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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Ultra-Low Viscosity and High Magnetic Susceptibility Magnetic Ionic Liquids Featuring Functionalized Diglycolic Acid Ester Rare-Earth and Transition Metal Chelates

Magnetic ionic liquids (MILs) comprise a subcategory of ionic liquids (ILs) and contain a paramagnetic metal center allowing them to be readily manipulated by an external magnetic field. While MILs are popularly employed as solvents in catalysis, separations, and organic synthesis, most low viscosity combinations possess a hydrophilic character that limits their use in aqueous matrices. To date, no study has reported the synthesis and characterization of hydrophobic MILs with viscosities similar to those of hydrophilic MILs and organic solvents while simultaneously exhibiting enhanced magnetic and thermal properties. In this study, diglycolic acid esters are employed as ligands to chelate with paramagnetic metals to produce cations that are paired with metal chelates composed of hexafluoroacetylacetonate ligands to form MILs incorporating multiple metal centers in the cation and anion. Viscosity values below 31.6 cP were obtained for these solvents, the lowest ever reported for hydrophobic MILs. Solubilities in nonpolar solvents such as benzene were observed to be as high as 50% (w/v) MIL-to-solvent ratio while being insoluble in water at concentrations as low as 0.01% (w/v). Effective paramagnetic moment values for these solvents ranged from 5.33 to 15.56 Bohr magnetons (μB), with mixed metal MILs containing multiple lanthanides in the anion generally offering higher magnetic susceptibilities. MILs composed of ligands containing octyl substituents were found to possess thermal stabilities up to 190 °C. The synthetic strategies explored in this study exploit the highly tunable nature of the employed cation and anion pairs to design versatile ultra-low viscosity magnetoactive solvents that possess tremendous potential and applicability in liquid–liquid separation systems, catalysis, and microfluidics where the mechanical movement of the solvent can be easily facilitated using electromagnets.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

The effect of magnetic susceptibility and magnetic field strength on porosity estimates determined from low-field nuclear magnetic resonance

The presence of materials with high magnetic susceptibility are known to have an impact on 1H nuclear magnetic resonance (NMR) measurements and in laboratory data this often results in poor estimates of porosity from NMR data. To quantify and understand the cause of the poor NMR porosity estimations, in this laboratory study, we examine the effect of magnetic susceptibility, NMR measurement parameters, and NMR instrument design on NMR measurements. Data were collected with two instruments, each with a different Larmor frequency (2 MHz and 485 kHz), on water-saturated unconsolidated sediments with magnetic susceptibility values ranging from 3.6 × 10 -6 to 7020 × 10 -6 SI. The results show that for materials with low magnetic susceptibility (<378 × 10 -6 SI), the gravimetric porosity is accurately predicted from the NMR measurements. For the samples with high magnetic susceptibility (>987 × 10 -6 SI) the gravimetric porosity is poorly predicted from the 2 MHz NMR measurements made at all echo times (from 0.2 to 3.0 ms). In contrast, the gravimetric porosity is more accurately predicted at an echo time of 0.2 ms for measurements made using the 485 kHz instrument, although at larger echo times (>1.0 ms), the porosity estimate becomes poor. The 485 kHz NMR instrument has non-zero internal magnetic field gradients, similar to those found in borehole instruments, in contrast to the 2 MHz NMR instrument, which has a homogeneous applied magnetic field. Finally, we conclude that differences is the magnetic field strength and higher magnetic field inhomogeneities in the 485 kHz NMR instrument contribute to a reduction of the impact of inhomogeneities in the magnetic field caused by materials with high magnetic susceptibility, allowing for improved porosity estimation. These results indicate that NMR measurements collected at short echo times in low, inhomogeneous static fields, e.g., borehole instruments, may provide accurate estimates of porosity in water saturated sediments, even in the presence of magnetic minerals.

58 GEOSCIENCES↗
DOE OSTI2020

Spin dynamics and relaxation in 7.6 nm thin film of La 0.7 Sr 0.3 MnO 3 /SrTiO 3 : ac magnetic susceptibility and magnetic viscosity investigations

Analysis of the results from our investigations of the temperature dependence of ac susceptibilities (χ' and χ'') and magnetic viscosity in a 7.6 nm thin film of La 0.7 Sr 0.3 MnO 3 grown on SrTiO 3 (001) substrate is presented. The Curie temperature (T C ) of this film is magnetic field (H) dependent, varying as [T C (H) - T C (0)] ~ H n with T C (0) = 270 K and n = 0.15. Temperature dependence of χ' and χ'' measured at ac frequencies f m in the range of 0.1–10 kHz shows a broad peak near 230 K associated with the blocking temperature (T B ) of spin clusters present in the 1.4 nm surface layer and a frequency dependent peak near 270 K associated with T C . The mean relaxation time τ determined from the Cole–Cole analysis of the temperature dependent χ' and χ'' is shown to fit the Vogel–Fulcher law: τ = τ 0 exp[ΔE/k B (T - T 0 )] with T 0 = 245 K, ΔE/k B = 270 K = T C and τ 0 = 1.2 x 10 -9 s. Magnetic viscosity S (measured in H = 0 for a sample cooled in H = 50 Oe) determined from the fit to the magnetization: M (t)= M (0) – S ln t, with time t up to 2 h, shows a peak at 230 K above which M (2 h) switches to negative values for temperatures up to T C (0). It is argued that this negative magnetization results from an interaction between the superparamagnetic spin clusters and the ferromagnetic phase, both being present in the temperature range of T B < T < T C .

36 MATERIALS SCIENCE↗
DOE OSTI2021

Evaluation of riverbed magnetic susceptibility for mapping biogeochemical hot spots in groundwater‐impacted rivers

Abstract Redox hot spots occurring as metal‐rich anoxic groundwater discharges through oxic wetland and river sediments commonly result in the formation of iron (Fe) oxide precipitates. These redox‐sensitive precipitates influence the release of nutrients and metals to surface water and can act as ‘contaminant sponges’ by absorbing toxic compounds. We explore the feasibility of a non‐invasive, high‐resolution magnetic susceptibility (MS) technique to efficiently map the spatial variations of magnetic Fe oxide precipitates in the shallow bed of three rivers impacted by anoxic groundwater discharge. Laboratory analyses on Mashpee River (MA, USA) sediments demonstrate the sensitivity of MS to sediment Fe concentrations. Field surveys in the Mashpee and Quashnet rivers (MA, USA) reveal several discrete high MS zones, which are associated with likely anoxic groundwater discharge as evaluated by riverbed temperature, vertical head gradient, and groundwater chemistry measurements. In the East River (CO, USA), widespread cobbles/rocks exhibit high background MS from geological ferrimagnetic minerals, thereby obscuring the relatively small enhancement of MS from groundwater induced Fe oxide precipitates. Our study suggests that, in settings with low geological sources of magnetic minerals such as lowland rivers and wetlands, MS may serve as a complementary tool to temperature methods for efficiently mapping Fe oxide accumulation zones due to anoxic groundwater discharges that may function as biogeochemical hot spots and water quality control points in gaining systems.

Wang, Chen↗
DOE OSTI2026

Evolution of magnetic bubble domains in the uniaxial ferromaget CeRu 2 Ga 2 B inferred from the Hall effect and ac magnetic susceptibility

We study the Hall effect, AC magnetic susceptibility (χ ac ), and magnetic force microscopy of the uniaxial ferromagnet CeRu 2 Ga 2 B with a centrosymmetric crystal structure. We observe a finite topological Hall effect (THE) within the ordered phase, before the magnetization is polarized by applied field. By comparing the field dependences of the area fraction of the magnetic bubbles, the derivative of χ ac , and the THE signal, we deduce that the magnetic bubbles in CeRu 2 Ga 2 B evolve from the trivial to topological spin texture with field. Our findings enable the expansion of the search for magnetic materials hosting topological spin textures to include uniaxial ferromagnets and open a new possibility to tailor the topological spin texture.

AC magnetic susceptibility↗
DOE OSTI2021

Low-temperature high-frequency dynamic magnetic susceptibility of classical spin-ice Dy 2 Ti 2 O 7

In this study, radio-frequency (14.6 MHz) AC magnetic susceptibility, , of Dy 2 Ti 2 O 7 was measured using self-oscillating tunnel-diode resonator. Measurements were made with the excitation AC field parallel to the superimposed DC magnetic field up to 5 T in a wide temperature range from 50 mK to 100 K. At 14.6 MHz, a known broad peak of from kHz—range audio-frequency measurements around 15 K for both [111] and [110] directions shifts to 45 K, continuing the Arrhenius activated behavior with the same activation energy barrier of E a ≈ 230 K. Magnetic field dependence of along [111] reproduces previously reported low-temperature two-in-two-out to three-in-one-out spin configuration transition at about 1 T, and an intermediate phase between 1 and 1.5 T. The boundaries of the intermediate phase show reasonable overlap with the literature data and connect at a critical endpoint of the first order transition line, suggesting that these features are frequency independent. An unusual upturn of the magnetic susceptibility at T → 0 was observed in magnetic fields between 1.5 T and 2 T for both magnetic field directions, before fully polarized configuration sets in above 2 T.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Linear magnetic susceptibility of anisotropic superconductors of cuboidal shape

In this study, a simplified model of anisotropic magnetic susceptibility in the Meissner–London vortex-free state of cuboidal superconducting samples is presented. Using this model, precision measurements of the magnetic response in three perpendicular directions of a magnetic field with respect to primary crystal axes can be used to extract the components of the London penetration depth, thus enabling the evaluation of the general superfluid density tensor, which is needed in the analysis of the superconducting gap structure.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Isolating Detrital and Diagenetic Signals in Magnetic Susceptibility Records From Methane‐Bearing Marine Sediments

Abstract Volume‐dependent magnetic susceptibility (κ) is commonly used for paleoenvironmental reconstructions in both terrestrial and marine sedimentary environments where it reflects a mixed signal between primary deposition and secondary diagenesis. In the marine environment, κ is strongly influenced by the abundance of ferrimagnetic minerals regulated by sediment transport processes. Post‐depositional alteration by H 2 S, however, can dissolve titanomagnetite, releasing reactive Fe that promotes pyritization and subsequently decreases κ. Here, we provide a new approach for isolating the detrital signal in κ and identifying intervals of diagenetic alteration of κ driven by organoclastic sulfate reduction (OSR) and the anaerobic oxidation of methane (AOM) in methane‐bearing marine sediments offshore India. Using the correlation of a heavy mineral proxy from X‐ray fluorescence data (Zr/Rb) and κ in unaltered sediments, we predict the primary detrital κ signal and identify intervals of decreased κ, which correspond to increased total sulfur content. Our approach is a rapid, high‐resolution method that can identify overprinted κ resulting from pyritization of titanomagnetite due to H 2 S production in marine sediments. In addition, total organic carbon, total sulfur, and authigenic carbonate δ 13 C measurements indicate that both OSR and AOM can drive the observed κ loss, but AOM drives the greatest decreases in κ. Overall, our approach can enhance paleoenvironmental reconstructions and provide insight into paleo‐positions of the sulfate‐methane transition zone, past enhancements of OSR or paleo‐methane seepage, and the role of detrital iron oxide minerals on the marine sediment sulfur sink, with consequences influencing the development of chemosynthetic biological communities at methane seeps.

58 GEOSCIENCES↗
DOE OSTI2021

Molecular-field-theory fits to magnetic susceptibilities of antiferromagnetic GdCu 2 Si 2 , CuO, LiCrO 2 , and α-CaCr 2 O 4 single crystals below their Néel temperatures

A recently-developed molecular field theory (MFT) has been used to fit single-crystal magnetic susceptibility χ versus temperature T data below the respective antiferromagnetic ordering temperature T N for a variety of collinear and coplanar noncollinear Heisenberg antiferromagnets. The spins in the system are assumed to interact by Heisenberg exchange and to be identical and crystallographically equivalent. The fitting parameters for χ(T ) of collinear antiferromagnets are measurable quantities: the Weiss temperature θ p in the Curie-Weiss law, TN, χ(T N ), and the spin S. For coplanar noncollinear helix and cycloid structures, an additional fitting parameter is the turn angle between layers of ferromagnetically-aligned spins. Here MFT fits to anisotropic χ(T) data from the literature for single crystals of the collinear antiferromagnets GdCu 2 Si 2 and CuO and the noncollinear antiferromagnets LiCrO 2 with a 120° cycloidal structure and α-CaCr 2 O 4 with a 120° helical structure below their respective N´eel temperatures are presented. The MFT fit to the anisotropic χ(T ≤ T N ) data for CuO is poor, whereas the fits to the data for GdCu 2 Si 2 , LiCrO 2 , and α-CaCr 2 O 4 are quite good. The poor fit for CuO is attributed to the influence of strong quantum fluctuations associated with the small Cu spin and the quasi-one-dimensional magnetism that are not taken into account by the MFT. The magnetic contribution to the zero-field heat capacity of the collinear antiferromagnet GdNiGe 3 at T ≤ T N is also fitted by the MFT.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Combining molecular beam epitaxy and low-energy electron microscopy with in situ magnetic susceptibility measurements within an integrated ultrahigh vacuum system

Quantum two-dimensional materials, including ultrathin superconducting films, are of great current research interest. These films are typically fabricated under ultra-high vacuum (UHV) conditions and are sensitive to the environment—prone to oxidation and contamination when exposed to the atmosphere. This hampers the study of their intrinsic properties by standard ex situ techniques. Here, we present a variable-temperature mutual inductance probe system integrated under UHV with molecular beam epitaxy (MBE) synthesis and low-energy electron microscopy, enabling nondestructive in situ characterization of superconducting thin films. The system employs a reflection-type configuration and reaches a low temperature (∼4 K) using a high-cooling-power, vibration-isolated cryocooler. In conclusion, we demonstrate the system performance by measuring the superconducting critical temperature in a copper-oxide thin film.

2D materials↗
DOE OSTI2021

Magnetic anisotropy and spin dynamics in the kagome magnet Fe 4 Si 2 Sn 7 O 16 : NMR and magnetic susceptibility study on oriented powder

Fe 4 Si 2 Sn 7 O 16 hosts an undistorted kagome lattice of Fe 2+ (3d 6 , S = 2) ions. We present results of bulk magnetization and Sn nuclear magnetic resonance (NMR) measurements on an oriented Fe 4 Si 2 Sn 7 O 16 powder sample oriented in geometries parallel (∥) and perpendicular (⊥) to the external applied magnetic field used for orienting the powder (Bori). The bulk susceptibility χ shows a broad peak at T N ~ 3 K associated with antiferromagnetic ordering. NMR spectra indicate the presence of planar anisotropy in the kagome planes. From an analysis of the static NMR shift (K) and dynamic spin-lattice relaxation rate (1/T 1 ) we conclude the presence of dominant magnetic fluctuations in the kagome planes. For the ∥ orientation, K scales linearly with the bulk susceptibility for temperatures down to ~ 4 K, while in the ⊥ orientation K starts to deviate strongly below T ~ 30 K. We associate this deviation with the onset of spin-tilting towards the kagome planes. These correlations are also reflected in the 1/T 1 data for the ∥ orientation, which starts to decrease below T ~ 30 K. Here, in this correlated regime, T N < T < ~ 30 K, we discuss the formation of positive chiral spin correlations in the kagome planes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Overcoming magnetic susceptibility broadening in NMR of coin cell batteries to achieve chemical resolution

We develop methods for previously introduced NMR hardware that enables sensitive, noninvasive spectroscopic study of coin cell batteries, by overcoming the magnetic field distortions intrinsic to the battery limited chemical resolution. Specifically, we employ an interferometric NMR technique to overcome field heterogeneity, reducing peak widths by two orders of magnitude and obtaining chemically resolved solution-state spectra.

25 ENERGY STORAGE↗
DOE OSTI2021

Reply to: “Extracting Kondo temperature of strongly-correlated systems from the inverse local magnetic susceptibility”

In his comment1, Katanin reanalyzes our LDA + DMFT results for the temperature-dependent static local spin susceptibility of Sr 2 RuO 4 and V 2 O 3 fitting them to a Curie–Weiss (CW) form, χ(T) ≃ a/(T + θ). Invoking Wilson’s analysis of the impurity susceptibility of the spin-½ one-channel Kondo model (1CKM) in the wide-band limit, he extracts spin Kondo temperatures using T K = θ/√2, obtaining T K = 350 K and 100 K for Sr 2 RuO 4 and V 2 O 3 , respectively. Noting that these are significantly smaller than the scales $T$$^{onset}_{sp}$ = 2300 K and 1000 K reported in ref. 2, he argues that our $T$$^{onset}_{sp}$ scales “do not characterize the screening process”.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗