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At least 505 records · Page 28
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Effect of Spin–Orbit Coupling on Phonon-Mediated Magnetic Relaxation in a Series of Zero-Valent Vanadium, Niobium, and Tantalum Isocyanide Complexes

Spin-vibronic coupling leads to spin relaxation in paramagnetic molecules, and an understanding of factors that contribute to this phenomenon is essential for designing next-generation spintronics technology, including single-molecule magnets and spin-based qubits, wherein long-lifetime magnetic ground states are desired. We report spectroscopic and magnetic characterization of the isoelectronic and isostructural series of homoleptic zerovalent transition metal triad M(CNDipp) 6 (M = V, Nb, Ta; CNDipp = 2,6-diisopropylphenyl isocyanide) and show experimentally the significant increase in spin relaxation rate upon going from V to Nb to Ta. Correlated electronic calculations and first principle spin–phonon computations support the role of spin–orbit coupling in modulating spin–phonon relaxation. Furthermore, our results provide experimental evidence that increasing magnetic anisotropy through spin–orbit coupling interactions leads to increased spin–vibronic relaxation, which is detrimental to long spin lifetime in paramagnetic molecules.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Light- and Chemical-Doping-Induced Magnetic Behavior of Eu Molecular Systems

Variable temperature electron paramagnetic resonance (VT-EPR) was used to investigate the role of the environment and oxidation states of several coordinated Eu compounds. We find that while Eu(III) chelating complexes are diamagnetic, simple chemical reduction results in the formation of paramagnetic species. In agreement with the distorted D 3h symmetry of Eu molecular complexes investigated in this study, the EPR spectrum of reduced complexes showed axially symmetric signals (g ⊥ = 2.001 and g ∥ = 1.994) that were successfully simulated with two Eu isotopes with nuclear spin 5/2 ( 151 Eu and 153 Eu with 48% and 52% natural abundance, respectively) and nuclear g-factors 151 Eu/ 153 Eu = 2.27. Illumination of water-soluble complex Eu(dipic) 3 at 4 K led to the ligand-to-metal charge transfer (LMCT) that resulted in the formation of Eu(II) in a rhombic environment (g x = 2.006, g y = 1.995, g z = 1.988). The existence of LMCT affects the luminescence of Eu(dipic) 3 , and pre-reduction of the complex to Eu(II)(dipic) 3 reversibly reduces red luminescence with the appearance of a weak CT blue luminescence. Furthermore, encapsulation of a large portion of the dipic ligand with Cucurbit[7]uril, a pumpkin-shaped macrocycle, inhibited ligand-to-metal charge transfer, preventing the formation of Eu(II) upon illumination.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

EPR of Photoexcited Triplet-State Acceptor Porphyrins

The photoexcited triplet states of porphyrin architectures are of significant interest in a wide range of fields including molecular wires, nonlinear optics, and molecular spintronics. Electron paramagnetic resonance (EPR) is a key spectroscopic tool in the characterization of these transient paramagnetic states singularly well suited to quantify spin delocalization. Previous work proposed a means of extracting the absolute signs of the zero-field splitting (ZFS) parameters, D and E, and triplet sublevel populations by transient continuous wave, hyperfine measurements, and magnetophotoselection. Here, we present challenges of this methodology for a series of mesoperfluoroalkyl-substituted zinc porphyrin monomers with orthorhombic symmetries, where interpretation of experimental data must proceed with caution and the validity of the assumptions used in the analysis must be scrutinized. The EPR data are discussed alongside quantum chemical calculations, employing both DFT and CASSCF methodologies. Despite some success of the latter in quantifying the magnitude of the ZFS interaction, the results clearly provide motivation to develop improved methods for ZFS calculations of highly delocalized organic triplet states.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Electronic Spin Relaxation and Clustering in High-Pressure High-Temperature Synthesized Microcrystalline Diamond Particles with Reduced Nitrogen Content

The negatively charged nitrogen-vacancy (NV – ) color center in diamonds is widely studied because of numerous applications of this unique quantum system in sensing and quantum information sciences. While substitutional nitrogen is required to form the NV – centers in diamond, it also yields other paramagnetic defects─primarily the neutrally charged substitutional nitrogen centers (P1)─that decrease NV – spin coherence, which in turn degrades performance in applications. Herein, we investigate high-pressure high-temperature synthesized diamond microparticles (ca. 140–185 μm) having lower─ranging from 3 to 38 ppm─than the typical nitrogen content of type 1b diamond ( ca. 100 ppm and higher) typically used for the production of fluorescent diamond particles with NV – centers. A suite of electron paramagnetic resonance, optically detected magnetic resonance, and nuclear magnetic resonance methods are used to characterize spin properties of P1 and NV – centers in the particles. Upon decreasing the nitrogen content from 29 to 3 ppm, the ensemble NV – T 2 relaxation time increased by about 3-fold as measured directly in the Hahn Echo experiment at magnetic field of 1.2 T. Analysis of electronic relaxation of P1 centers revealed the existence of at least two distinct populations of P1 centers, consisting of fast and slower relaxing spins and allowed for an estimation of local concentrations. Even with <10 ppm nitrogen contents, the analysis indicated a highly heterogeneous distribution of P1 centers, suggesting the possibility of P1 spin clustering even at low nitrogen concentrations. The combined data demonstrate that the particles prepared from HPHT diamond with a low nitrogen content offer improved spin properties that are beneficial for NV – sensing applications.

Carbon↗
DOE OSTI2022

Illuminating Ligand Field Contributions to Molecular Qubit Spin Relaxation via T 1 Anisotropy

Electron spin relaxation in paramagnetic transition metal complexes constitutes a key limitation on the growth of molecular quantum information science. However, there exist very few experimental observables for probing spin relaxation mechanisms, leading to a proliferation of inconsistent theoretical models. Here we demonstrate that spin relaxation anisotropy in pulsed electron paramagnetic resonance is a powerful spectroscopic probe for molecular spin dynamics across a library of highly coherent Cu(II) and V(IV) complexes. Here, neither the static spin Hamiltonian anisotropy nor contemporary computational models of spin relaxation are able to account for the experimental T 1 anisotropy. Through analysis of the spin-orbit coupled wavefunctions, we derive an analytical theory for the T 1 anisotropy that accurately reproduces the average experimental anisotropy of 2.5. Furthermore, compound-by-compound deviations from the average anisotropy provide a promising approach for observing specific ligand field and vibronic excited state coupling effects on spin relaxation. Finally, we present a simple density functional theory workflow for computationally predicting T 1 anisotropy. Analysis of spin relaxation anisotropy leads to deeper fundamental understanding of spin-phonon coupling and relaxation mechanisms, promising to complement temperature-dependent relaxation rates as a key metric for understanding molecular spin qubits.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Cationic Cobalt(II) Bisphosphine Hydroformylation Catalysis: In Situ Spectroscopic and Reaction Studies

[HCo(CO) x (bisphosphine)](BF 4 ), x = 1–3, is a highly active hydroformylation catalyst system, especially for internal branched alkenes. In situ infrared spectroscopy (IR), electron paramagnetic resonance (EPR), and nuclear magnetic resonance studies support the proposed catalyst formulation. IR studies reveal the formation of a dicationic Co(I) paramagnetic CO-bridged dimer, [Co 2 (μ-CO) 2 (CO)(bisphosphine) 2 ] 2+ , at lower temperatures formed from the reaction of two catalyst complexes via the elimination of H 2 . Here, DFT studies indicate a dimer structure with square-pyramidal and tetrahedral cobalt centers. This monomer–dimer equilibrium is analogous to that seen for HCo(CO) 4 , reacting to eliminate H 2 and form Co 2 (CO) 8 . EPR studies on the catalyst show a high-spin (S = 3/2) Co(II) complex. Reaction studies are presented that support the cationic Co(II) bisphosphine catalyst as the catalyst species present in this system and minimize the possible role of neutral Co(I) species, HCo(CO) 4 or HCo(CO) 3 (phosphine), as catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Large Hyperfine Coupling Arising from Pseudo- 2 S Ground States in a Series of Lutetium(II) Metallocene Complexes

The synthesis of molecules with strong coupling between electronic and nuclear spins represents an important challenge in molecular quantum information science. Here, we report the synthesis and characterization of the divalent lutetium metallocene complexes Lu(Cp Me 5 )(Cp iPr 5 ) (Cp Me 5 = pentamethylcyclopentadienyl; Cp iPr 5 = pentaisopropylcyclopentadienyl), Lu(Cp iPr 4 Et ) 2 (Cp iPr 4 Et = ethyltetraisopropylcyclopentadienyl), and Lu(Cp iPr 4 ) 2 (Cp iPr 4 = tetraisopropylcyclopentadienyl). The molecular structures of these complexes, as determined through singlecrystal X-ray diffraction, feature a common bent sandwich geometry, with average Cp–Lu–Cp angles ranging from 159.9° to 152.6°. Analysis of continuous-wave electron paramagnetic resonance (EPR) spectra for the complexes reveals nearly isotropic g tensors with only a slight deviation from that of a free electron. Moreover, an extremely large splitting of the eight-line spectra indicates the presence of strong hyperfine coupling, and simulations provide isotropic hyperfine coupling constants of A iso = 4.38, 4.30, and 4.17 GHz across the series, where the value of A iso is found to decrease as the Cp–Lu–Cp angle becomes more acute. Notably, these values are the largest yet observed for any lanthanide complex. Moreover, EPR and computational analysis show that the large values of A iso stem from large s-orbital character up to 41.2% in the corresponding singly occupied molecular orbitals. To our knowledge, this degree of s-character in a molecular orbital is the largest yet reported for an open-shell isolable complex. These results outline a general strategy toward the isolation of paramagnetic molecules with strong hyperfine coupling and highly isotropic doublet electronic ground states.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Atomic structure of light-induced efficiency-degrading defects in boron-doped Czochralski silicon solar cells

Boron-doped Czochralski (Cz) Si is the most commonly used semiconductor in the fabrication of solar cells. The minority carrier lifetime of boron-doped Cz Si decreases upon exposure to light due to B–O-related defects, which reduce the performance of ~10 9 solar modules worldwide. Using electron paramagnetic resonance (EPR), we have identified the spin-active paramagnetic signatures of this phenomenon and gained insights into its microscopic mechanism. We found a distinct defect signature, which diminished when the degraded sample was annealed. The second signature, a broad magnetic field spectrum, due to the unionized B acceptors, was present in the annealed state but vanished upon light exposure. These observations show that, on degradation, nearly all the ~10 16 cm –3 B atoms in Cz Si complexed with interstitial O atoms, whereas only ~10 12 cm –3 of these complexes created defects that were recombination-active. The formation rate of these recombination-active defects correlated with the decay of the minority carrier lifetime. Furthermore, the line shape parameters linked these defects to both B and O impurities in Cz Si.

14 SOLAR ENERGY↗
DOE OSTI2012

Macroscopic and microscopic defects and nonlinear optical properties of KH{sub 2}PO{sub 4} crystals with embedded TiO{sub 2} nanoparticles

Results from the successful growth of high quality KH{sub 2}PO{sub 4} (KDP) crystals with incorporated TiO{sub 2} anatase nanoparticles and the characterization of these crystals using several complementary methods are presented. The study allowed the nature and distribution of macroscopic and microscopic defects in the KDP:TiO{sub 2} crystals to be clarified. The relationship between these defects and the distribution of TiO{sub 2} nanoparticles, and the influence of incorporated nanoparticles on the nonlinear optical properties of composite crystals in comparison with pure crystals were also elucidated. Visual observations, transmission and scanning electron microscopy have shown that the anatase nanoparticles were captured mainly by the pyramidal growth sector and, to a considerably lesser extent, by the prismatic growth sector. Energy dispersive x-ray analysis was able to confirm that the growth layer stacks contain the TiO{sub 2} particles. Fourier transformation infrared spectra have clearly shown the presence of an absorption band at about 800 cm{sup -1} in both KDP:TiO{sub 2} and TiO{sub 2}, and the disappearance of the band, associated with hydroxyl OH{sup -} groups on the TiO{sub 2} surface in KDP:TiO{sub 2}. Significant variation in the imaginary and real parts of the cubic nonlinear optical susceptibilities and refractive index changes at continuous wave excitation were found in prism and pyramid parts of pure KDP and KDP:TiO{sub 2} samples. Deciphering complicated electron paramagnetic resonance spectra in KDP:TiO{sub 2} and comparison with published data permitted the identification of paramagnetic defects along with their associated g-factors and zero-field splitting parameters (in some cases for the first time). It was found that the dominant lines belong to four different centers Fe{sub A}{sup 3+}, Fe{sub B}{sup 3+}, Cr{sub R}{sup 3+}, and Cr{sub GB}{sup 3+}. From analysis of line intensities it was concluded that the concentration of intrinsic defects like potassium and hydrogen vacancies in KDP:TiO{sub 2} is comparatively small, that the concentration of non-controlled impurities in nominally pure KDP samples is several times larger than in KDP:TiO{sub 2}, and that the concentration of non-controlled impurities in the prismatic part of the KDP:TiO{sub 2} boule is approximately twice as large as in the pyramid part.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Magnetic nanoparticles formed in glasses co-doped with iron and larger radius elements

A new type of nanoparticle-containing glasses based on borate glasses co-doped with low contents of iron and larger radius elements, Dy, Tb, Gd, Ho, Er, Y, and Bi, is studied. Heat treatment of these glasses results in formation of magnetic nanoparticles, radically changing their physical properties. Transmission electron microscopy and synchrotron radiation-based techniques: x-ray diffraction, extended x-ray absorption fine structure, x-ray absorption near-edge structure, and small-angle x-ray scattering, show a broad distribution of nanoparticle sizes with characteristics depending on the treatment regime; a crystalline structure of these nanoparticles is detected in heat treated samples. Magnetic circular dichroism (MCD) studies of samples subjected to heat treatment as well as of maghemite, magnetite, and iron garnet allow to unambiguously assign the nanoparticle structure to maghemite, independently of co-dopant nature and of heat treatment regime used. Different features observed in the MCD spectra are related to different electron transitions in Fe{sup 3+} ions gathered in the nanoparticles. The static magnetization in heat treated samples has non-linear dependence on the magnetizing field with hysteresis. Zero-field cooled magnetization curves show that at higher temperatures the nanoparticles occur in superparamagnetic state with blocking temperatures above 100 K. Below ca. 20 K, a considerable contribution to both zero field-cooled and field-cooled magnetizations occurs from diluted paramagnetic ions. Variable-temperature electron magnetic resonance (EMR) studies unambiguously show that in as-prepared glasses paramagnetic ions are in diluted state and confirm the formation of magnetic nanoparticles already at earlier stages of heat treatment. Computer simulations of the EMR spectra corroborate the broad distribution of nanoparticle sizes found by 'direct' techniques as well as superparamagnetic nanoparticle behaviour demonstrated in the magnetization studies.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2013

Magnetic properties of proton irradiated BiFeO{sub 3}

The crystal structure and magnetic properties of BiFeO{sub 3} samples, proton-irradiated with 0, 10, and 20 pC/{mu}m{sup 2}, were investigated with x-ray diffraction (XRD), vibrating sample magnetometer, and Moessbauer spectroscopy measurements. From the Rietveld refinement analysis of the XRD patterns, the crystal structure of BiFeO{sub 3} is determined to be rhombohedral with the space group of R3c. We have observed the decrease in the lattice constant and oxygen occupancy with proton irradiation. The magnetization hysteresis (M-H) curves show the appearance of the weak ferromagnetic behavior in the proton irradiated BiFeO{sub 3} samples. The Moessbauer spectra of proton irradiated BiFeO{sub 3} samples at 295 K were analyzed with two-sextets (B{sub 1} and B{sub 2}) and doublet. From the isomer shift ({delta}) values, ionic states were determined to be Fe{sup 3+}. Compared to non-irradiated sample, having the antiferromagnetic area ratio (two-sextets) of 45.47, 54.53% the antiferromagnetic and paramagnetic area ratios (doublet) of 10 and 20 pC/{mu}m{sup 2} proton irradiated BiFeO{sub 3} samples are 41.36, 51.26, and 7.38% and 41.03, 50.90, and 8.07%, respectively. Our experimental observation suggests that the increase in the paramagnetic area ratio is due to the disappearance of superexchange interaction, resulted from the removal of the oxygen with proton irradiation. Also, the appearance of the weak ferromagnetic behavior is caused by the breaking of the antiferromagnetic coupling.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Magnetic properties of nanocrystalline KNbO{sub 3}

Newly synthesized undoped and iron-doped nanoscale powders of KNbO{sub 3} are investigated using magnetic resonance and static magnetization methods in order to determine how the crystal size and doping affect the structure of magnetic defects and material properties. Although the bulk crystals of KNbO{sub 3} are nonmagnetic, the undoped KNbO{sub 3} powder with average particle size of 80 nm exhibits magnetic properties. The ferromagnetic resonance signal and the magnetization curve registered on the powder are thoroughly analyzed. It is concluded that the appearance of the defect driven ferromagnetism in the undoped powder is due to the nano-size of the particles. This effect disappears in the iron-doped KNbO{sub 3} powder with particle sizes above 300 nm. In case of low doping (<1 mol. % Fe), a new electron paramagnetic resonance signal with g{sub eff} = 4.21 is found out in the KNbO{sub 3}:Fe powder. Such a signal has not been observed in the bulk crystals of KNbO{sub 3}:Fe. We suppose that this signal corresponds to individual paramagnetic Fe{sup 3+} ions having rhombic symmetry.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Long-range ferromagnetic order induced by a donor impurity band exchange in SnO{sub 2}:Er{sup 3+} nanoparticles

In this work, the structural and magnetic properties of Er-doped SnO{sub 2} (SnO{sub 2}:Er) nanoparticles are reported. The SnO{sub 2}:Er nanoparticles have been synthesized by a polymer precursor method with Er content from 1.0% to 10.0%. X-ray diffraction results indicate the formation of only the rutile-type structure in all samples. The estimated mean crystallite size shows a decrease from ∼10 to ∼4 nm when the Er content is increased from 1.0% to 10.0%. The particle size values have been corroborated by transmission electron microscopy technique. The thermal dependence of the magnetization is consistent with the 3+ oxidation state of erbium ions for all samples. A strong paramagnetic-like behavior coexisting with a ferromagnetic phase has been determined for samples with Er content below 5.0%. Above this concentration, only a paramagnetic behavior has been determined. Isothermal magnetization curves are consistent with the occurrence of long-range ferromagnetic order mediated by donor electrons forming bound magnetic polarons which overlap to produce a spin-split impurity band.

36 MATERIALS SCIENCE↗
DOE OSTI2013

ESR lineshape and {sup 1}H spin-lattice relaxation dispersion in propylene glycol solutions of nitroxide radicals – Joint analysis

Electron Spin Resonance (ESR) spectroscopy and Nuclear Magnetic Relaxation Dispersion (NMRD) experiments are reported for propylene glycol solutions of the nitroxide radical: 4-oxo-TEMPO-d{sub 16} containing {sup 15}N and {sup 14}N isotopes. The NMRD experiments refer to {sup 1}H spin-lattice relaxation measurements in a broad frequency range (10 kHz–20 MHz). A joint analysis of the ESR and NMRD data is performed. The ESR lineshapes give access to the nitrogen hyperfine tensor components and the rotational correlation time of the paramagnetic molecule. The NMRD data are interpreted in terms of the theory of paramagnetic relaxation enhancement in solutions of nitroxide radicals, recently presented by Kruk et al. [J. Chem. Phys. 138, 124506 (2013)]. The theory includes the effect of the electron spin relaxation on the {sup 1}H relaxation of the solvent. The {sup 1}H relaxation is caused by dipole-dipole interactions between the electron spin of the radical and the proton spins of the solvent molecules. These interactions are modulated by three dynamic processes: relative translational dynamics of the involved molecules, molecular rotation, and electron spin relaxation. The sensitivity to rotation originates from the non-central positions of the interacting spin in the molecules. The electronic relaxation is assumed to stem from the electron spin–nitrogen spin hyperfine coupling, modulated by rotation of the radical molecule. For the interpretation of the NMRD data, we use the nitrogen hyperfine coupling tensor obtained from ESR and fit the other relevant parameters. The consistency of the unified analysis of ESR and NMRD, evaluated by the agreement between the rotational correlation times obtained from ESR and NMRD, respectively, and the agreement of the translation diffusion coefficients with literature values obtained for pure propylene glycol, is demonstrated to be satisfactory.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

In situ X-ray powder diffraction study of Ho{sub 5}Ge{sub 4}

In Ho{sub 5}Ge{sub 4} the magnetostructural transition (MST) from high temperature paramagnetic Sm{sub 5}Ge{sub 4}-type (O-II type) orthorhombic structure to a new low temperature antiferromagnetic (AFM) monoclinic structure (Mβ-structure; the distortion occurs in the ac-plane) results in discontinuities of 400, 400, and 300 ppm along a, b, and c axes, respectively. During MST the unit cell volume exhibits discontinuity of 1000 ppm, and changes in both inter and intra slab bonds are less than 2%. In the AFM state the application of 35 kOe magnetic field leads to a partial reconstruction of the high temperature O-II structure, which is accompanied with a large magnetostriction. The strain energy associated with magnetostriction effects leads to an incomplete field driven MST in the magnetically ordered state.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Growth modes and epitaxy of FeAl thin films on a-cut sapphire prepared by pulsed laser and ion beam assisted deposition

FeAl films around equiatomic composition are grown on a-cut (112{sup ¯}0) sapphire substrates by ion beam assisted deposition (IBAD) and pulsed laser deposition (PLD) at ambient temperature. Subsequent successive annealing is used to establish chemical order and crystallographic orientation of the films with respect to the substrate. We find a strongly [110]-textured growth for both deposition techniques. Pole figures prove the successful preparation of high quality epitaxial films by PLD with a single in-plane orientation. IBAD-grown films, however, exhibit three in-plane orientations, all of them with broad angular distributions. The difference of the two growth modes is attributed to the existence of a metastable intermediate crystalline orientation as concluded from nonassisted sputter depositions at different substrate temperatures. The formation of the chemically ordered crystalline B2 phase is accompanied by the expected transition from ferromagnetic to paramagnetic behavior of the films. In accordance with the different thermally induced structural recovery, we find a step-like magnetic transition to paramagnetic behavior after annealing for 1 h at T{sub A} = 300 °C for IBAD deposition, while PLD-grown films show a gradual decrease of ferromagnetic signals with rising annealing temperatures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Calculation of metallic and insulating phases of V{sub 2}O{sub 3} by hybrid density functionals

The electronic structure of vanadium sesquioxide V{sub 2}O{sub 3} in its different phases has been calculated using the screened exchange hybrid density functional. The hybrid functional accurately reproduces the experimental electronic properties of all three phases, the paramagnetic metal (PM) phase, the anti-ferromagnetic insulating phase, and the Cr-doped paramagnetic insulating (PI) phase. We find that a fully relaxed supercell model of the Cr-doped PI phase based on the corundum structure has a monoclinic-like local strain around the substitutional Cr atoms. This is found to drive the PI-PM transition, consistent with a Peierls-Mott transition. The PI phase has a calculated band gap of 0.15 eV, in good agreement with experiment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗