Stray Field Imaging Research Articles

Stray-Field Imaging of a Chiral Artificial Spin Ice during Magnetization Reversal

Artificial spin ices are a class of metamaterials consisting of magnetostatically coupled nanomagnets. Their interactions give rise to emergent behavior, which has the potential to be harnessed for the creation of functional materials. Consequently, the ability to map the stray field of such systems can be decisive for gaining an understanding of their properties. Here, we use a scanning nanometer-scale superconducting quantum interference device (SQUID) to image the magnetic stray field distribution of an artificial spin ice system exhibiting structural chirality as a function of applied magnetic fields at 4.2 K. The images reveal that the magnetostatic interaction gives rise to a measurable bending of the magnetization at the edges of the nanomagnets. Micromagnetic simulations predict that, owing to the structural chirality of the system, this edge bending is asymmetric in the presence of an external field and gives rise to a preferred direction for the reversal of the magnetization. This effect is not captured by models assuming a uniform magnetization. Our technique thus provides a promising means for understanding the collective response of artificial spin ices and their interactions.

Nanoscale magnetic field sensing and imaging based on nitrogen-vacancy center in diamond

Magnetic field measurement and imaging with nanometer resolution is a key tool in the study of magnetism. There have been several powerful techniques such as superconducting quantum interference device, hall sensor, electron microscopy, magnetic force microscopy and spin polarized scanning tunneling microscopy. However, they either have poor sensitivity or resolution, or need severe environment of cryogenic temperature or vacuum. The nitrogen-vacancy color center (NV center) in diamond, serving as a quantum magnetic sensor, has great advantages such as long decoherence time, atomic size, and ambient working conditions. The NV center consists of a substitutional nitrogen atom and an adjacent vacancy in diamond. Its electronic structure of ground state is a spin triplet. The spin state can be initialized to mS=0 state and read out by laser pulse, and coherently manipulated by microwave pulse. It is sensitive to the magnetic field by measuring the magnetic Zeeman splitting or quantum phase in quantum interferometer strategies. By using dynamical decoupling sequence to prolong the decoherence time, the sensitivities approach to nano tesla for a single NV center and pico tesla for the NV center ensemble, respectively. As a sensor with an atomic size, it reaches single-nuclear-spin sensitivity and sub-nanometer spatial resolution. Combining with scanning microscopy technology, it can accomplish high-sensitivity and high-resolution magnetic field imaging so that the stray field can be reconstructed quantitatively. The magnetic field is calculated from the two resonant frequencies by solving the Hamiltonian of NV center in order to obtain the value of stray field. Recently, this novel magnetic imaging technique has revealed the magnetization structures of many important objects in magnetism research. The polarity and chirality of magnetic vortex core are determined by imaging its stray field; laser induced domain wall hopping is observed quantitatively with a nanoscale resolution; non-linear antimagnetic order is imaged in real space by NV center. It was recently reported that magnetization of the magnetic skyrmion is imaged by NV center. The magnetization distribution is reconstructed from stray field imaging. With the topological number limited to one, the Nel type magnetization is uniquely determined. These results show that the magnetic imaging method has great advantages to resolve the emerging magnetic structure materials. The magnetic imaging technology based on the NV center will potentially become an important method to study magnetic materials under continuous development.

Nitrogen-vacancy-center imaging of bubble domains in a 6-Å film of cobalt with perpendicular magnetization

We employ a scanning nitrogen-vacancy-center microscope to perform stray field imaging of bubble magnetic domains in a perpendicularly magnetized Pt/Co/AlOx trilayer with 6 Å of Co. The stray field created by the domain walls is quantitatively mapped with few-nanometer spatial resolution, with a probe-sample distance of about 100 nm. As an example of application, we show that it should be possible to determine the Bloch or Néel nature of the domain walls, which is of crucial importance to the understanding of current-controlled domain wall motion.

Quantitative stray field imaging of a magnetic vortex core

Thin-film ferromagnetic disks present a vortex spin structure whose dynamics, added to the small size (~10 nm) of their core, earned them intensive study. Here we use a scanning nitrogen-vacancy (NV) center microscope to quantitatively map the stray magnetic field above a 1 micron-diameter disk of permalloy, unambiguously revealing the vortex core. Analysis of both probe-to-sample distance and tip motion effects through stroboscopic measurements, allows us to compare directly our quantitative images to micromagnetic simulations of an ideal structure. Slight perturbations with respect to the perfect vortex structure are clearly detected either due to an applied in-plane magnetic field or imperfections of the magnetic structures. This work demonstrates the potential of scanning NV microscopy to map tiny stray field variations from nanostructures, providing a nanoscale, non-perturbative detection of their magnetic texture.

Non-Destructive Monitoring of Charge-Discharge Cycles on Lithium Ion Batteries using 7Li Stray-Field Imaging

Magnetic resonance imaging provides a noninvasive method for in situ monitoring of electrochemical processes involved in charge/discharge cycling of batteries. Determining how the electrochemical processes become irreversible, ultimately resulting in degraded battery performance, will aid in developing new battery materials and designing better batteries. Here we introduce the use of an alternative in situ diagnostic tool to monitor the electrochemical processes. Utilizing a very large field-gradient in the fringe field of a magnet, stray-field-imaging (STRAFI) technique significantly improves the image resolution. These STRAFI images enable the real time monitoring of the electrodes at a micron level. It is demonstrated by two prototype half-cells, graphite∥Li and LiFePO4∥Li, that the high-resolution 7Li STRAFI profiles allow one to visualize in situ Li-ions transfer between the electrodes during charge/discharge cyclings as well as the formation and changes of irreversible microstructures of the Li components, and particularly reveal a non-uniform Li-ion distribution in the graphite.

Stray-field imaging of magnetic vortices with a single diamond spin

Despite decades of advances in magnetic imaging, obtaining direct, quantitative information with nanometre scale spatial resolution remains an outstanding challenge. Recently, a technique has emerged that employs a single nitrogen-vacancy defect in diamond as an atomic-size magnetometer, which promises significant advances. However, the effectiveness of the technique when applied to magnetic nanostructures remains to be demonstrated. Here we use a scanning nitrogen-vacancy magnetometer to image a magnetic vortex, which is one of the most iconic objects of nanomagnetism, owing to the small size (~10 nm) of the vortex core. We report three-dimensional, vectorial and quantitative measurements of the stray magnetic field emitted by a vortex in a ferromagnetic square dot, including the detection of the vortex core. We find excellent agreement with micromagnetic simulations, both for regular vortex structures and for higher-order magnetization states. These experiments establish scanning nitrogen-vacancy magnetometry as a practical and unique tool for fundamental studies in nanomagnetism.

Solid-state STRAFI NMR probe for material imaging of quadrupolar nuclei

Stray field imaging (STRAFI) has provided an alternative imaging method to study solid materials that are typically difficult to obtain using conventional MRI methods. For small volume samples, image resolution is a challenge since extremely strong gradients are required to examine narrow slices. Here we present a STRAFI probe for imaging materials with quadrupolar nuclei. Experiments were performed on a 19.6T magnet which has a fringe field gradient strength of 72T/m, nearly 50 times stronger than commercial microimagers. We demonstrate the ability to acquire 7Li 1D profiles of liquid and solid state lithium phantoms with clearly resolved features in the micrometer scale and as a practical example a Li ion battery electrode material is also examined.

An expansion of the field modulus suitable for the description of strong field gradients in axisymmetric magnetic fields: Application to single-sided magnet design, field mapping and STRAFI

Mapping (or plotting) the magnetic field has a critical importance for the achievement of the homogeneous magnetic field necessary to standard MR experiments. A powerful tool for this purpose is the Spherical Harmonic Expansion (SHE), which provides a simple way to describe the spatial variations of a field in free space. Well-controlled non-zero spatial variations of the field are critical to MRI. The resolution of the image is directly related to the strength of the gradient used to encode space. As a result, it is desirable to have strong variations of the field. In that case, the SHE cannot be used as is, because the field modulus variations are affected by the variations of all components of the field. In this paper, we propose a method based on the SHE to characterize such variations, theoretically and experimentally, in the limit of an axisymmetric magnetic field. Practical applications of this method are proposed through the examples of single-sided magnet design and characterization, along with Stray-Field Imaging (STRAFI).

Micrometer scale resolution of materials by stray-field Magnetic Resonance Imaging

As Magnetic Resonance Imaging devices are becoming more and more powerful, resolutions as small as 10 μm can now be obtained. But, this is only possible when systems with slow transverse relaxation rates, like living tissues, are investigated. In this case, the time available for gradients space-encoding is long, and high k values can be reached in the Fourier domain. However, numerous materials have fast relaxation rates, thus limiting the spatial resolution to a few hundreds of microns. The Stray Field Imaging technique has solved this problem by using a very high (typically 5000 G/cm) static gradient. Consequently, the trajectory in k space is accelerated and it is possible, in principle, to reach a micrometer resolution in a few hundreds of microseconds. Most of the time, however, only resolutions in the millimeter range can be achieved due to mispositioning of the sample within the static magnetic field. Here, we show that by finely mapping the magnetic field and precisely positioning the sample, it is possible with a standard spectrometer to reach a micrometer resolution even on very fast relaxing materials.

Two‐ and three‐dimensional multinuclear stray‐field imaging of rotating samples with magic‐angle spinning (STRAFI‐MAS): From bio to inorganic materials

To revisit and illustrate the potential of a simple and effective multidimensional stray-field imaging technique with magic-angle spinning, known as STRAFI-MAS. STRAFI-MAS images are acquired with a standard NMR magnet and a traditional magic-angle sample spinning (MAS) probe. The stray-field gradients are achieved by placing the MAS probe, along the z-direction, at a distance from the center of the magnet. No pulsed-field gradients are applied. The multidimensional spatial encoding is carried out by synchronizing the radiofrequency pulses with the sample MAS rotation. Two-dimensional (2D) and 3D multinuclear images of various phantoms, including a tibia bone and silicon carbide, are recorded. Images of inorganic solids containing quadrupolar nuclei, (23)Na and (27)Al, are also explored for the first time by STRAFI-MAS. We have demonstrated that STRAFI-MAS is a simple and user-friendly technique for multidimensional imaging without the need of imaging equipment. With the current advancements in NMR and MRI methodologies, STRAFI-MAS is expected to be further developed and improved. We anticipate that STRAFI-MAS can spark a wide spectrum of interest, from material to bio science, where can benefit from high-resolution images.

Contrast STRAFI–MAS imaging

We demonstrate the possibility of multidimensional contrast ( T 1-, T 2-weighted and triple-quantum filtered) magnetic resonance imaging using a simple and effective solid-state NMR technique, stray-field imaging with sample magic-angle spinning (STRAFI–MAS). This imaging technique can be easily implemented in today’s standard solid-state NMR laboratory, making it a potentially valuable imaging application to material science.

A Methodology for the Indirect Determination and Spatial Resolution of Shear Modulus of PDMS−Silica Elastomers

A methodology is described that allows for the spatial resolution of shear modulus in silica-filled PDMS elastomers via {sup 1}H relaxation measurements and stray-field imaging (STRAFI) techniques. Traditional Hahn echoes provide a simple, robust route to the extraction of a proton residual dipolar coupling constant (RDC), a direct measure of chain mobility and a parameter that can be corollated to numerous mechanical properties. Defining a dimensionless RDC eliminates any artifacts associated with low-field measurement and allows the RDC to become independent of field strength. A direct correlation between the NMR determined dimensionless RDC and results from dynamic mechanical analysis is presented, then employed via STRAFI to determine spatial variations in moduli associated with irradiated elastomeric materials. Reliable performance, despite poorly optimized STRAFI conditions, is demonstrated with an error of no more than 22% between the calculated shear modulus and the measured value via DMA.

Three-dimensional micromagnetic domain structure of MnAs films on GaAs(001): Experimental imaging and simulations

The micromagnetic domain structure of MnAs films on GaAs(001) has been systematically investigated by micromagnetic imaging and simulations. The magnetic force microscopy (MFM) contrast resulting from the stray field of the simulated three-dimensional domain patterns was calculated and found to be in excellent agreement with MFM experiments. By combining three-dimensional stray-field imaging by MFM with surface sensitive probing and micromagnetic simulations, we were able to derive a consistent picture of the micromagnetic structure of MnAs. For example, the origin of the comblike contrast observed through MFM was identified as a metastable domain configuration exhibiting a cross-tie wall.

Structural and spatially resolved studies on the hardening of a commercial resin-modified glass-ionomer cement

A commercial photopolymerizable resin-modified glass-ionomer (Fuji II LC) was studied using a variety of nuclear magnetic resonance (NMR) techniques. (1)H and (19)F stray-field imaging (STRAFI) enabled to follow the acid-base reaction kinetics in self-cured (SC) samples. Gelation and maturation processes with 25 min and 40 h average time constants, respectively, were distinguished. In self- & photo-cured (SPC) samples, two processes were also observed, which occurred with 2 s and 47 s average time constants. (1)H, (27)Al and (29)Si magic angle spinning (MAS) NMR, (13)C cross-polarization (CP)/MAS NMR and (27)Al multiple quanta (MQ)MAS NMR spectroscopy were used to obtain structural information on the glass and cements that were either SC or SPC. The presence of methacrylate groups was identified in the solid component. Unreacted hydroxyl ethylmethacrylate (HEMA) was detected in self-cured cement. (27)Al data showed that approximately 28% and 20% of Al is leached out from glass particles in SC and SPC samples, respectively. The upfield shift detected in (29)Si MAS NMR spectra of the cements is consistent with a decrease in the number of Al species in the second coordination sphere of the silicon structures. Scanning electron microscopy (SEM) showed existence of 3D shrinkage of the cement matrix in photo-cured cements.

Influence of Grain Size on the Setting of Portland Cement: A Stray-Field Magnetic Resonance Imaging Study

A number of failures of large concrete structures during construction have been reported in the last decades [1]. The overestimation of concrete strength at early ages was one of the reasons for the failures. Consequently, reliable information about early age properties of the material is essential to guarantee life-time performance of structures. Portland cement is a complex heterogeneous particulate material and a full knowledge of kinetics of the hydration reactions, for example, is still missing. Gel constitutes the major phase in the hardening cement paste and the corresponding structure and dynamics represent an important contribution to determine the concrete performance. X-ray diffraction, which is widely used for the study of crystalline cement components, does not give information about the gel, amorphous, phase. Conversely, 1H stray-field magnetic resonance imaging (STRAFI-MRI) technique has proved to be a powerful tool to follow the early hydration and hardening periods of Portland cement (type I) [2-4]. The setting of cement pastes depends on parameters like the initial water/cement ratio, R, or particle size of the powder (G) and the compressive strength can be used to characterize the behaviour of hardening concrete. Water availability at the particle surfaces, which is controlled by R and G, limits cement hydration. At low R, G effects are less important. In general, it is accepted that for R<0.42, unreacted solid remain, as all the free volume is filled with hydration products [5]. For example, hydration of Portland cement pastes as a function of R (0.24-0.48) was studied using by STRAFI-MRI and hydrogen maps, from different types of water (capillary, gel or chemically bound water), enabled a spatially-resolved kinetics to be obtained [4]. Using STRAFI-MRI was now evaluated the influence of G (<70 μm to < 90 μm) on the early stages of hydration and hardening of Portland cement. Portland cement uses extend well beyond construction. For example, a mineral trioxide aggregate is now being applied as a root-end filling material, which was shown to have a similar chemical constitution to that of Portland cement except for the addition of bismuth compounds, seemingly to make the materials radiopaque for dental use [6].

Combined optical and force microscopy of patterned magnetic films

Combined magneto-optic indicator film (MOIF) and magnetic force microscopy (MFM) is introduced as an advanced tool for the characterization of patterned ferromagnetic films. The MOIF technique combines quantitative stray field imaging of individual micron-sized magnetic elements with a large-area overview of the patterned film while MFM provides nanometer spatial resolution. In order to demonstrate the potential of this approach, lithographically patterned CoPt films with out-of-plane anisotropy were characterized. The large-scale MOIF images reveal variations of the magnetization state and the magnetization reversal among individual magnetic elements. Corresponding high-resolution MFM images relate these results to the micromagnetic configuration of the elements.

Magnetic resonance studies of cement based materials in inhomogeneous magnetic fields

Single-sided magnets give hope that Nuclear Magnetic Resonance (NMR) might in future be used for in situ characterisation of hydration and water transport in the surface layers of concrete slabs. Towards that end, a portable NMR-MOUSE (MObile Universal Surface Explorer) has been used to follow the hydration of gypsum based plaster, a Portland cement paste and concrete mortar. The results compare favourably to those obtained using a standard laboratory bench-top spectrometer. Further, stray field imaging (STRAFI) based methods have been used with embedded NMR detector coils to study water transport across a mortar/topping interface. The measured signal amplitudes are found to correlate with varying sample conditions.

Multi-dimensional magnetic resonance imaging in a stray magnetic field

Stray field imaging has been extensively utilized in the last 10 years to perform very high resolution imaging of samples in a single dimension using the massive field gradient present in the fringe of a superconducting magnet. By spinning the sample around the magic-angle, the stray field gradient is successively reoriented along three orthogonal directions in the sample reference frame, allowing the acquisition of a full three-dimensional Fourier image, thereby providing the possibility to perform multi-dimensional very high-resolution imaging with standard nuclear magnetic resonance spectroscopy equipment. Here, we show multi-dimensional images demonstrating the feasibility of this technique.

Stray-field imaging and multinuclear magnetic resonance spectroscopy studies on the setting of a commercial glass-ionomer cement.

A commercial glass-ionomer (Fuji II) was studied using different NMR techniques. 1H and 19F stray-field imaging (STRAFI) were used to monitor the curing kinetics of the cement and two processes were distinguished: the gelation and maturation phases. Characterization of the aluminium and silicon species present in the glass component and cement was performed by conventional 27Al and 29Si MAS and two-dimensional 27Al triple quantum MAS NMR (MQMAS) techniques. Quantification of the aluminium in the glass component and in the cement indicates the leaching of about 32% of the 4-coordinate aluminium, about 100% of the 5-coordinate aluminium and about 41% of the 6-coordinate aluminium, during the setting reaction. It is also shown that the 5-coordinate aluminium is only present in the surface layer created by the acid attack during the cement formation process. In the cement, silicon maintains species with four bridging oxygens after the leaching of tetrahedral (4-coordinate) aluminium. The silicon analysis correlates well with the aluminium determinations.

Spatially-resolvedmagnetic resonance study of the dissolution interface between soapsand water

The developing interfacial region between a soap bar and water has been studied using a suite of spatially resolved NMR techniques. Stray field imaging (STRAFI) allowed the dynamics of water ingress into a shop-bought, commercial soap to be followed. A simplistic analysis of the data shows the ingress to be a Fickian process (∝t1/2) in the first 4 h. The T2 contrast employed in the STRAFI method is not sufficient to resolve detail of the mesophase formation at the interface. However, double quantum filtered 2H spectroscopy at different positions in the interfacial region allowed water concentration (and mesophase distribution) to be mapped over the first 120 h of dissolution. A simple model shows good agreement with the water concentration data. In the isotropic soap solution above the interfacial region, J-cyclic cross polarization was used to selectively interrogate the CH2 1H of the soap alkyl chains and, in combination with a pulsed field gradient measurement of self-diffusion, suggests a micellar solution in which the hydrodynamic radius of the micelles is ~5nm.