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The growth of cobalt nanopatterns (NPs) using focused electron‐beam induced deposition (FEBID) for localised magnetic studies is presented. The initial FEBID products are shown to be polycrystalline and form hetero‐structured core‐shell NPs through surface oxidation. Off‐axis electron holography is performed to reconstruct their morphology, thickness profile and image their individual magnetic vortex domain states. In situ annealing to 400°C promoted migration of the Co‐overspray to grow the Co NPs and improved their crystallinity through coarsening, as well as induced diffusion of embedded carbon out of their surface. It is found that the change in their morphology and chemical instability under heating restricts their suitability for examining thermally induced magnetic variations.

The thermal demagnetization of pseudo‐single‐domain (PSD) magnetite (Fe3O4) particles, which govern the magnetic signal in many igneous rocks, is examined using off‐axis electron holography. Visualization of a vortex structure held by an individual Fe3O4 particle (~250 nm in diameter) during in situ heating is achieved through the construction and examination of magnetic‐induction maps. Stepwise demagnetization of the remanence‐induced Fe3O4 particle upon heating to above the Curie temperature, performed in a similar fashion to bulk thermal demagnetization measurements, revealed that its vortex state remains stable under heating close to its unblocking temperature and is recovered upon cooling with the same or reversed vorticity. Hence, the PSD Fe3O4 particle exhibits thermomagnetic behavior comparable to a single‐domain carrier, and thus, vortex states are considered reliable magnetic recorders for paleomagnetic investigations., Key Points Thermal demagnetization of nonideal magnetite particlesVisualized magnetization of vortex state with temperatureVortex structures are reliable paleomagnetic signal recorders

Equi-atomic FeRh is a very interesting material as it undergoes a magnetostructural transition from an antiferromagnetic (AF) to a ferromagnetic (FM) phase between 75–105 °C. Its ability to present phase co-existence separated by domain walls (DWs) above room temperature provides immense potential for exploitation of their DW motion in spintronic devices. To be able to effectively control the DWs associated with AF/FM coexistence in FeRh thin films we must fully understand the magnetostructural transition and thermomagnetic behaviour of DWs at a localised scale. Here we present a transmission electron microscopy investigation of the transition in planar FeRh thin-film samples by combining differential phase contrast (DPC) magnetic imaging with in situ heating. We perform quantitative measurements from individual DWs as a function of temperature, showing that FeRh on NiAl exhibits thermomagnetic behaviour consistent with the transition from AF to FM. DPC imaging of an FeRh sample with HF-etched substrate reveals a state of AF/FM co-existence and shows the transition from AF to FM regions proceeds via nucleation of small vortex structures, which then grow by combining with newly nucleated vortex states into larger complex magnetic domains, until it is in a fully-FM state.

The preparation of a planar FeRh thin film using a focused ion beam (FIB) secondary electron microscope (SEM) for the purpose of in situ transmission electron microscopy (TEM) is presented. A custom SEM stub with 45° faces allows for the transfer and milling of the sample on a TEM heating chip, whilst Fresnel imaging within the TEM revealed the presence of the magnetic domain walls, confirming the quality of the FIB-prepared sample.

Supplementary material

The study of the paleomagnetic signal recorded by rocks allows scientists to understand Earth’s past magnetic field and the formation of the geodynamo. The magnetic recording fidelity of this signal is dependent on the magnetic domain state it adopts. The most prevalent example found in nature is the pseudo–single-domain (PSD) structure, yet its recording fidelity is poorly understood. Here, the thermoremanent behavior of PSD magnetite (Fe3O4) particles, which dominate the magnetic signatures of many rock lithologies, is investigated using electron holography. This study provides spatially resolved magnetic information from individual Fe3O4 grains as a function of temperature, which has been previously inaccessible. A small exemplar Fe3O4 grain (~150 nm) exhibits dynamic movement of its magnetic vortex structure above 400°C, recovering its original state upon cooling, whereas a larger exemplar Fe3O4 grain (~250 nm) is shown to retain its vortex state on heating to 550°C, close to the Curie temperature of 580°C. Hence, we demonstrate that Fe3O4 grains containing vortex structures are indeed reliable recorders of paleodirectional and paleointensity information, and the presence of PSD magnetic signals does not preclude the successful recovery of paleomagnetic signals.

The thermal demagnetization of pseudo-single-domain (PSD) magnetite (Fe3O4) particles, which govern the magnetic signal in many igneous rocks, is examined using off-axis electron holography. Visualization of a vortex structure held by an individual Fe3O4 particle (~250nm in diameter) during in situ heating is achieved through the construction and examination of magnetic-induction maps. Stepwise demagnetization of the remanence-induced Fe3O4 particle upon heating to above the Curie temperature, performed in a similar fashion to bulk thermal demagnetization measurements, revealed that its vortex state remains stable under heating close to its unblocking temperature and is recovered upon cooling with the same or reversed vorticity. Hence, the PSD Fe3O4 particle exhibits thermomagnetic behavior comparable to a single-domain carrier, and thus, vortex states are considered reliable magnetic recorders for paleomagnetic investigations.

Magnetite (Fe3O4) is an important magnetic mineral to Earth scientists, as it carries the dominant magnetic signature in rocks, and the understanding of its magnetic recording fidelity provides a critical tool in the field of palaeomagnetism. However, reliable interpretation of the recording fidelity of Fe3O4 particles is greatly diminished over time by progressive oxidation to less magnetic iron oxides, such as maghemite (g-Fe2O3), with consequent alteration of remanent magnetization potentially having important geological significance. Here we use the complementary techniques of environmental transmission electron microscopy and off-axis electron holography to induce and visualize the effects of oxidation on the magnetization of individual nanoscale Fe3O4 particles as they transform towards g-Fe2O3. Magnetic induction maps demonstrate a change in both strength and direction of remanent magnetization within Fe3O4 particles in the size range dominant in rocks, confirming that oxidation can modify the original stored magnetic information.

A suite of near-identical magnetite nanodot samples produced by electron-beam lithography have been used to test the thermomagnetic recording fidelity of particles in the 74–333 nm size range; the grain size range most commonly found in rocks. In addition to controlled grain size, the samples had identical particle spacings, meaning that intergrain magnetostatic interactions could be controlled. Their magnetic hysteresis parameters were indicative of particles thought not to be ideal magnetic recorders; however, the samples were found to be excellent thermomagnetic recorders of the magnetic field direction. They were also found to be relatively good recorders of the field intensity in a standard paleointensity experiment. The samples' intensities were all within ∼15% of the expected answer and the mean of the samples within 3% of the actual field. These nonideal magnetic systems have been shown to be reliable records of the geomagnetic field in terms of both direction and intensity even though their magnetic hysteresis characteristics indicate less than ideal magnetic grains. Key Points Nonideal magnetic systems accurately record field direction Weak-field remanences more stable than strong-field remanences

The thermomagnetic behavior of remanence-induced magnetite (Fe3O4) particles in the pseudo-single-domain (PSD) size range (similar to 0.1-10 mu m), which dominate the magnetic signature of many rock lithologies, is investigated using off-axis electron holography. Construction of magnetic induction maps allowed for the visualization of the vortex domain state in an individual Fe3O4 grain (similar to 200nm in diameter) as a function of temperature. Acquisition of a series of electron holograms at 100 degrees C intervals during in situ heating up to 700 degrees C demonstrates the vortex state of the Fe3O4 grain, in this instance, remains thermally stable close to its unblocking temperature and exhibits a similar in-plane remanent state upon cooling; i.e., the particle is effectively behaving like a uniaxial single-domain particle to temperatures near T-C. Such particles are thought to be robust magnetic recorders. It is suggested that evidence for PSD behavior should therefore not preclude paleomagnetic investigation.