In the field of nanomagnetism and spintronics, integral magnetometry is nowadays challenged by samples with low magnetic moments and/or low coercive fields. Commercial superconducting quantum interference device magnetometers are versatile experimental tools to magnetically characterize samples with ultimate sensitivity as well as with a high degree of automation. For realistic experimental conditions, the as-recorded magnetic signal contains several artifacts, especially if small signals are measured on top of a large magnetic background or low magnetic fields are required. In this Tutorial, we will briefly review the basic principles of magnetometry and present a representative discussion of artifacts which can occur in studying samples like soft magnetic materials as well as low moment samples. It turns out that special attention is needed to quantify and correct the residual fields of the superconducting magnet to derive useful information from integral magnetometry while pushing the limits of detection and to avoid erroneous conclusions.
The evolution of the structural and magnetic properties of Co doped ZnO has been investigated over an unprecedented concentration range above the coalescence limit. ZnO films with Co concentrations from 20% to 60% of the cationic lattice have been grown by reactive magnetron sputtering. The wurtzite crystal structure was maintained even for these high dopant concentrations. By measuring the x-ray absorption at the near edge and the linear and circular dichroism of the films at the Zn and Co K edge, it could be shown that Co substitutes predominantly for Zn in the lattice. No indications of metallic Co have been found in the samples. At low Co concentrations, the films are paramagnetic, but with increasing Co content, the films become antiferromagnetically ordered with increasing order temperature. Uncompensated spins, coupled to the antiferromagnetic dopant configurations, lead to a vertical exchange-bias-like effect, which increases with increasing Co concentration. In parallel, the single-ion anisotropy is gradually lost.
The exchange bias effect is usually defined as horizontal shift of the field-cooled magnetization loop when an antiferromagnet is directly coupled to a ferromagnet. Uncompensated spins at the interface between the two layers are believed to cause this phenomenon. The presence of such, on the other hand, would infer a vertical, i.e., a magnetization-like shift stemming from the antiferromagnet. Observations of this effect are sparse, especially in the absence of a ferromagnet. We present a model system based on extremely Co doped ZnO in which the uncompensated spins of antiferromagnetic CoO Co . .. configurations lead to this vertical shift and therefore to a field-resistant magnetization. A simple Stoner-Wohlfarth-like model based on configurations of different sizes is used to explain the occurrence of this exchange-bias-like shift and a narrow opening of the magnetization curves.
Highly Co-doped ZnO shows uncompensated antiferromagnetic order and a vertical exchange bias shift even in the absence of a ferromagnet. Therefore, it is an ideal model system to study the behavior of uncompensated antiferromagnetic moments, which play a crucial role in the description of conventional exchange bias. Temperature-and cooling-field-dependent magnetometry measurements provide further information on the compensated and uncompensated antiferromagnetic configurations in Co-doped ZnO, revealing that observed effects of both vertical exchange shift and open hysteresis stem from similar magnetic configurations. This transition is evidenced by the increase of the vertical exchange shift on the expense of the hysteresis opening by lowering the temperature.
We have investigated the relation between local structure, valence and carrier type with magnetism in the Zn-Co-O system. Thin films ranging from wurtzite Zn1−xCoxO (Co:ZnO) to ZnCo2O4 spinel were grown on c-sapphire substrates. On the one hand, the unprecedented doping of x = 0.6 Co in ZnO enables to study the structural and magnetic properties well-above the coalescence limit. On the other hand, the ZnCo2O4 spinel provides a p-type environment. We find a strong correlation between local structure, valence and carrier type throughout the Zn-Co-O system. In contrast to earlier publications neither 60% Co:ZnO nor ZnCo2O4 exhibit any sign of ferromagnetic order despite of the high concentration of magnetic ions and a p-type carrier background. Instead, antiferromagnetic exchange is found to be the predominant magnetic interaction in the Zn-Co-O system.
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