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At least 19 records

Saturation magnetization of polycrystalline iron

The magnetic moment per gram, sigma (H sub I, T), where H sub I is the internal field and T is the temperature, was measured for a polycrystalline iron sphere with the vibrating-sample magnetometer. The instrument was calibrated by using a method utilizing the high permeability of an iron sphere. The spontaneous moment, sigma(0, T),was obtained from plots of sigma(H sub I, T) as a function of H sub I for temperatures from 4.2 K to room temperature. The value of the spontaneous moment, sigma(0, T), at 298.9 K was 217.5 + or -0.4 emu/g. The extrapolated moment, sigma(0, 0),at absolute zero from a plot of sigma(0, T) as a function of T to 3/2 power was 221.7 + or - 0.4 emu/g.

Behrendt, D. R.↗

Thermally generated magnonic spin currents in a polycrystalline gadolinium iron garnet thin film with perpendicular magnetic anisotropy

Rare-earth iron garnets (REIGs) are the benchmark systems for magnonics, including the longitudinal spin Seebeck effect (LSSE). While most research has focused on single-crystalline REIGs on complimentary garnet substrates, moving to more, cost-effective complementary metal-oxide semiconductor (CMOS)-compatible substrates is important to integrate REIG thin films with existing technology. In this regard, we grow a 130 nm-thick polycrystalline gadolinium iron garnet (GdIG) film on the Si/SiO2 substrate and investigate the temperature-dependent LSSE. Interestingly, the polycrystalline GdIG film exhibits perpendicular magnetic anisotropy (PMA) at room temperature which is induced by tensile in-plane (IP)-strain originating from the thermal-expansion mismatch between the GdIG film and the substrate during rapid thermal annealing. Further, a spin-reorientation transition from the out-of-plane IP direction below TS = 180 K is observed. Additionally, the film reveals a magnetic compensation temperature, TComp, of ≈240 K. The LSSE voltage not only demonstrates a sign-inversion around TComp, but also shows noticeable changes around TS. As compared to a single-crystalline GdIG film, the lower LSSE voltage for the polycrystalline GdIG is attributed to the higher effective magnetic anisotropy and enhanced magnon scattering at the grain boundaries. Our study not only paves the way for the cost-effective growth of CMOS-compatible REIG-based systems with PMA for magnonic memory and information processing applications, but also highlights the fact that the spincaloritronic and spin-insulatronic properties of the polycrystalline REIGs follow those of their single-crystalline counterparts with reduced spin-to-charge conversion efficiency through LSSE which can be tuned further by controlling the average gran size and interface engineering.

Physics↗

Oxidation in Ca/K-1144 iron-based superconductors polycrystalline compounds

Iron-based superconductors (IBSCs) are a class of material under investigation for the development of superconducting wires in the low-temperature-high magnetic fields power application. Among the various families of IBSCs, the 1144 CaKFe$_4$As$_4$ compound is a promising material able to achieve outstanding superconducting properties with a cheap and simple chemical composition. Oxidation, in these compounds, is considered an obstacle for high intergranular critical current density, J c,GB . A study devoted to the evaluation of oxidation phenomena and their effects on the superconducting properties is thus needed in order to fully understand the involved mechanisms. From the evaluation of polycrystalline samples obtained by a mechanochemically assisted synthesis route, a degradation of the critical temperature and critical currents has been observed concurrently with oxygen accumulation at grain boundaries in open porosities. However, the crystalline structure at an atomic level seems not affected, as well as intragranular superconducting properties assessed by means of calorimetric methods. These results suggest that loss of superconducting properties in Ca/K-1144 compounds following oxidation is significantly associated with the worsening of grain connectivity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A spall and diffraction study of nanosecond pressure release across the iron ε-α phase boundary

The extreme response of polycrystalline iron at high pressures and high strain rates is revealed by means of high-power laser pulses. The compression portion of the pulse coupled with x-ray diffraction identifies the expected body-centered cubic (α) to hexagonal close packed (ε) displacive transformation. Upon release, observation shows that the complete reverse transformation takes approximately 8 ns and that the structure returns to its initial microstructural configuration, in a reversible transformation path. This is in good agreement with molecular dynamics (MD) simulations which predict an inverse dependence between transformation time and strain rate. The grain size is reduced from μm to nm range during compression and begins increasing back to the original grain size on decompression. The kinetics of the transition is dictated by heterogenous nucleation as it follows the Johnson-Mehl-Avrami-Kolmogorov equation with the appropriate time exponent of ~1. This is confirmed by MD simulations which also identify profuse twinning and dislocation generation. Here, the tensile pulse generated upon reflection at the free surface is captured by time-resolved free surface velocity measurements from which a peak tensile stress of 7 GPa is obtained, in stark contrast with its quasi-static value of ~200 MPa. At these strain rates, the strength of grain interiors, which is determined by twinning and slip exceeds the strength of the boundaries, and failure initiates preferentially in the latter.

36 MATERIALS SCIENCE↗

Muon hyperfine fields in iron and its dilute alloys

The temperature dependence of the interstitial magnetic field, B, as determined by the rotation of the spin of the muon, has been measured for dilute polycrystalline iron alloys with Mo, Ti, and Nb additions over a temperature range of 240 to 633 K. In all cases the behaviors differ from one another and from the Fe(Al) alloys previously studied. B, which is negative with respect to the magnetization, is increased in magnitude by Al and Mo, and decreased greatly by Ti. The addition of Nb creates a two-phase alloy from which the role of heterogeneity and/or strain on B in iron can be assessed. If the temperature dependence of the hyperfine field extracted from B for Fe(Mo) alloys is interpreted on the model previously used to discuss the Fe(Al) data, then the muon must be attracted to the Mo atom while repelled by the Al atoms as the temperature decreases.

Stronach, C. E.↗

The adsorption and thermal decomposition of tricresylphosphate (TCP) on iron and gold

Because tricresyl-phosphate (TCP) is a common antiwear additive in lubricants, there is great interest in its interactions with metal substrates. The TCP was allowed to adsorb on polycrystalline iron and gold at room temperature. X-ray photoelectron spectroscopy (XPS) was used to analyze the adsorbed species. The substrate was then heated in steps to 330 C, and the changes in the adsorbate were analyzed after each step. On both substrates saturation adsorption occurred at about one monolayer, but the sticking coefficient was less on gold than on iron. Comparison of the XPS spectra of TCP on each substrate with the spectrum from condensed TCP indicated nondissociative adsorption on gold, possibly by dipole-induced dipole interaction. On iron, there was apparently additional interaction between the substrate and the tolyl groups on the TCP molecule. TCP began to desorb molecularly from gold as soon as the gold was heated above room temperature. The desorption was complete by 200 C. However, when the iron substrate was heated, TCP did not desorb but decomposed between 150 and 250 C.

Wheeler, D. R.↗

Dynamic fracture processes in hydrogen embrittled iron

Mechanistic understanding of hydrogen embrittlement is critical to the transport and storage of hydrogen as a sustainable fuel. Experimental observation of dynamic fracture processes in hydrogen environments has been challenging. Here, in-situ transmission X-ray microscopy is used to image polycrystalline iron foils that are concurrently strained and electrochemically charged with hydrogen. Using this technique, voids and microcracks down to ∼30 nm in size are identified at or near the crack tip and tracked as strain is increased. We observe both hydrogen-induced transgranular failure and hydrogen-induced intergranular failure with distinct fracture processes. We find that transgranular fracture occurs through the formation of sharp branched structures at the main crack tip that are reminiscent of slip band formation. This is followed by void growth and coalescence, and interaction with secondary cracks that lead to propagation of the main crack. Intergranular fracture is found to occur through void coalescence along grain boundaries, along with significant secondary cracking near the crack tip. The crack growth rate is greater for void-mediated intergranular failure than for slip-mediated transgranular failure. Additionally, the removal of hydrogen results in recovered ductility for a crack initially propagated under hydrogen charging.

36 MATERIALS SCIENCE↗

Studies of the kinetics and mechanisms of perfluoroether reactions on iron and oxidized iron surfaces

Polymeric perfluoroalkylethers are being considered for use as lubricants in high temperature applications, but have been observed to catalytically decompose in the presence of metals. X-ray photoelectron spectroscopy (XPS) and temperature programmed desorption (TPD) were used to explore the decomposition of three model fluorinated ethers on clean polycrystalline iron surfaces and iron surfaces chemically modified with oxygen. Low temperature adsorption of the model fluorinated ethers on the clean, oxygen modified and oxidized iron surfaces was molecular. Thermally activated defluorination of the three model compounds was observed on the clean iron surface at remarkably low temperatures, 155 K and below, with formation of iron fluoride. Preferential C-F bond scission occurred at the terminal fluoromethoxy, CF3O, of perfluoro-1-methoxy-2-ethoxy ethane and perfluoro-1-methoxy-2-ethoxy propane and at CF3/CF2O of perfluoro-1,3-diethoxy propane. The reactivity of the clean iron toward perfluoroalkylether decomposition when compared to other metals is due to the strength of the iron fluoride bond and the strong electron donating ability of the metallic iron. Chemisorption of an oxygen overlayer lowered the reactivity of the iron surface to the adsorption and decomposition of the three model fluorinated ethers by blocking active sites on the metal surface. Incomplete coverage of the iron surface with chemisorbed oxygen results in a reaction which resembles the defluorination reaction observed on the clean iron surface. Perfluoro-1-methoxy-2-ethoxy ethane reacts on the oxidized iron surface at 138 K, through a Lewis acid assisted cleavage of the carbon oxygen bond, with preferential attack at the terminal fluoromethoxy, CF3O. The oxidized iron surface did not passivate, but became more reactive with time. Perfluoro-1-methoxy-2-ethoxy propane and perfluoro-1,3-diethoxy propane desorbed prior to the observation of decomposition on the oxidized iron surface.

Napier, Mary E.↗

Surface chemistry and friction behavior of the silicon carbide (0001) surface at temperatures to 1500 deg C

X-ray photoelectron and Auger electron spectroscopy analyses and friction studies were conducted with a silicon carbide (0001) surface in contact with iron at various temperatures to 1200 or 1500 C in a vacuum of 10 to the minus 8th power Pa. The results indicate that there is a significant temperature influence on both the surface chemistry and friction properties of silicon carbide. The principal contaminant of adsorbed amorphous carbon on the silicon carbide surface in the as received state is removed by simply heating to 400 C. Above 400 C, graphite and carbide type carbine are the primary species on the silicon carbide surface, in addition to silicon. The coefficients of friction of polycrystalline iron sliding against a single crystal silicon carbide (0001) surface were high at temperatures to 800 C. Similar coefficients of friction were obtained at room temperature after the silicon carbide was preheated at various temperatures up 800 C. When the friction experiments were conducted above 800 C or when the specimens were preheated to above 800 C, the coefficients of friction were dramatically lower. At 800 C the silicon and carbide type carbon are at a maximum intensity in the XPS spectra. With increasing temperature above 800 C, the concentration of the graphite increases rapidly on the surface, whereas those of the carbide type carbon and silicon decrease rapidly.

Miyoshi, K.↗

Understanding Reaction Networks through Controlled Approach to Equilibrium Experiments Using Transient Methods

We report a combined experimental/theoretical approach to studying heterogeneous gas/solid catalytic processes using low-pressure pulse response experiments achieving a controlled approach to equilibrium that combined with quantum mechanics (QM)-based computational analysis provides information needed to reconstruct the role of the different surface reaction steps. We demonstrate this approach using model catalysts for ammonia synthesis/decomposition. Polycrystalline iron and cobalt are studied via low-pressure TAP (temporal analysis of products) pulse response, with the results interpreted through reaction free energies calculated using QM on Fe-BCC(110), Fe-BCC(111), and Co-FCC(111) facets. In TAP experiments, simultaneous pulsing of ammonia and deuterium creates a condition where the participation of reactants and products can be distinguished in both forward and reverse reaction steps. This establishes a balance between competitive reactions for D* surface species that is used to observe the influence of steps leading to nitrogen formation as the nitrogen product remains far from equilibrium. Here, the approach to equilibrium is further controlled by introducing delay timing between NH 3 and D 2 which allows time for surface reactions to evolve before being driven in the reverse direction from the gas phase. The resulting isotopic product distributions for NH 2 D, NHD 2 , and HD at different temperatures and delay times and NH 3 /D 2 pulsing order reveal the role of the N 2 formation barrier in controlling the surface concentration of NH x * species, as well as providing information on the surface lifetimes of key reaction intermediates. Conclusions derived for monometallic materials are used to interpret experimental results on a more complex and active CoFe bimetallic catalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Laser, vacuum and gas reaction chamber for operando measurements at NSLS-II's 28-ID-2

We present a laser reaction chamber that we have developed for in situ/operando X-ray diffraction measurements at the NSLS-II 28-ID-2 X-ray powder diffraction beamline. This chamber allows for rapid and dynamic sample heating under specialized gas environments, spanning ambient conditions down to vacuum pressures. We demonstrate the capabilities of this setup through two applications: laser-driven heating in polycrystalline iron oxide and in single-crystal WTe 2 . Our measurements reveal the ability to resolve chemical reaction kinetics over minutes with 1 s time resolution. This setup advances opportunities for in situ/operando X-ray diffraction studies of both bulk and single-crystal materials.

36 MATERIALS SCIENCE↗

Changes in surface chemistry of silicon carbide (0001) surface with temperature and their effect on friction

Friction studies were conducted with a silicon carbide (0001) surface contacting polycrystalline iron. The surface of silicon carbide was pretreated: (1) by bombarding it with argon ions for 30 minutes at a pressure of 1.3 pascals; (2) by heating it at 800 C for 3 hours in vacuum at a pressure of 10 to the minus eighth power pascal; or (3) by heating it at 1500 C for 3 hours in a vacuum of 10 to the minus eighth power pascal. Auger emission spectroscopy was used to determine the presence of silicon and carbon and the form of the carbon. The surfaces of silicon carbide bombarded with argon ions or preheated to 800 C revealed the main Si peak and a carbide type of C peak in the Auger spectra. The surfaces preheated to 1500 C revealed only a graphite type of C peak in the Auger spectra, and the Si peak had diminished to a barely perceptible amount. The surfaces of silicon carbide preheated to 800 C gave a 1.5 to 3 times higher coefficient of friction than did the surfaces of silicon carbide preheated to 1500 C. The coefficient of friction was lower in the 11(-2)0 direction than in the 10(-1)0 direction; that is, it was lower in the preferred crystallographic slip direction.

Miyoshi, K.↗

Polarized neutron measurements of the internal magnetization of a ferrimagnet across its compensation temperature

We present the first polarized neutron transmission image of a model Néel ferrimagnetic material, polycrystalline terbium iron garnet (Tb 3 Fe 5 O 12 , TbIG for short), as it is taken through its compensation temperature T comp where the macroscopic magnetization vanishes. Our polarized neutron imaging data and the additional supporting measurements using neutron spin echo spectroscopy and SQUID magnetometry are all consistent with a vanishing internal magnetization at T comp .

Ferrimagnetism↗

Shock induced magnetic effects in fine particle iron dispersions

Magnetic effects associated with shock induced transformation of fcc antiferromagnetic iron precipitates in polycrystalline copper disks at levels up to 5 GPa in weak magnetic fields (H not greater than 0.5 Oe) were investigated. The demagnetization and anisotropy associated with second order transition, the effects of plastic deformation in imparting magnetic anisotropy and magnetic hardening, and the influence of post shock thermal transients on magnetization associated with recovery, recrystallization and grain growth were studied. It was found that on the microsecond time scale of the shock induced first order transformation, the field sense is recorded in the transformed iron particles. For a given particle size the degree of transformation of fcc iron depends on the level of the shock. For a given shock level the resultant magnetic properties depend on the particle size distribution, with maximum effects noted in specimens with 400 to 600 A particles.

Wasilewski, P. J.↗

Iron-rich permanent magnet

The disclosure is directed to an iron-nitride material having a polycrystalline microstructure including a plurality of elongated crystallographic grains with grain boundaries, the iron-nitride material including at least one of an α″-Fe16N2 phase and a body-center-tetragonal (bct) phase comprising Fe and N. The disclosure is also directed a method producing an iron-nitride material. The method includes some combinations of preparing a raw material comprising iron, carrying out a microstructure build-up by annealing the prepared raw material at an elevated temperature and subsequently quenching the prepared raw material to produce a microstructure build-up material, annealing the microstructure build-up material, reducing the microstructure build-up material in a hydrogen environment, nitriding the reduced material to produce a nitrided material and subsequently quenching the nitrided material to a martensitic transformation temperature, stress annealing the nitrided material, and magnetic field annealing the stress-annealed material.

Wang, Jian-Ping↗