Mikkel Fougt Hansen

We have developed an in situ sample-holder—akin to a quartz-based plug-flow reactor—for vibrating sample magnetometry (VSM) in gas-controlled environments at ambient pressure and temperatures up to ∼1000 °C. The holder matches onto a specific type of vibrating sample magnetometer (Lake Shore model 7404-S), but the principles are applicable to other types of VSM. The holder has been tested on powder samples of Co particles on a MgAl2O4 support in both reducing and oxidizing atmospheres. The results show control of gas composition and sample reduction/oxidation. In comparison with conventional sample cups, the in situ holder shows a similar measurement sensitivity but a better repeatability due to the well-controlled gas atmosphere. Moreover, the in situ holder uses a closed gas tubing system such that the active gas only passes by the sample and it is not in contact with the VSM and oven parts. At the outlet, the gas can be collected for analysis and safe handling.

An important step in establishing any new metrological method is a prenormative interlaboratory study, designed to verify and validate the method against its stated aims. Here, the ⁵⁷Fe Mössbauer spectrometric ‘centre of gravity’ (COG) method was tested as a means of quantifying the magnetite/maghemite (Fe₃O₄/γ-Fe₂O₃) composition ratio in biphasic magnetic nanoparticles. The study involved seven laboratories across Europe and North and South America, and six samples—a verification set of three microcrystalline mixtures of known composition, and a validation set of three nanoparticle samples of unknown composition. The spectra were analysed by each participant using in-house fitting packages, and ex post facto by a single operator using an independent package. Repeatability analysis was performed using Mandel’s h statistic and modified Youden plots. It is shown that almost all (83/84) of the Mandel h statistic values fall within the 0.5% significance level, with the one exception being borderline. Youden-based pairwise analysis indicates the dominance of random uncertainties; and in almost all cases the data analysis phase is only a minor contributor to the overall measurement uncertainty. It is concluded that the COG method is a robust and promising candidate for its intended purpose.

Electrical four-terminal sensing at (sub-)micrometer scales enables the characterization of key electromagnetic properties within the semiconductor industry, including materials’ resistivity, Hall mobility/carrier density, and magnetoresistance. However, as devices’ critical dimensions continue to shrink, significant over/underestimation of properties due to a by-product Joule heating of the probed volume becomes increasingly common. Here, we demonstrate how self-heating effects can be quantified and compensated for via 3ω signals to yield zero-current transfer resistance. Under further assumptions, these signals can be used to characterize selected thermal properties of the probed volume, such as the temperature coefficient of resistance and/or the Seebeck coefficient.

The continuing miniaturization of optoelectronic devices, alongside the rise of electromagnetic metamaterials, poses an ongoing challenge to nanofabrication. With the increasing impracticality of quality control at a single-feature (-device) resolution, there is an increasing demand for array-based metrologies, where compliance to specifications can be monitored via signals arising from a multitude of features (devices). To this end, a square grid with quadratic sub-features is amongst the more common designs in nanotechnology (e.g. nanofishnets, nanoholes, nanopyramids, μLED arrays etc.). The electrical resistivity of such a quadratic grid may be essential to its functionality; it can also be used to characterize the critical dimensions of the periodic features. While the problem of the effective electrical resistivity ρ_eff of a thin sheet with resistivity ρ_1, hosting a doubly-periodic array of oriented square inclusions with resistivity ρ_2, has been treated before [Obnosov Y V 1999 SIAM J. Appl. Math. 59, 1267-1287], a closed-form solution has been found for only one case, where the inclusion occupies c=1/4 of the unit cell. Here we combine first-principle approximations, numerical modelling, and mathematical analysis to generalize ρeff for an arbitrary inclusion size (0<c<1). We find that in the range 0.01≤c≤0.99, ρeff may be approximated (to within <0.3% error with respect to finite element simulations) by: [formula] whereby at the limiting cases of c→0 and c→1, α approaches asymptotic values of α=2.039 and α=1/c-1, respectively. The applicability of the approximation to considerably more complex structures, such as recursively-nested inclusions and/or nonplanar topologies, is demonstrated and discussed. While certainly not limited to, the theory is examined from within the scope of micro four-point probe (M4PP) metrology, which currently lacks data reduction schemes for periodic materials whose cell is smaller than the typical μm-scale M4PP footprint.

Rolling circle amplification (RCA) is a robust isothermal nucleic acid amplification method producing nanocomposites of DNA and inorganic magnesium pyrophosphate precipitates. Although the conformation and structure of such nanocomposites impact applications, most studies of them have been performed at the end‐point after exposure to a treatment. Here, we use real‐time optomagnetic measurements of the hydrodynamic size of magnetic nanoparticles (MNPs) to study the growth of RCA products grafted onto MNPs as well as the effect of post‐RCA temperature annealing and chemical treatment. As a key result, we show that secondary structures in the RCA products trap and partially protect magnesium pyrophosphate precipitates and that these are reversibly released upon heating above a characteristic temperature defined by the sequence of the RCA product. These findings provide a deeper mechanistic understanding of the synthesis and structure of DNA nanocomposites, which impacts applications of DNA nanocomposites in sensing and drug delivery.

Detection of a single base mutation in Mycobacterium tuberculosis DNA can provide fast and highly specific diagnosis of antibiotic-resistant tuberculosis. Mutation-specific ligation of padlock probes (PLPs) on the target followed by rolling circle amplification (RCA) is highly specific, but challenging to integrate in a simple microfluidic device due to the low temperature stability of the phi29 polymerase and the interference of phi29 with the PLP annealing and ligation. Here, we utilized the higher operation temperature and temperature stability of Equiphi29 polymerase to simplify the integration of the PLP ligation and RCA steps of an RCA assay in two different strategies performed at uniform temperature. In strategy I, PLP annealing took place off-chip and the PLP ligation and RCA were performed in one pot and the two reactions were clocked by a change of the temperature. For a total assay time of about 1.5 h, we obtained a limit of detection of 2 pM. In strategy II, the DNA ligation mixture and the RCA mixture were separated into two chambers on a microfluidic disc. After on-disc PLP annealing and ligation, the disc was spun to mix reagents and initiate RCA. For a total assay time of about 2 h, we obtained a limit of detection of 5 pM. Graphical abstract