both: sintering and thermal treatment. The obtained results showed that the synthesized materials could be promising as structured reactors for endothermic or exothermic reactions. - Highlights: • An efficient method for manufactured of aluminum sponges is reported. • Methods for productions of superficial Al_2O_3 are studied. • Al_2O_3–Al sponges could be used as structured reactors.

The Properties of Sintered Calcium Phosphate with [Ca]/[P] = 1.50

Directory of Open Access Journals (Sweden)

Moo-Chin Wang

2012-10-01

Full Text Available In order to obtain the properties of the sintered as-dried calcium phosphate with [Ca]/[P] = 1.50, the characteristics of sintered pellets have been investigated using X-ray diffraction (XRD, inductively coupled plasma-mass spectrometry (ICP-MS, Fourier-transform infrared (FT-IR spectra, Vickers hardness indentation and scanning electron microscopy (SEM. When the pellet samples were sintered between 700 °C and 1200 °C for 4 h, the hydroxyapatite (Ca10(PO46(OH2, HA still maintained the major phase, accompanied with the rhenanite (NaCaPO4 as the secondary phase and β-tricalcium phosphate (β-Ca3(PO42, β-TCP as the minor phases. In addition, the HA partially transformed to α-tricalcium phosphate (α-Ca3(PO42, α-TCP and tetracalcium phosphate (Ca4(PO42O, TTCP, when the pellet samples were sintered at 1300 °C and 1400 °C, respectively, for 4 h. The maximum density and Vickers Hardness (HV of sintered pellet samples were 2.85 g/cm3 (90.18% theoretical density (T.D. and 407, which appeared at 1200 °C and 900 °C, respectively.

Critical issues and future directions in sintering science

International Nuclear Information System (INIS)

Brook, R.J.; Tuan, W.H.; Xue, L.A.

1988-01-01

The quality of available powders and the emphasis on direct microstructural observation have continued to improve the value of sintering studies for the processing of ceramics. Future concerns will relate to mechanisms for the correction of microstructural inhomogeneity so that pressureless processing of composites can be reliably achieved and to more systematic exploitation of dopants (sintering additives). These themes are illustrated using examples from the processing of alumina composites and doped barium titanate compositions

High temperature oxidation-sulfidation behavior of Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composites densified by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Saucedo-Acuna, R.A. [Instituto e Ingenieria y Tecnologia, Universidad Autonoma de Cd. Juarez, Av. Del Charro 450 Norte, Col. Partido Romero, C.P. 32310, Cd. Juarez, Chihuahua (Mexico); Monreal-Romero, H.; Martinez-Villafane, A. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); Chacon-Nava, J.G. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico)], E-mail: jose.chacon@cimav.edu.mx; Arce-Colunga, U. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); Universidad Autonoma de Tamaulipas, Matamoros 8 y 9 Col. Centro C.P. 87110, Cd. Victoria, Tamaulipas (Mexico); Gaona-Tiburcio, C. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); De la Torre, S.D. [Centro de Investigacion e Innovacion Tecnologica (CIITEC)-IPN, D.F. Mexico (Mexico)

2007-12-15

The high temperature oxidation-sulfidation behavior of Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composites prepared by mechanical alloying (MA) and spark plasma sintering (SPS) has been studied. These composite powders have a particular metal-ceramic interpenetrating network and excellent mechanical properties. Oxidation-sulfidation tests were carried out at 900 deg. C, in a 2.5%SO{sub 2} + 3.6%O{sub 2} + N{sub 2}(balance) atmosphere for 48 h. The results revealed the influence of the sintering conditions on the specimens corrosion resistance, i.e. the Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composite sintered at 1310 deg. C/4 min showed better corrosion resistance (lower weight gains) compared with those found for the 1440 deg. C/5 min conditions. For the former composite, a protective Cr{sub 2}O{sub 3} layer immediately forms upon heating, whereas for the later pest disintegration was noted. Thus, under the same sintering conditions the Nb-Al{sub 2}O{sub 3} composites showed the highest weight gains. The oxidation products were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy.

Integrated analysis of oxide nuclear fuel sintering

International Nuclear Information System (INIS)

Baranov, V.; Kuzmin, R.; Tenishev, A.; Timoshin, I.; Khlunov, A.; Ivanov, A.; Petrov, I.

2011-01-01

Dilatometric and thermal-gravimetric investigations have been carried out for the sintering process of oxide nuclear fuel in gaseous Ar - 8% H 2 atmosphere at temperatures up to 1600 0 C. The pressed compacts were fabricated under real production conditions of the OAO MSZ with application of two different technologies, so called 'dry' and 'wet' technologies. Effects of the grain size growth after the heating to different temperatures were observed. In order to investigate the effects produced by rate of heating on properties of sintered fuel pellets, the heating rates were varied from 1 to 8 0 C per minute. Time of isothermal overexposure at maximal temperature (1600 0 C) was about 8 hours. Real production conditions were imitated. The results showed that the sintering process of the fuel pellets produced by two technologies differs. The samples sintered under different heating rates were studied with application of scanning electronic microscopy analysis for determination of mean grain size. A simulation of heating profile for industrial furnaces was performed to reduce the beam cycles and estimate the effects of variation of the isothermal overexposure temperatures. Based on this data, an optimization of the sintering conditions was performed in operations terms of OAO MSZ. (authors)

Mechanical characteristics of microwave sintered silicon carbide

Indian Academy of Sciences (India)

In firing of products by conventionally sintered process, SiC grain gets oxidized producing SiO2 (∼ 32 wt%) and deteriorates the quality of the product substantially. Partially sintered silicon carbide by such a method is a useful material for a varieties of applications ranging from kiln furniture to membrane material.

Advanced research and development for plasma processing of polymers with combinatorial plasma-process analyzer

International Nuclear Information System (INIS)

Setsuhara, Yuichi; Cho, Ken; Takenaka, Kosuke; Shiratani, Masaharu; Sekine, Makoto; Hori, Masaru

2010-01-01

A plasma-process analyzer has been developed on the basis of combinatorial method, in which process examinations with continuous variations of plasma-process conditions can be carried out on a substrate holder with an inclined distribution of process parameters. Combinatorial plasma-process analyses have been demonstrated for examinations of plasma-polymer interactions in terms of etching characteristics and surface morphologies in order to show feasibility and effectiveness of the methodology as advanced research and development for next-generation plasma nano processes. The etching properties and surface morphologies have been investigated for polyethylene terephthalate (PET) films exposed to argon-oxygen mixture plasmas. The etching depth data obtained from three independent batches of the experiments showed universal and almost linear dependence with increasing product of (ion saturation current) x (exposure time); i.e. ion dose. Surface roughness of the polymer slightly increased with increasing ion dose, while the mean spacing after plasma exposure was found to decrease monotonically with increasing ion dose but was saturated at the level of approximately 250 nm.

Alloying behavior and deformation twinning in a CoNiFeCrAl0.6Ti0.4 high entropy alloy processed by spark plasma sintering

International Nuclear Information System (INIS)

Fu, Zhiqiang; Chen, Weiping; Fang, Sicong; Zhang, Dayue; Xiao, Huaqiang; Zhu, Dezhi

2013-01-01

Highlights: ► CoNiFeCrAl 0.6 Ti 0.4 high entropy alloy has been synthesized via MA and SPS. ► Deformation twinning possibly occurred during MA or SPS. ► This alloy exhibits excellent mechanical properties. ► The fracture mechanism of this alloy is intergranular fracture and plastic fracture. -- Abstract: Inequi-atomic CoNiFeCrAl 0.6 Ti 0.4 high entropy alloy has been designed and fabricated by mechanical alloying (MA) and spark plasma sintering (SPS). Alloying behavior, microstructure, phase evolution and mechanical properties of CoNiFeCrAl 0.6 Ti 0.4 alloy were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM), as well as by an Instron testing system. During MA, a supersaturated solid solution consisting of a FCC phase and a metastable BCC phase was formed. Two FCC phases (named FCC1 and FCC2) and a new BCC phase were observed after SPS. During SPS, the metastable BCC phase transformed into the FCC2 phase and the new BCC phase. Meanwhile, the FCC1 phase was the initial FCC phase which was formed during MA. Moreover, nanoscale twins obviously presented only in partial FCC1 phase after SPS. Deformation twinning may be occurred during MA or SPS. The sintered alloy with a high relative density of 98.83% exhibits excellent comprehensive mechanical properties. The yield stress, compressive strength, compression ratio and Vickers hardness of the alloy are 2.08, 2.52 GPa, 11.5% and 573 H V , respectively. The fracture mechanism of CoNiFeCrAl 0.6 Ti 0.4 high entropy alloy is mainly performed at intergranular fracture and plastic fracture mode

Improving NASICON Sinterability through Crystallization under High Frequency Electrical Fields

Directory of Open Access Journals (Sweden)

Ilya eLisenker

2016-03-01

Full Text Available The effect of high frequency (HF electric fields on the crystallization and sintering rates of a lithium aluminum germanium phosphate (LAGP ion conducting ceramic was investigated. LAGP with the nominal composition Li1.5Al0.5Ge1.5(PO43 was crystallized and sintered, both conventionally and under effect of electrical field. Electrical field application, of 300V/cm at 1MHz, produced up to a 40% improvement in sintering rate of LAGP that was crystallized and sintered under the HF field. Heat sink effect of the electrodes appears to arrest thermal runaway and subsequent flash behavior. Sintered pellets were characterized using XRD, SEM, TEM and EIS to compare conventionally and field sintered processes. The as-sintered structure appears largely unaffected by the field as the sintering curves tend to converge beyond initial stages of sintering. Differences in densities and microstructure after 1 hour of sintering were minor with measured sintering strains of 31% vs. 26% with and without field, respectively . Ionic conductivity of the sintered pellets was evaluated and no deterioration due to the use of HF field was noted, though capacitance of grain boundaries due to secondary phases was significantly increased.

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

Science.gov (United States)

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

2014-02-01

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

Rapid laser sintering of metal nano-particles inks.

Science.gov (United States)

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.

Interface structure and properties of CNTs/Cu composites fabricated by electroless deposition and spark plasma sintering