Near-Field Scanning Microwave Microscope at 30mK
Scanning techniques such as atomic force microscopy (AFM) or scanning tunnelling microscopy (STM) offer a wide range of material investigation possibilities. Depending on the environmental conditions and the required scanning resolution scanning probe microscopes are hard to design and setup and not seldom homemade devices, adapted to their special proposes and requirements. A new low temperature near-field scanning microwave microscope working at 30 mK, designed to meet emerging needs of the quantum technologies sector, was now developed by the group of Sebastian de Graaf at NPL (National Physical Laboratory, Teddington, UK) in collaboration with the group of Prof. Sergey Kubatkin (Chalmers University of Technology, SE). It combines microwave characterization up to 6 GHz with STM or AFM techniques. The environment of a dilution cryostat makes special demands on the stability and stiffness of the used components. The group used a set of ANPx100 and ANPz100 nanopositioners (former versions of the ANP101 positioners) to align the sample with the tip in x, y, and z direction and a small ANPz51 positioner for the RF waveguide positioning. First verifications of the instrument showed the capability to image dielectric contrast down to the single microwave photon regime.
S. Geaney et al; Scientific Report 9, 12539 (2019)
Isolating Hydrogen Gas inside H-BN Bubbles
Storing small amounts of gas even in the atomic scale is extremely interesting for a lot of research fields. An important role plays the choose of the barrier material: It has to form bubbles to surround the stored gas, it has to be stable under extreme conditions, and it shall not interfere with the enclosed gas on chemical or physical terms. New results were now published by the group of Haomin Wang at the Chinese Academy of Sciences (Shanghai, CN) presenting the production of isolated hydrogen inside hexagonal boron nitride (h-BN) bubbles via plasma treatment.
Low temperature atomic force measurements were carried out to prove that the surrounded gas is indeed hydrogen. Therefore, the authors used a cryogenic atomic force microscope, the attoAFM I, cooled by the closed cycle cryostat attoDRY1100, the 4 K version of the attoDRY2100. Setting exactly the measurement temperature and performing temperature sweeps gave the researches the possibility to show the bubble’s disappearance at a temperature of 33.2 K ± 3.9 K indicating a transition or disappearing of the enclosed gas. As this temperature is close to condensing temperature of H2 (33.18 K), the results point to the presence of atomic hydrogen inside the h-BN bubbles. The successful production of hydrogen inside the bubbles and presented results are a next step for hydrogen storage.
Li He, et al; Nature Communications 10, 2815 (2019)
In-situ electrical biasing technique in MoS2
Due to their strong spin-orbit coupling and resulting large spin-orbit splitting in the valence band, layered transition metal dichalcogenides (TMD) are promising materials among the family of 2D materials for spintronic applications. The groups of Nathaniel Stern and Vinayak Dravid at Northwestern University (Evanston, Illinois, USA) used a film of monolayer MoS2 to present a new in-situ electrical biasing technique with transmission electron microscopy. They found that with an applied electric field a net vacancy flux towards the grain boundaries occurs. This vacancy flow results in a regions of Mo-rich nanoparticles aggregating near the voids (see figure c) which appear at strained regions around the grain boundaries (blue colored in figure (b)). The vacancy flow process saturates after several initial biasing cycles when the material reaches a stable state. To characterize these samples, they used the closed cycle cryostat attoDRY2100 combined with the attoCFM I and optical head to study structural dynamics by Raman spectroscopy.
A.A. Murthy et al., ACS Nano 14, 2, 1569-1576 (2020)
Charge Carrier Mobility in Perovskite thin films
One of today’s main challenges is a pollution-free resource of energy which allows us to limit global climate change. A promising way is the use of solar energy with the optimal photo absorber material. In a joint project, the groups of Achim Hartschuh at the Ludwig Maximilians University (Munich, D) and Pablo Docampo at Newcastle University (Newcastle upon Tyne, UK) presented an optical study about charge carrier transport in a thin film of methylammonium lead iodide - a material which is prototypical for the new class of hybrid perovskites, reaching a solar cell efficiency of more than 22%. Temperature-dependent photoluminescence measurements were performed with the table-integrated closed-cycle cryostat attoDRY800 which allowed for flexible integration of the microscope setup and reliable low-temperature operation.
Photoluminescence measurements indicated a steady decrease of the charge carrier diffusion constant with increasing temperature, see figure. Depending on the structure of the material - tetragonal or orthorhombic crystal phase - the mobility follows a power law dependence as Tm with m = -1.8 +/- 0.1 (tetragonal) or m = -1.2 +/- 0.1 (orthorhombic). The dynamics of the excited charge carriers is in agreement with theoretical models based on a temperature-dependent diffusion constant and several decay channels. Their study opens up the possibility to investigate other material compositions in the same way in the future.
Single Spin Magnetometry at the Nansocale
Since the discovery of ferromagnetism in 2D van der Waals crystals, the community aims to study the feature quantitatively at the nanoscale. This feat was now approached by the group of Patrick Maletinsky at the University of Basel (Basel, CH).
Using their single-spin magnetometer based on electronic spins in diamond with the attoAFM/CFM, they detected the magnetization distribution of atomically thin crystals of CrI3. attocube's attoAFM/CFM offers the possibility to combine atomic force with confocal microscopy for optically detected magnetic resonance. With their technique they found the magnetization of one monolayer to be ≈ 16 µB/nm2 and addressed an open question regarding the thickness-dependence of magnetisation in CrI3.
Next to the outstanding physical result it is the technique that will add new ways of detecting and manipulating of magnetic properties at the nanoscale. According to P. Maletinsky the "single-spin magnetometry" is a "close-to ideal tool to study the physics of atomically thin 2D magnets."
This measurement was realized with the attoAFM/CFM.
Uncompensated Bound Charges at Improper Ferroelectric Domain Walls
The research focus of an international team led by researchers from NTNU Trondheim, ETH Zurich, and Institut Néel, CNRS, lies on domain walls in improper ferroelectrics, a promising type of functional interface for nanoscale electronics. The team demonstrated the stability of improper ferroelectric domain walls in hexagonal manganites against electrically uncompensated bound charges.
Using the attoAFM I, the authors investigated the electronic domain-wall transport, carrier distribution, and electrostatics at temperatures down to 4.2 K. attocube's atomic force microscope, the attoAFM I, enables atomic force microscopy at cryogenic temperatures, down to mK. The findings provide new insight into the fundamental domain-wall properties, bringing us yet another step closer towards next-generation's durable and ultra-small electronic components.
Peggy Schoenherr, et al.; Nano Lett.19, 3, 1659-1664 (2019)
Fine-scale Stripey Morphology of an Iron Pnictide - New Findings in Material Science
Iron-based superconducting pnictides feature relatively high transition temperature and a co-existence of the superconducting state with antiferromagnetic ordering. This remarkable combination brings these materials into the focus of research. The group of Prof. Susannah Speller at the Materials Department of the University of Oxford (Oxford, UK) used an attoAFM I cooled by a closed cycle attoDRY1000 for magnetic force measurements at about 4.6 K to investigate the local electronic structure and chemistry of RbxFe2-ySe2 crystals.
The group showed a fine-scale stripey morphology of the superconducting phase which - combined with previous findings - paves the way to understand the intriguing electronic and magnetic properties of these compounds.
P Dudin et al.; Supercond. Sci. Technol. 32, 044005 (2019)
A nanoscale quantum sensor at high pressures
Pressure affects phenomena ranging from the properties of planetary interiors to transitions between quantum mechanical phases. However, the enormous stress gradients generated in high pressure experimental apparatuses, such as the diamond anvil cell, limit the utility of most conventional spectroscopy techniques. To address this challenge, a novel nanoscale sensing platform was independently developed by three groups (given in alphabetic order): the Jean-Francois Roch group (Université Paris-Sud, FR), the Sen Yang group (Chinese University of Hong Kong, CN), and the Norman Yao group (University of California, Berkeley, USA). The researchers used quantum spin defects integrated into an anvil cell to detect minuscule signals under extreme pressures and temperatures with diffraction-limited spatial resolution.
For this purpose, Norman Yao and colleagues utilized the table-integrated closed cycle attoDRY800 cryostat - the ideal platform for precise and rapid temperature control of a diamond anvil cell while offering a large sample chamber and free-beam optical access. The convenience of the closed-cycle cryostat allowed the researchers to publish their results to arXiv just nine months after installation.
Rotating transport measurement setup at 25mK
When designing a setup for mK applications material choice and thermalization is crucial. Titanium becomes superconducting at temperatures below 400 mK consequently, the thermal contact to the sample is not ensure anymore. At Peking University (Beijing, China), Dr. Pengjie Wang from Xi Lin group has chosen the beryllium-copper version of the ANR101 positioner with resistive readout to realize their low-electron-temperature sample rotation system for transport measurements inside a dilution cryostat. The rotator allows to orient the sample in-situ with respect to a high magnetic field of up to 10 T.
The dilution cryostat with a diameter of 81 mm offers the required space for the rotator setup, see picture. The sample holder is designed for the use of up to four sample, each 5 mm x 5 mm large, a red LED is installed to illuminate the samples at 4 K for an easier orientation. The measured electron temperature in the setup is 25 mK, the same as the environmental temperature.The setup is designed for transport measurements and material characterization at ultra-low electron temperatures. A first application shows the tilt-induced localization and delocalization of the second landing level of the two-dimensional electron gas - an experiment for which a pressurized liquid ³He cell had been necessary elsewise.
(Figure reproduced from Rev. Sci. Instrum. 90, 023905 (2019); doi: 10.1063/1.5083994, with the permission of AIP Publishing)
This measurement was realized with the ANR101/RES/LT - rotator (360° endless).
Cryogenic Infrared Nanoscopy of Conducting Oxide Interfaces
Scattering scanning near-field optical microscopy (s-SNOM) analyses complex optical and electrical properties of a sample on the nanoscale by scanning it with an illuminated sharp tip and detecting the backscattered light. neaspec and attocube improved this technique to enter the cryogenic regime, which offers completely new ways to study material properties and exploit new phase regimes.
In a first project the group of Alexey Kuzmenko from the University of Geneva (Geneva, CH) used the cryogenic s-SNOM system - the cryo-neaSNOM - to study the nearfield response of LaAlO3/SrTiO3 heterostructures in the range of wavelengths from 9.3 to 10.7 μm from room temperature to 6 K.
Using an AFM-writing technique, the team managed to image conducting wires written in an insulating interface with a conducting AFM, see figure 1. With the near-field optical measurements they showed a signal dependence on the transport properties of the electron system which is present in the interface (figure 2). A theoretical model based on the plasmon-phonon coupling as a central player explains the measured results quantitatively and predicts the correct frequency, temperature and gate-voltage dependence of the near-field amplitude and the phase. This result clearly shows the ability of s-SNOM to analyze buried conducting layers - an important feature for the future oxide electronics.
This measurement was realized with the cryo-neaSNOM.
Weiwie Luo, et al; Nature Communications 10, 2774 (2019)
Angle-dependent characterizations of materials at mK temperatures
Attocube's rotators offer a way to use the full magnetic field of a 1D magnet for field-angle dependent transport measurements at the sample. This benefit is used by the group of Anne de Visser at the Van der Waals - Zeeman Institute (University of Amsterdam, NL) in two setups with an ANR51 and an ANRv220 both in a closed loop configuration.
Magnetotransport measurements as a function of the angle θ in the trigonal basal plane of the topological superconductor SrxBi2Se3 revealed a large two-fold anisotropy of the upper critical field Bc2. Such a rotational symmetry breaking of Bc2(θ) cannot be explained with standard models, and indicates unconventional superconductivity with an exotic order parameter. More about this work can be found at .
In the second setup a home-built compact dilatometer was mounted on the ANRv220 in a dilution refrigerator. This was used to measure the anisotropy in the ferromagnetic and superconducting phase diagram of a single crystal of UCoGe by applying magnetic fields up to 14 T along the different crystallographic axes .
MFM for Optimization of Sintered Magnets
MFM image of a NdFeB sintered magnet with the nominal c-axis orientation perpendicular to the surface. The sample is in the remanent state but some surface grains show already magnetization reversal. High resolution imaging allows deeper insights into the magnetic reversal mechanism and the optimization of magnetic properties. Image size is 30x30µm2.
(Image courtesy of T. Helbig and O. Gutfleisch, Functional Materials Group, TU Darmstadt, Germany and Fraunhofer IWKS Hanau, Germany.)
Vortex Barriers in Iron Pnictides
Iron-pnictide high-temperature superconductors are widely studied, but many open questions still remain. Using an attoAFM I for magnetic force microscopy, the group of O. Auslaender has studied twin boundaries and their interaction with vortices over a range of magnetic fields and temperatures. They find that stripes parallel to the twin boundaries repel vortices, effectively hindering vortex motion, and hence potentially affecting the critical current in such materials.
(Data courtesy of O. Auslaender, Technion, Israel)
A. Yagil et al., Phys. Rev. B 94, 064510 (2016)
Low Temperature MFM on Artifical Spin Ice
Frustrated systems are intriguing for physicists since they possess highly degenerate ground states with non-zero entropy at 0 K, which can give rise to interesting new phenomena. A prominent example which has been widely studied in condensed matter physics is artificial spin ice. Using Magnetic Force Microscopy (MFM), the group of W. Branford (Imperial College, UK) have studied the magnetic reversal of a nanostructured permalloy honeycomb lattice, demonstrating the breakdown of the artifical spin ice regime at cryogenic temperatures and in high magnetic fields.
(Data courtesy of W.R. Branford, Imperial College, UK)
K. Zeissler et al., Scientific Reports 6, 30218 (2016)
Transition from slow Abrikosov to fast moving Josephson vortices
attocube proudly presents his cutting edge application using the ANR31 rotator: They observed the formation of fast moving Josephson vortices, which depends critically on the angular alignment. Using the ANR31, they were able to rotate the sample below 2 K with better than 0.1° precision and could observe no drifts while sweeping temperature and magnetic field.
This measurement was realized with the ANR31/LT rotator made from Titanium and CuBe.
Magnetic Resonance Imaging of Nanoscale Virus at 300 mK
attocube’s ANPx51 positioners were used in an MRFM setup with the task to precisely and reliably position a magnetic tip and a copper nanowire to close proximity of an ultra-sensitive cantilever. The MRFM setup was applied to investigate and reconstruct the 1H spin distribution of Tobacco Mosaic Virus particles, representing a 100-million fold improvement in volume resolution over conventional MRI.
This measurement was realized with the ANPx51/LT - linear x-nanopositioner.
Visualization of Edge State in LPCMO Manganite Strip
Edge states that are induced by broken symmetry effects in two-dimensional electronic systems are in the focus of research. However, the question about the existence of edge states in strong correlated oxides was not fully answered until the group of Prof J. Shen (State Key Laboratory of Surface Physics and Department of Physics, Fudan University, Shanghai, China) demonstrated edge states in exactly these type of materials.
They used La0.325Pr0.3Ca0.275MnO3 (LPCMO) manganite strips and characterised these with an attoAFM Ixs with the upgrade for magnetic force measurements in a PPMS system at low temperatures. Experimental results including MFM images help to understand the edge states which are associated with the broken symmetry effect in manganites. The Figure shows MFM images under 9T and at temperatures of 10 K and 120 K. The scanned areas are 20?µm × 20?µm in the figures of the first row and 15?µm × 15?µm below.
Their findings prove the existence of novel edge state in strongly correlated oxides beyond the current two-dimensional electronic systems and opens a new understanding of broken symmetry effects in complex oxides.
(Image courtesy of K. Du, K. Zhang, and J.Shen, Fudan University, Shanghai, China)
Vortex Imaging on Iron Pnictides using the attoMFM Ixs
In their latest publication, H. Yang and co-workers from the group of Prof. Hai-Hu Wen, from Nanjing University, present results on vortex studies on Ba1-xKxFe2As2 - a potassium-doped superconductor of the pnictide family. Since their discovery in 2008, the iron-pnictides have drawn intensive attention, not only because they have broken the monopoly of the cuprates but also because of strong pinning effects observed in certain pnictide-compounds. A vortex consists of a circular supercurrent, which allows for exactly one flux quantum each to penetrate the superconductor.
Angle Dependent Magnetoresistance Measurement at Cryogenics
Due to the arbitrary orientation inherent to self-assembled materials on the substrate, typical characterization techniques such as magnetoresistance measurements conducted at cryogenic temperatures greatly benefit from the possibility to freely change the mutual orientation of external magnetic field and sample. Although this is easily possible e.g. by using a 3D vector magnet setup, the associated costs (>> 100 k$) are often prohibitive. Single axis sample rotator setups on the other hand not only require choosing either an out-of-plane or in-plane configuration prior to cooldown, but also put firm restrictions on certain measurements which rely on a precise orientation of the field e.g. perpendicular or parallel to an initially unknown direction along a sample structure. The perfect solution to such applications is attocube’s 3-dimensional rotator atto3DR.
Similar to a recent publication by C. H. Butschkow and co-workers from the group of Prof. Dieter Weiss (Univ. of Regensburg), magnetotransport measurements on individual GaAs/(Ga,Mn)As core-shell nanowires (top figure) have been conducted.
The center figure shows magnetoresistance at 5 T as a function of the angle between externally applied magnetic field and the nanowire axis for different rotation planes: (orange) in-plane rotation, referring to the SiO2 substrate plane, (green) out of plane (perpendicular) rotation with the long nanowire axis (typically 4 µm long and 100 nm in diameter) entirely in the rotation plane, and (blue) out of plane (transversal) rotation with the rotation plane transversal to the nanowire axis.
The bottom figure shows the normalized magnetoresistance as a function of the angle between externally applied magnetic field and the nanowire axis for various magnitudes of the external magnetic field.
(measured by C. Butschkow in collaboration with attocube application labs 2012; sample courtesy of C. Butschkow, University of Regensburg).
C. Butschkow et al., Phys. Rev. B 87, 245303 (2013)
MFM on Co Doped Mn2Sb Single Crystal
Magnetic domain structure in the ferrimagnetic state of Co doped Mn2Sb single crystal imaged using an attoAFM Ixs Magnetic Force Microscopy (here at 290 K). The image was taken in constant distance mode with the height above the sample surface set to 50 nm. The area shown in the figure corresponds to 15 µm x 15 µm with a size of 800 x 800 pixel.
(Image courtesy of Rajeev Rawat, UGC-DAE Consortium for Scientific Research, Indore, India)
Link between bulk electric and microscopic magnetic properties of LaPryCaMnO
A research team around Prof. Jian Shen from the low-dimensional material physics group at Fudan University (China) has studied extensively thin films of manganites (LaPrCaMnO on SrTiO). This family of materials has very unique electronic and magnetic properties, which can be tailored for all sorts of spintronic and electronic applications.
Their findings have been published in a series of 5 papers, in which they have been using an attoAFM/MFM Ixs in an attoDRY1000 & PPMS to characterize the microscopic origins of a magnetic and electronic phase separation at low temperatures and in high magnetic fields controlled by nanopatterning as well as shedding light on the connection between bulk electric and microscopic magnetic properties of such films.
Switching the Magnetic Vortex Core in a Single Nanoparticle
Manipulating magnetic nanostructures is not only scientifically interesting but also offers great potential in nonvolatile data storage devices and spintronic applications.
Elena Pinilla-Cienfuegos and co-workers used a low temperature variable field attoAFM/MFM I to observe and manipulate the magnetic vortex states in 25nm diameter molecular-based magnetic nanoparticles. They found that the vortex core can be switched by the application of a very small magnetic field.
E. Pinilla-Cienfuegos, et al., ACS Nano 10 (2), 1764–1770 (2016)
Helimagnetic Phase of FeCo0.5Si0.5
Real space imaging of exotic magnetic phases provides a level of understanding that cannot be achieved with indirect techniques. The figure on the left shows one of the first observations of a helimagnetic phase using the attoMFM I. The periodicity of the stripes is around 100 nm. This phase is of particular interest because of its proximity to a skyrmion phase. Skyrmions are exotic magnetic excitations, studied extensively because of their potential use in spintronic applications. The measurement was performed on a FeCo0.5Si0.5 sample at cryogenic temperature (4K) using an attoMFM I inside a liquid helium cryostat (attoLIQUID).
(attocube application labs, 2013; sample courtesy of A. Bauer and C. Pfleiderer, Technical University of Munich, Garching, Germany)
MFM imaging of a Skyrmion lattice
In collaboration with Jan Seidel from UNSW Sydney, A. Bauer & C. Pfleiderer, TU Munich we have successfully imaged the elusive Skyrmions and their magnetic field evolution in the attoDRY1000 cryostats using the attoAFM/MFM I. See what’s possible nowadays with our sophisticated commercial instruments!