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At least 1,099 records · Page 61
All sourcesNASA NTRSDOE OSTI
NASA NTRS1987

Structure and grain coarsening during the processing of engineering ceramics

Studies have been made of three ceramic systems (Al2O3, Y2O3/MgO, and SiC/C/B), both to explore a surface area/density diagram approach to examining the coarsening processes during sintering and to explore an alternative coarsening parameter, i.e., the grain boundary surface area (raising it at a given value of the density) and not the pore surface area; therefore, pinning of the grain boundaries by solid-solution drag is the only function evidenced by these results. The importance of such pinning even at densities as low as 75% of theoretical is linked to the existence of microstructural inhomogeneities. The early stages of sintering of Y2O3 powder have been examined using two techniques, BET surface area analysis and transmission electron microscopy. Each has given some insight into the process occurring and, used together, have provided some indication of the effect of MgO on coarsening during sintering. Attempts to further elucidate effects of MgO on the coarsening behavior of Y2O3 by the surface area/density diagram approach were unsuccessful due to masking effects of contaminating reactions during sintering and/or thermal etching. The behavior of the undoped SiC which only coarsens can be clearly distinguished by the surface area/density diagram from that of SiC/C/B which also concurrently densifies. Little additional information was obtainable by this method due to unfavorable sample etching characteristics. The advantages, disadvantages, and difficulties of application of these techniques to the study of coarsening during sintering are discussed.

Shaw, Nancy J.↗
NASA NTRS1986

Improved silicon carbide for advanced heat engines

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

Whalen, T. J.↗
NASA NTRS1990

Processing effects on the mechanical properties of tungsten heavy alloys

Tungsten heavy alloys exhibit significant mechanical property sensitivities to the fabrication variables. These sensitivities are illustrated in this examination of vacuum sintering and the effects of composition, sintering temperature, and sintering time on the mechanical properties of tungsten heavy alloys. Measurements were conducted to assess the density, strength, hardness, and elongation dependencies. A detrimental aspect of vacuum sintering is matrix phase evaporation, although vacuum sintering does eliminate the need for postsintering heat treatments.

Kishi, Toshihito↗
NASA NTRS1992

Development of high T(sub c) (greater than 110 K) Bi, Tl, and Y-based materials as superconducting circuit elements

Experimental work has continued on the development and characterization of bulk and hot pressed powders and tapecast materials in the Bi-Sr-Ca-Cu-O and Tl-Ba-Ca-Cu-O systems. A process for producing warp-free, sintered, superconducting tapes of Bi composition Bi2Sr2Ca2Cu3O(x) with a mixed oxide process was established. This procedure required a triple calcination at 830 C for 24 hours and sintering at 845 C from 20 to 200 hours. Hot pressing the triple calcined powder at 845 C for 6 hours at 5000 psi yielded a dense material which on further heat treatment at 845 C for 24 hours exhibited a Tc of 108.2 K. A further improvement in the processing of the bismuth materials was achieved via a chemical coprecipitation process wherein the starting nitrate materials were coprecipitated with oxalic acid, thus yielding a more chemically homogeneous, more reactive powder. With the coprecipitated powders, only one calcine at 830 C for 12 hours and a final sinter at 845 C for 30 hours was sufficient to produce a bulk superconducting material with a Tc of 108.4 K. SAFIRE-type grounding links were successfully fabricated from sintered, tapecast, coprecipitated BSCCO 2223 powders. Compositional and processing investigations were continued on the Tl-based superconductors. Manganese and lithium additions and sintering temperature and time were examined to determine their influence on superconducting properties. It was found that lithium substitutions for copper enhance the transition temperatures while manganese additions produced deleterious effects on the superconducting properties. A suitable procedure for producing reproducible bulk and tapecast material of Tl composition Tl2Ba2Ca2Cu3O(x) was developed and used in fabricating uniform superconducting tapes. The highest transition temperature for Tl-based tapes was measured at 110.2 K. Thallium superconducting SAFIRE-type grounding links were fabricated from the tapes.

Haertling, Gene H.↗
NASA NTRS2000

Long Life Nickel Electrodes for Nickel-Hydrogen Cells: Fiber Substrates Nickel Electrodes

Samples of nickel fiber mat electrodes were investigated over a wide range of fiber diameters, electrode thickness, porosity and active material loading levels. Thickness' were 0.040, 0.060 and 0.080 inches for the plaque: fiber diameters were primarily 2, 4, and 8 micron and porosity was 85, 90, and 95%. Capacities of 3.5 in. diameter electrodes were determined in the flooded condition with both 26 and 31% potassium hydroxide solution. These capacity tests indicated that the highest capacities per unit weight were obtained at the 90% porosity level with a 4 micron diameter fiber plaque. It appeared that the thinner electrodes had somewhat better performance, consistent with sintered electrode history. Limited testing with two-positive-electrode boiler plate cells was also carried out. Considerable difficulty with constructing the cells was encountered with short circuits the major problem. Nevertheless, four cells were tested. The cell with 95% porosity electrodes failed during conditioning cycling due to high voltage during charge. Discharge showed that this cell had lost nearly all of its capacity. The other three cells after 20 conditioning cycles showed capacities consistent with the flooded capacities of the electrodes. Positive electrodes made from fiber substrates may well show a weight advantage of standard sintered electrodes, but need considerably more work to prove this statement. A major problem to be investigated is the lower strength of the substrate compared to standard sintered electrodes. Problems with welding of leads were significant and implications that the electrodes would expand more than sintered electrodes need to be investigated. Loading levels were lower than had been expected based on sintered electrode experiences and the lower loading led to lower capacity values. However, lower loading causes less expansion and contraction during cycling so that stress on the substrate is reduced.

Rogers, Howard H.↗
NASA NTRS2002

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

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

Zhu, Dongming↗
NASA NTRS1984

Method of forming a relatively stable slip of silicon metal particles and yttrium containing particles

The method concerns forming a relatively stable slip of silicon metal particles and yttrium containing particles. In one embodiment, a casting slip of silicon metal particles is formed in water. Particles of a yttrium containing sintering aid are added to the casting slip. The yttrium containing sintering aid is a compound which has at least some solubility in water to form Y.sup.+3 ions which have a high potential for totally flocculating the silicon metal particles into a semiporous solid. A small amount of a fluoride salt is added to the casting slip which contains the yttrium containing sintering aid. The fluoride salt is one which will produce fluoride anions when dissolved in water. The small amount of the fluoride anions produced are effective to suppress the flocculation of the silicon metal particles by the Y.sup.+3 ions so that all particles remain in suspension in the casting slip and the casting slip has both an increased shelf life and can be used to cast articles having a relatively thick cross-section. The pH of the casting slip is maintained in a range from 7.5 to 9. Preferably, the fluoride salt used is one which is based on a monovalent cation such as sodium or ammonia. The steps of adding the yttrium containing sintering aid and the fluoride salt may be interchanged if desired, and the salt may be added to a solution containing the sintering aid prior to addition of the silicon metal particles.

Dickie, Ray A.↗
DOE OSTI2018

Hybrid additive manufacturing methods using hybrid additively manufactured features for hybrid components

A hybrid additive manufacturing method comprises building an additive structure on a pre-sintered preform base, wherein building the additive structure comprises iteratively fusing together a plurality of layers of additive material with at least a first layer of additive material joined to the pre-sintered preform base, and wherein the pre-sintered preform base comprises an initial shape. The hybrid additive manufacturing method further comprises modifying the initial shape of the pre-sintered preform base comprising the additive structure into a modified shape comprising the additive structure, and, joining the pre-sintered preform base in its modified shape to a component.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure Evolution During Controlled Solidification of “Fe{sub 2}O{sub 3}”-CaO-SiO{sub 2} Liquids in Air

The principal chemical components in iron ore sintering are Fe{sub 2}O{sub 3}, CaO, and SiO{sub 2}. This sintering process consists of three key steps: heating, holding at peak temperature, and cooling. During the cooling stage, a liquid oxide solidifies to form the final sinter microstructures. To investigate the fundamental processes taking place during the cooling of sinters, a new experimental technique has been developed that allows the stages of solidification to be determined in isolation, rather than inferred from the final microstructures. Fe{sub 2}O{sub 3}-CaO-SiO{sub 2} oxide samples of a bulk composition having a CaO/SiO{sub 2} mass ratio of 3.46 and 73.2 wt pct Fe{sub 2}O{sub 3} were cooled in air from 1623 K (1350 °C) at 2 K/s, quenched at 5 K temperature intervals from 1533 K to 1453 K (1260 °C to 1180 °C), and analyzed using Electron Probe Micro X-Ray Analysis (EPMA). During cooling, four distinct stages were observed, consisting of the phase assemblages Liquid + Hematite (I), Liquid + Hematite + C{sub 2}S(II), Liquid + C{sub 2}S + CF{sub 2}(III), and C{sub 2}S + CF{sub 2} + CF (IV). This solidification sequence differs from that predicted under equilibrium and Scheil–Gulliver Cooling. Importantly, no Silico-Ferrite of Calcium (SFC) phase was observed to form on solidification of the liquid. Based on the microstructures formed and liquid compositions, measured by EPMA, it was demonstrated that kinetic factors play a major role in determining the phases and microstructures formed under the conditions investigated.

36 MATERIALS SCIENCE↗
DOE OSTI2018

In situ measurement of temperature and reduction of rutile titania using energy dispersive x-ray diffraction

Using in situ energy dispersive x-ray diffraction (EDXRD) the average specimen temperature of TiO 2 in the steady state of flash is experimentally determined. Comparison of the microstructure for flash sintering and conventional sintering in addition to the temperature determined from calibration of the unit cell expansion indicates that rapid Joule heating during flash sintering causes densification and grain growth comparable with conventional sintering. An average temperature approximation model is proposed to account for greybody radiation and thermal conduction. In conclusion, the inhomogeneity of the grain growth across the sample length is confirmed to correlate with inhomogeneity in temperature distribution and this suggests a current induced Peltier effect in n-type TiO 2 .

36 MATERIALS SCIENCE↗
DOE OSTI2018

Synthesis, Processing and Properties of Calcium- and Nickel-Doped Yttrium Chromates(III) Y{sub 0.8}Ca{sub 0.2}Cr{sub 1−x}Ni{sub x}O{sub 3} (x = 0-0.3) and Studies on Their Potential Application as Coatings for SOFC Interconnects

In the present study, a calcium- and nickel-doped yttrium chromates (YCCN)-based, conductive–protective layers for metallic interconnects used in the intermediate-temperature solid oxide fuel cells (IT-SOFCs) were investigated. Synthesis of Y{sub 0.8}Ca{sub 0.2}Cr{sub 1−x}Ni{sub x}O{sub 3} (x = 0; 0.15 and 0.3) powders was performed using a wet chemistry method with two different complexing agents: ethylenediaminetetraacetic acid and glycine. Based on the result of thermal analysis of obtained precursors, optimal conditions of the calcination process were determined. Powders were then milled, compacted and sintered at different temperatures using free sintering method, into series of dense, polycrystalline sinters. The use of glycine precursor allowed obtaining a single-phase material in all cases. Based on the electrical and sintering properties, the Y{sub 0.8}Ca{sub 0.2}Cr{sub 0.85}Ni{sub 0.15}O{sub 3} material was selected for further studies. It was deposited using cost-effective screen-printing method on the Crofer 22APU ferritic stainless steel. To investigate properties and suitability of the resulting layer/steel system for IT-SOFCs applications, the high-temperature, dual-atmosphere studies were carried out for the first time for ceramic/metallic system, in conditions as close as possible to actual working conditions of the fuel cell. The layer exhibited high stability and good protective properties. The area-specific resistance of the studied ceramic layer/metallic substrate composite was determined, with the obtained value of 0.0366 Ω cm{sup 2} being within the arbitrary limit set for these materials (0.1 Ω cm{sup 2}). The results show that the investigated materials are suitable for the projected application.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Enhanced Mechanical, Tribological, and Thermal Properties of Fe{sub 3}Al Composites with Carbon Nanotubes

In this work, Fe{sub 3}Al-based composites reinforced with carbon nanotubes were fabricated by a hot-press sintering process under various sintering pressures. The effects of sintering pressure and additives (alumina and lanthanum) on both the physical and the mechanical properties were systematically investigated. Results showed that with the sintering pressure of 15 MPa and incorporation of carbon nanotubes (CNTs), the microhardness of Fe{sub 3}Al composite exhibited a peak value at 1038.1 HV, which was ~ 60% higher than those without the addition of carbon nanotubes (644.9 HV). Also, both the compressive yield strength and the thermal conductivity of Fe{sub 3}Al composite were also significantly improved. Results of wear test showed the Fe{sub 3}Al composite exhibited a low wearing rate (10{sup −6}-10{sup −5} order of magnitude) and a friction coefficient (0.53-0.67).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Manufacturing and characterization of Ni-free N-containing ODS austenitic alloys

Ni-free N-containing oxide dispersion strengthened (ODS) austenitic alloys were manufactured by mechanical alloying (MA) followed by spark plasma sintering (SPS). The phase evolutions during milling under a nitrogen atmosphere and after sintering were studied by X-ray diffraction (XRD). Transmission electron microcopy (TEM) and contrast variation analysis (ACV), including small-angle neutron scattering (SANS) and ultra-small X-ray scattering (USAXS), revealed the existence of nanoparticles with a diameter of 3-51 nm for the samples sintered at 950 ºC. Sintering at 1000 ºC for 5 and 15 min caused slight growth and a significant coarsening of the nanoparticles, up to 70 nm and 128 nm, respectively. The ACV analysis indicated the existence of two populations of Y2O3, ε-martensite and MnO. The dispersive X-ray spectrometry (EDS) confirmed two kinds of nanoparticles, Y2O3 and MnO. The material was characterized by superior micro-hardness, of above 500 HV0.1.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The Li{sup +} conducting composite based on LiTi{sub 2}(PO{sub 4}){sub 3} and Li{sub 3}BO{sub 3} glass

Highlights: • Addition of the LBO glass enhance total ion conductivity up to four orders of magnitude. • Transport of Li{sup +} could be attributed to two media: grains and grain boundaries. • Sintering temperature is the most influential factor affecting the σ{sub tot}. • Melting of the LBO above 700 °C supports the sintering process. - Abstract: The LiTi{sub 2}(PO{sub 4}){sub 3} based composites containing amorphous Li{sub 3}BO{sub 3} were formed and investigated by means of X–ray diffractometry, thermogravimetry, scanning electron microscopy, impedance spectroscopy and density methods. The study shows that when a polycrystalline LiTi{sub 2}(PO{sub 4}){sub 3} material is sintered with Li{sub 3}BO{sub 3} glass, the resultant ceramics exhibit very high total ion conductivity. The maximum conductivity of 1.43 × 10{sup −4} S cm{sup −1} at 30 °C was achieved for the LTP–0.3LBO material sintered at 900 °C compared to 5.15 × 10{sup −8} S cm{sup −1} of the ceramic LiTi{sub 2}(PO{sub 4}){sub 3}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

The facile synthesis, crystallization behavior and magnetic property of FeNiP amorphous nanoparticles

Highlights: • A facile chemistry method was proposed to synthesize amorphous FeNiP nanoparticle. • Phase transformation happened during sintering the amorphous nanoparticle. • Ni nanospheres and monoclinic (Ni,Fe){sub 3}[PO4]{sub 2} nanorods appeared at 800 °C. • Crystallization behavior is α-FeNiP → Ni + FeNi{sub 3} + Ni{sub 3}P → Ni + (Ni,Fe){sub 3}[PO{sub 4}]{sub 2}. • Sintered powders have varied magnetic properties due to phase proportion change. - Abstract: Amorphous FeNiP nanoparticles with homogeneous composition are synthesized by reduction of aqueous Fe{sup 2 +} and Ni{sup 2 +} with sodium borohydride (NaBH{sub 4}) and hypophosphite at room temperature. These amorphous nanoparticles can be crystallized by heating up to 300 °C to form FeNi{sub 3} and Ni{sub 3}P crystals. Ni phase appeared at the sintering temperature of 500 °C, and a special net structure was formed at 700 °C due to the joining and diffusion among different nanoparticles. At a higher temperature of 800 °C, phase transformation happened and only pure Ni nanospheres and monoclinic ((Ni, Fe){sub 3}[PO{sub 4}]{sub 2}) nanorods can be observed, which should be governed by the long-range diffusion in the net structure. The amorphous FeNiP nanoparticles have excellent soft magnetic property with Ms of 13.2 emu/g and Hc of 0.7 Oe. However, the sintered mixing nanoparticles show varied magnetic properties due to the phase transformation and proportion change among different phases involved in.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Comparative investigation on microstructures and mechanical properties of (TiB + TiC)/Ti-6Al-4V composites from Ti-B4C-C and Ti-TiB2-TiC systems

Highlights: • The (TiB{sub w}+TiC{sub p})/Ti-6Al-4V composites were fabricated from Ti-B{sub 4}C-C and Ti-TiB{sub 2}-TiC systems by reactive hot-pressed sintering. • Microstructures and mechanical properties of the two kinds of composites were comparatively investigated. • The composites from Ti-TiB{sub 2}-TiC system possess higher elastic modulus and Vickers hardness than those from Ti-B{sub 4}C-C system. • The composites from Ti-TiB{sub 2}-TiC system have higher bending strength than the other system while employing same conditions. • The composites from Ti-B{sub 4}C-C system present better abrasion resistance than those from Ti-TiB{sub 2}-TiC system. - Abstract: Two percentages of TiB + TiC reinforced Ti-6Al-4V composites from Ti-B{sub 4}C-C and Ti-TiB{sub 2}-TiC systems were fabricated by reactive hot-pressed sintering. Their microstructures and mechanical properties involving elastic modulus, Vickers hardness, bending strength and wear property were investigated comparatively. The experimental results show that needle-like TiB whiskers and near-equiaxed TiC particles are evenly distributed in the Ti-6Al-4V matrix. The mechanical properties of the (TiB + TiC)/Ti-6Al-4V composites are closely related with the nominal composition and synthesis system of TiB + TiC reinforcement and the microstructures of composites. With increasing the nominal volume fraction of reinforcement, both elastic modulus and Vickers hardness increase more or less and the bending strength decreases in varying degrees. A certain increase of pores in the composites with the sintering temperature increasing to 1300 °C can markedly affect the bending strength. Moreover, no matter what the sintering temperature and nominal volume fraction of reinforcement, the elastic modulus and Vickers hardness of composites from the Ti-TiB{sub 2}-TiC system are higher than those from the Ti-B{sub 4}C-C system. Similarly, the composites from the Ti-B{sub 4}C-C system present better abrasion resistance than those from the Ti-TiB{sub 2}-TiC system due to the difference of interfacial bonding between the TiC particles and Ti-6Al-4V matrix in the two kinds of composites.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Braunite phase embedded Y2O3/MnO2-Al2O3-CaO-SiO2 glass ceramics and their properties

Highlights: • Nucleation of synthetic braunite structure (Mn{sub 7}SiO{sub 12}) on sintering of Y{sub 2}O{sub 3}/MnO{sub 2}-CaO-Al{sub 2}O{sub 3}-SiO{sub 2} glasses at 850 °C. • Lossy capacitor behaviour. • Exhibits a critical temperature in 500–600 °C range. • Conduction mechanism shift from Superlinear power law to universal dielectric response law with increase in temperature. - Abstract: Glass series (20-x)Y{sub 2}O{sub 3}-xMnO{sub 2}-20Al{sub 2}O{sub 3}-40SiO{sub 2}-20CaO (x = 5, 10, 15 and 20, mol%) have been synthesized by melt quench technique followed by sintering at 850 °C. The optical band gap of the samples is in wide semiconductor range and increased with MnO{sub 2} content. Photoluminescence study exhibits emission in Mn{sup 2+} d-states. On the other hand, hardness decreases with MnO{sub 2} content except for 10 mol% MnO{sub 2} containing glasses (YM10). The formation of braunite phase in glass ceramics induces capacitive losses. In lower temperature region, the conductivity behaviour of samples follows superlinear power law. In higher temperature region, it follows the universal law of conduction. The dielectric constant for the sintered glasses is constant with respect to temperature, approximately upto 350 °C and 1 MHz frequency. Above 350 °C, the ionic conduction dominates in all the sintered glasses. The anomaly in properties is observed when the ratio of Y{sub 2}O{sub 3}/MnO{sub 2} is 1:1.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Superconductor-in-an-Hour: Spark Plasma Synthesis of Co- and Ni-Doped BaFe 2 As 2

In this work, BaFe 2 As 2 superconductors doped with Co or Ni were synthesized by heat treatment of the reactive BaH 2 precursor and elemental Fe, Co, Ni, and As in a sealed niobium container. The hydride route provides better mixing of the starting materials, resulting in faster preparation of the target phases. The hydrogen gas evolved during sintering facilitates the preparation of the oxygen-free powders. Using powder X-ray diffraction (PXRD), including low-temperature synchrotron PXRD, it was shown that this route leads to successful doping of the Co (Ni) dopant and that the actual dopant content in the produced powdered samples of BaFe 2– x Co x As 2 (0 ≤ x ≤ 0.4) and BaFe 2– x Ni x As 2 (0 ≤ x ≤ 0.18) is close to the nominal content. The optimally doped samples of BaFe 2– x Co x As 2 and BaFe 2– x Ni x As 2 exhibit bulk superconducting properties. The highest T c for the Co-doped sample is 24 K when x = 0.15–0.175 and 21 K for the Ni-doped sample when x ~ 0.1. The reaction mechanism between the BaH 2 hydride precursor and elemental Fe and As was studied by operando high-temperature synchrotron PXRD. The formation of the target BaFe 2 As 2 phase occurs at the relatively low temperature of 785 K with binary iron arsenide (FeAs) being an intermediate product. Finally, the in situ combined synthesis and sintering of the intimately mixed BaH 2 and Fe, Co, and As was performed inside the spark plasma sintering apparatus to obtain compact pellets of the BaFe 2– x Co x As 2 superconductors. A higher sintering temperature (>873 K) is needed to ensure a homogeneous Co dopant distribution and, thus, the abrupt superconducting transitions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗