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At least 55 records · Page 3

Plastic and low-cost axial zero thermal expansion alloy by a natural dual-phase composite

Zero thermal expansion (ZTE) alloys possess unique dimensional stability, high thermal and electrical conductivities. Their practical application under heat and stress is however limited by their inherent brittleness because ZTE and plasticity are generally exclusive in a single-phase material. Besides, the performance of ZTE alloys is highly sensitive to change of compositions, so conventional synthesis methods such as alloying or the design of multiphase to improve its thermal and mechanical properties are usually inapplicable. In this study, by adopting a one-step eutectic reaction method, we overcome this challenge. A natural dual-phase composite with ZTE and plasticity was synthesized by melting 4 atom% holmium with pure iron. The dual-phase alloy shows moderate plasticity and strength, axial zero thermal expansion, and stable thermal cycling performance as well as low cost. By using synchrotron X-ray diffraction, in-situ neutron diffraction and microscopy, the critical mechanism of dual-phase synergy on both thermal expansion regulation and mechanical property enhancement is revealed. These results demonstrate that eutectic reaction is likely to be a universal and effective method for the design of high-performance intermetallic-compound-based ZTE alloys.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Room temperature colossal superparamagnetic order in aminoferrocene–graphene molecular magnets

Intensive studies are published for graphene-based molecular magnets due to their remarkable electric, thermal, and mechanical properties. However, to date, most of all produced molecular magnets are ligand based and subject to challenges regarding the stability of the ligand(s). The lack of long-range coupling limits high operating temperature and leads to a short-range magnetic order. Herein, we introduce an aminoferrocene-based graphene system with room temperature superparamagnetic behavior in the long-range magnetic order that exhibits colossal magnetocrystalline anisotropy of 8 × 10 5 and 3 × 10 7 J/m 3 in aminoferrocene and graphene-based aminoferrocene, respectively. These values are comparable to and even two orders of magnitude larger than pure iron metal. Aminoferrocene [C 10 H 11 FeN] + is synthesized by an electrophilic substitution reaction. It was then reacted with graphene oxide that was prepared by the modified Hammers method. The phase structure and functionalization of surface groups were characterized and confirmed by XRD, FT-IR, and Raman spectroscopy. To model the behavior of the aminoferrocene between two sheets of hydroxylated graphene, we have used density functional theory by placing the aminoferrocene molecule between two highly ordered hydroxylated sheets and allowing the structure to relax. Here, the strong bowing of the isolated graphene sheets suggests that the charge transfer and resulting magnetization could be strongly influenced by pressure effects. In contrast to strategies based on ligands surface attachment, our present work that uses interlayer intercalated aminoferrocene opens routes for future molecular magnets as well as the design of qubit arrays and quantum systems.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Effect of Metal Chloride Impurities on Equilibrium Potential of Fe/FeCl 2 in Eutectic LiCl-KCl

In this study, interaction of dilute metal chloride solutes in molten eutectic LiCl-KCl was studied via equilibrium potential measurements. Open circuit potential (OCP) was measured between a pure iron rod and a Ag/AgCl reference electrode with concentration of FeCl 2 varying from 0.2–1 mol% at 530 °C. The Nernst equation was used to calculate activity coefficient of FeCl 2 based on OCP. Measurements were made in LiCl-KCl-FeCl 2 with and without additions of 0.5 mol% CsCl, NaCl, and LaCl 3 . The activity coefficient of FeCl 2 was found to be unaffected by these small concentrations of CsCl, LaCl 3 , and NaCl. However, there was observed evidence that the activity coefficient of FeCl 2 , above 0.8 mol% Fe, may be affected by the presence of LaCl 3 at higher concentrations beginning around 0.5 mol% La. Over the full range of conditions tested, the activity coefficient of FeCl 2 in molten LiCl-KCl ranged from 2.95 × 10 −5 to 1.01 × 10 −4 .

Electrochemistry↗

Research on metal solidification in zero-g state

The containerless solidification of several pure metals and metallic alloys was studied in a low gravity environment. The tests were performed in the MSFC 4.2 s drop tower using a rapid wire melting apparatus designed and built for this purpose. Pure iron and nickel, and alloys of iron-nickel, iron-carbon, nickel-aluminum and tungsten-rhenium were all melted and solidified at a gravity level of approximately 100.000/-4 g. Interpretation of the results has led to an appreciation of the factors controlling the successful execution of this drop test experiment and to a delineation of the limits of applicability of the apparatus. Preliminary metallurgical evaluations are presented of the overall shapes, lattice parameters, surface microstructure,, cross-sectional microstructures, solidification and transformation sequences, evaporative segregation, and localized solute redistribution observed in the low-gravity specimens. The effects of low gravity on metallic solidification are discussed with particular emphasis on observations of spontaneous undercooling and evaporative segregation in uncontained melts.

Papazian, J. M.↗

Utilization of nuclear methods for materials analysis and the determination of concentration gradients

The various types of nuclear chemical analysis methods are discussed. The possibilities of analysis through activation and direct observation of nuclear reactions are described. Such methods make it possible to analyze trace elements and impurities with selectivity, accuracy, and a high degree of sensitivity. Such methods are used in measuring major elements present in materials which are available for analysis only in small quantities. These methods are well suited to superficial analyses and to determination of concentration gradients; provided the nature and energy of the incident particles are chosen judiciously. Typical examples of steels, pure iron and refractory metals are illustrated.

Darras, R.↗

Evaluation and auger analysis of a zinc-dialkyl-dithiophosphate antiwear additive in several diester lubricants

The wear of pure iron in sliding contact with hardened M-2 tool steel was measured for a series of synthetic diester fluids, both with and without a zinc dialkyl dithiophosphate (ZDP) antiwear additive, as test lubricants. Selected wear scars were analyzed by an Auger emission spectroscopy (AES) depth profiling technique in order to assess the surface film elemental composition. The ZDP was an effective antiwear additive for all the diesters except dibutyl oxalate and dibutyl sebacate. The high wear measured for the additive-containing oxalate was related to corrosion; the higher wear measured for the additive-containing sebacate was due to an oxygen interaction. The AES of dibutyl sebacate surfaces run in dry air and in dry nitrogen showed large differences only in the amount of oxygen present. The AES of worn surfaces where the additive was effective showed no zinc, only a little phosphorus, and large amounts of sulfur.

Brainard, W. A.↗

Steady-state wear and friction in boundary lubrication studies

A friction and wear study was made at 20 C to obtain improved reproducibility and reliability in boundary lubrication testing. Ester-base and C-ether-base fluids were used to lubricate a pure iron rider in sliding contact with a rotating M-50 steel disk in a friction and wear apparatus. Conditions included loads of 1/2 and 1 kg and sliding velocities of 3.6 to 18.2 m/min in a dry air atmosphere and stepwise time intervals from 1 to 250 min for wear measurements. The wear rate results were compared with those from previous studies where a single 25 min test period was used. Satisfactory test conditions for studying friction and wear in boundary lubrication for this apparatus were found to be 1 kg load; sliding velocities of 7.1 to 9.1 m/min (50 rpm disk speed); and use of a time stepwise test procedure. Highly reproducible steady-state wear rates and steady-state friction coefficients were determined under boundary conditions. Wear rates and coefficients of friction were constant following initially high values during run-in periods.

Loomis, W. R.↗

Evaluation of boundary lubricants using steady-state wear and friction

A friction and wear study was made at 20 C to establish operating limits and procedures for obtaining improved reproducibility and reliability in boundary lubrication testing. Ester base and C-other base fluids were used to lubricate a pure iron rider in sliding contact with a rotating M-50 steel disk in a pin-on-disk apparatus. Results of a parametric study with varying loads and speeds slowed that satisfactory test conditions for studying the direction and wear characteristics in the boundary lubrication regime with this test device were found to be 1 kilogram load; 7 to 9 meters-per-minute (50 rpm) surface speed; dry air test atmosphere (less than 100 ppm H2O); and use of a time stepwise procedure for measuring wear. Highly reproducible steady-state wear rates resulted from the two fluid studies which had a linearity of about 99 percent after initially higher wear rates and friction coefficients during run-in periods of 20 to 40 minutes.

Loomis, W. R.↗

Steady-state boundary lubrication with formulated C-ethers to 260 C

Steady state wear and friction studies were made at boundary lubrication conditions in a pin on disk (pure iron on rotating CVM M 50 steel) sliding friction apparatus with five C ether formulated fluids (modified polyphenyl ether containing phosphrous ester, organic acid, and other additives). Conditions included 20, 150, and 260 C disk temperatures, dry air test atmosphere, 1 kilogram load, 50 rpm disk speed, and test times to 130 minutes. Results were compared with those obtained with a formulated MIL L 27502 candidate ester and the C ether base fluid. Three of the C ether formulations gave better lubrication than both reference fluids under most conditions. The other two C ether formulations yielded higher wear rates and friction coefficients than the C ether base fluid for most of the temperature range. Only one C ether formulation showed consistently higher steady state wear rates than the ester.

Loomis, W. R.↗

Effect of oxygen concentration in ZDP containing oils on surface composition and wear

A pin-on-disk wear study was performed with the lubricants dibutyl sebacate (DBS) and mineral oil (MO) with and without 1 weight percent zinc-dialkyl-dithiophospatee (ZDP) as an additive. The pin was annealed pure iron and the disk was M-2 tool steel. The selected load and speed guaranteed boundary lubrication. The ambient atmospheric oxygen concentration in an oxygen-nitrogen mixture was varied from 0 percent to 20 percent in order to examine its relationship to ZDP effectiveness. Auger electron spectroscopy combined with argon ion bombardment (depth profiling) was used to determine surface elemental composition on the pin when tested in DBS with and without ZDP. The ambient atmosphere was found to cause large variations in wear rate and surface composition. With MO, ZDP reduced wear under all conditions, but had little advantage over oxides formed at 20 percent oxygen atmosphere. With DBS, ZDP reduced wear at 0 percent oxygen, but gave varied results at other oxygen concentrations. Depth profiling revealed sulfuide formation at 0 percent oxygen and probably sulfates at 20 percent oxygen. The results are significant because varied oxygen concentrations can occur under actual lubricating conditions in practical machinery.

Brainard, W. A.↗

An experimental investigation of the internal methane pressure in hydrogen attack

An experimental investigation of the internal methane pressure that is the driving force for bubble growth in hydrogen attack (HA) was done on pure iron (204 ppm C) and on two low carbon steels of slightly different compositions. The methane content N (c.c gas/g. material) in attacked specimens was measured by a vacuum extraction technique. The total void volume V (c.c) was determined from density measurements before and after HA exposure. The two values, N and V, were then used in an equation of state to calculate an average methane pressure P for the attack stages beyond a density loss (d.l.) greater than 0.05 pct. It was determined that N and P depend on hydrogen exposure conditions and the presence of traces of strong carbide forming alloying elements (in steel). They are independent of specimen size and grain size over a limited range. P varies as the bubble volume increases, showing a generally decreasing trend which brings it to values lower than calculated equilibrium pressures, although well within the same order of magnitude. Possible reasons for this behavior are discussed.

Natan, M.↗

Phase relationships in Fe-Ni alloys at high pressures and temperatures

Diffusionless phase transformations in Fe-Ni alloys with up to 35 wt pct Ni were studied using resistance-heated diamond anvil cells and synchrotron radiation. At temperatures up to 600 C and pressures up to 25 GPa, Fe-35 percent Ni showed only the face-centered cubic (fcc) phase while Fe-25 percent Ni and Fe-10 percent Ni showed the body-centered cubic (bcc) and hexagonal close-packed (hcp) phases in addition to the fcc phase. The phase relationships of these solid phases are topologically similar to those of pure iron. The triple point becomes lower in temperature, and the slope (dT/dP) of the fcc/hcp boundary decreased as Ni-content increases in the alloys. From these results it is inferred that Fe-Ni alloys in the earth's inner core might exist as two phases, fcc and hcp. The existence of these two phases could have played an important role in the separation of the inner and outer core.

Huang, Eugene↗

Perfluoropolyalkylether decomposition on catalytic aluminas

The decomposition of Fomblin Z25, a commercial perfluoropolyalkylether liquid lubricant, was studied using the Penn State Micro-oxidation Test, and a thermal gravimetric/differential scanning calorimetry unit. The micro-oxidation test was conducted using 440C stainless steel and pure iron metal catalyst specimens, whereas the thermal gravimetric/differential scanning calorimetry tests were conducted using catalytic alumina pellets. Analysis of the thermal data, high pressure liquid chromatography data, and x-ray photoelectron spectroscopy data support evidence that there are two different decomposition mechanisms for Fomblin Z25, and that reductive sites on the catalytic surfaces are responsible for the decomposition of Fomblin Z25.

Morales, Wilfredo↗

Gravitational Constraints on the Internal Structure of Ganymede

Before the arrival of the Galileo spacecraft in the jovian system, there was little information on the interior structure of jupiter's largest moon, Ganymede. Its mean density (1,940 kg/cu m), determined by the Pioneer and Voyager spacecraft, implies a composition that is roughly 60% rock and 40% ice, which could be uniformly mixed or differentiated into a rocky core and icy mantle. Here we report measurements by the Galileo spacecraft of Ganymede's overall density and the spherical harmonics, J(sub 2) and C(sub 22) of its gravitational field. These data show clearly that Ganymede has differentiated into a core and mantle. Combined with the recent discovery of an intrinsic magnetic field, our gravity results suggest that Ganymede has a metallic core of radius 400-1,300 km surrounded by a silicate mantle, which is in turn enclosed by an ice she approx.800 km thick. Depending on whether the core is pure iron or an alloy of iron and iron sulphide, it could account for as little as 1.4% or as much as one-third of the total mass. If the ice were stripped away, Ganymede could look much like lo' in terms of its size and internal mass distribution.

Anderson, J. D.↗

Analysis of Phase Separation in Czochralski Grown Single Crystal Ilmenite

Ilmenite (FeTiOs) is a wide bandgap semiconductor with an energy gap of 2.58 eV. Ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Single crystal ilmenite has been grown from the melt using the Czochralski method. Growth conditions have a profound effect on the microstructure of the samples. Here we present data from a variety of analytical techniques which indicate that some grown crystals exhibit distinct phase separation during growth. This phase separation is apparent for both post-growth annealed and unannealed samples. Under optical microscopy, there appear two distinct areas forming a matrix with an array of dots on order of 5 pm diameter. While appearing bright in the optical micrograph, atomic force microscope (AFM) shows the dots to be shallow pits on the surface. Magnetic force microscope (MFM) shows the dots to be magnetic. Phase identification via electron microprobe analysis (EMPA) indicates two major phases in the unannealed samples and four in the annealed samples, where the dots appear to be almost pure iron. This is consistent with micrographs taken with a scanning probe microscope used in the magnetic force mode. Samples that do not exhibit the phase separation have little or no discernible magnetic structure detectable by the MFM.

Wilkins, R.↗

Self-Organized Criticality and Phase Problem in Magnetoaocustic Emission Burst in Ferromagnets

Two types of ferromagnets, pure iron and steel with varying geometry and microstructural properties, were prepared for the present study of magnetoacoustic emission (MAE). The purpose was to separate the effects of structural property variations from changes caused by differences in the sample geometry. The position and shape of the leading MAE sub-burst and its variation among the samples are explained by magnetic anisotropy and the results of numerical simulations which utilized the concept of self-organized criticality (SOC). The amplitude and duration of the second sub-burst, which previously was thought to occur as a result of a complicated interaction between non-180 deg domain walls and lattice defects, can easily be explained by the results of our simulation.

Namkung, M.↗