In-house synthesis and characterisation methods

Advances in materials synthesis and characterisation go hand in hand with a better understanding of fundamental physical processes as well as the discovery of new phenomena. Our division has unique expertise in both synthesis and characterisation of complex material systems. Our own labs complement larger infrastructures such as the Tandem Laboratory for ion-beam based methods and Super ADAM and other facilities for neutron scattering. We are also involved in common facilities at the Ångström Laboratory, such as Myfab, AM@Å and the X-ray laboratory.

Here you can find an overview of the set-ups situated in our own labs:

Materials growth

The synthesis of new materials is central to our research in order to be in control in all parts of the Materials research spiral (see figure on the right).

We use two techniques called magnetron sputter deposition and molecular beam epitaxy (MBE) to fabricate thin films, layers with thicknesses on the nanometre scale, of crystalline or amorphous materials. These thin films often have physical properties which differ significantly from those of thick bulk materials.

Layers of different materials can be deposited with thickness control down to a single layer of atoms. By simultaneous deposition of different materials from several sources we can produce alloys and phases that do not exist naturally. For sputter deposition it is also possible to admit a reactive gas into the sputtering chamber to produce compounds such as oxides or nitrides. These deposition processes are extremely versatile allowing us to tailor our samples to our research questions.

Illustration showing the “Materials Design Spiral”. The spiral starts at the outside at a point labelled “Design” (left side), then continues to “Synthesis” (top), “Advanced characterisation” (right) and “Analysis and modelling” (bottom). After one full turn, the spiral passes another point colour coded as “Design” and continues to “Synthesis” etc. as before. Each step is passed four times before the spiral arrives in the centre, which is labelled by bold text as “New properties & Understanding of physical phenomena”.

The Materials Design Spiral visualises the several steps and iterations necessary to develop new materials. The advanced synthesis and characterisation methods in our lab allow us to control this process from start to finish.

Nanopatterning

Illustration showing a 4-step process on how to create
a nanopatterned material. The first image is titled (I) Film growth and shows a
block consisting of four layers labelled from bottom to top: MgO substrate, V,
Pd, Cr. The second image, (II) Patterned mask, shows the same stack with an
additional layer on top that has holes arranged in a regular pattern and is
labelled Cr mask. (III) Implantation shows the stack from (II). Spheres
labelled 30 keV Fe+ and downwards pointing arrows indicate ions going through
the hole pattern. The last image, (IV) Removal of mask, shows only the MgO, V
and Pd layers. The top shows the same pattern from the holes in the same colour
as the Fe from (III) and is labelled FePd. Illustration by Christina Vantaraki.

Example for the creation of magnetic nanopatterns by ion implantation through a mask. Adapted from https://doi.org/10.1063/5.0239106.

In addition to using samples with thicknesses on the nanoscale, it is also possible to create lateral nanostructures. These structures can be topographic or distinguished by a different chemical composition.

In our division we use electron beam lithography at Myfab to create (topographic) nanostructure arrays over extended areas. Different shapes and sizes of individual structures (often called islands) and the pattern in which they are arranged are possible. We study how the structure connects to materials properties, for example magnetic behaviour.

Energetic ions can be used to remove material (“sputtering”) and for example create pores or etchable tracks in membranes. This way nanopatterned graphene can be fabricated. By irradiating a material through a patterned mask, we can also selectively implant ions and create structures with different chemical composition creating for example magnetic nanoarrays.

Self-assembly

Self-assembly is the spontaneous formation of structures on all length scales. Examples range from atoms forming galaxies containing millions of stars to cells growing into highly complex biological structures. The crucial parameter controlling self-assembly is the specific interaction between building blocks.

Self-assembly on intermediate length scales, tens of nanometres up to millimetres, allows to develop materials with new properties interesting for many applications. The most relevant interactions between building blocks for our research are van der Waals forces, hydrophobic, and magnetic and electrostatic interactions. The first two in particular are comparable to thermal excitations at room temperature, which might cause chemical bonds to break and reform resulting, for example in phase transitions.

In our group, we focus on fundamental understanding of self-assembly of colloids as well as viscoelastic properties. We study the first one by tuning magnetic and electrostatic interactions between nano- and micrometre sized particles. This way we control the self-assembly process and design materials in a bottom-up approach. We also drive self-assembled systems out of equilibrium and study the response. By combing stress-strain measurements with scattering methods we try to understand how elastic and flow properties of materials are related to the structure of the building blocks down to atomic length scales.

Black-and white-image of a drop on a surface. The drop
is reflected so that it looks like two partial spheres touching.

Self-assembled layers can for example convert a surface from a hydrophilic to a hydrophobic interface. The image shows a contact angle measurement of a droplet of water on a silicon wafer, which was coated with a self-assembled monolayer of a molecule called octadecyltrichlorosilane to turn it hydrophobic.

Structural analysis with X-rays

Photo of the set-up for measurements of pair
distribution functions. Two grey boxes, the source and detector, are mounted on
the left and right. A square sample is mounted on a movable sample stage in the
centre. A Swedish 5 kr coin is lying next to the sample showing that they are
of very comparable size.

Our set-up for measuring pair distribution function of thin films. The coin in the centre visualises the size of the square sample next to it. The sample is held by air suction to avoid additional scattering from the sample holder.

Information about crystal structure (or lack thereof), layering and interfaces can be obtained through X-ray scattering experiments in a range of different scattering geometries. X-ray diffraction is the standard method for determination of crystal structure. We also have instrumentation for X-ray reflectometry to measure the thickness of thin films. For amorphous thin films, the pair distribution function is used to quantify the distance between atoms in a sample. Our division has developed a new lab-based instrument for measuring these pair distribution functions.

We also develop and maintain several publicly available software packages for data processing and analysis of X-ray, neutron and ion scattering data.

Magnetic characterisation

The magneto-optical Kerr effect (MOKE) provides a convenient way to obtain the changes in magnetic moment at different fields and temperatures. We have several experimental setups using this effect.

Hysteresis loops, with shapes strongly dependent on e.g. anisotropy or interlayer coupling, are conveniently measured at room temperature or under other conditions, depending on which setup is used. For investigations of e.g. magnetic phase transitions, a set-up with extremely low background fields (less than 10 μT) is used. Here we can measure both AC susceptibility and low-field loops at different temperatures below 300 K. The sensitivity allows studies of even just a few monolayers of magnetic material.

At the other extreme, some samples need higher fields to reach saturation. The Vector MOKE setup combines three configuration modes with different wavelengths (spectroscopic MOKE; all elements respond differently to the incident light), a relatively high field, and a temperature range 4 – 500 K. Simultaneous measurement of the first harmonic (ellipticity) and second harmonic (rotation) of the modulated reflected light allows determination of the scaling of magnetisation with field in the vicinity of the ordering temperature as well as separation of the contribution from different elements in multilayered structures.

MOKE magnetometer

It is possible to see magnetic domains! It is even possible to distinguish between different directions of the magnetisation. Kerr microscopy has the advantage of directly monitoring the in-plane and out-of-plane magnetization components. Furthermore, Kerr microscopy can be used in a wide range, visualizing domains in the range of 0.0003 mm to a few mm. The resolution is limited, by the wavelength of the visible light to roughly 0.0003 mm.

Depending on the relative orientation of the incident light, the applied magnetic field, and the domains, patterns of black, white and greys are obtained. A large black and white contrast is obtained from areas with opposite magnetization directions.

Atomic force microscopy

AFM image

Atomic force microscopy where a sharp tip is scanned across a surface provides unique information about surface features on the nanometre scale. In our lab, we have an atomic force microscope to measure surface topography, from continuous and patterned surfaces to nanoparticles. Special tips coated in magnetic material are used for magnetic force microscopy to image nanoscale magnetic domains.

In-situ measurements

Our goal is to conduct advanced materials research leading to physics understanding of the whole life cycle of materials – from synthesis to recycling. One of the approaches we take to reach this goal are in-situ measurements, which do not take synthesis and characterisation as two separate steps as shown in the Materials research spiral but aim to characterise a sample during a specific process. In practice this can mean, that we keep a sample in the same controlled environment (for example a high vacuum) for synthesis and characterisation or that we expose it to a stimulus (for example temperature or gas pressure) and analyse induced changes at the same time.

In our specialised in-house set-up, samples can be exposed to a controlled hydrogen pressure during measurements. Crystallographic changes (rearrangements, phase transitions) can be followed in-situ at different selected pressures and a wide interval of temperatures during hydrogen uptake, even for nano-sized layers (> 50 Å), by measuring optical conductivity as well as resistivity.

Many characterisation techniques we are using can be combined with in-situ approaches. Ion beam analysis at the Tandem Laboratory can monitor depth resolved composition changes when a sample is exposed to elevated temperatures and/or different gases. Neutron scattering at Super Adam can be performed in a range of different environments, for example applied magnetic fields, a wide range of temperatures or at different gas pressures.

Our division is also one of the scientific leads of the LigHt project, which is a new multi-instrument platform for materials science with a specific focus on light-element characterisation and in-situ and in-operando experiments.

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