Exploring the structures of the smallest crystals

A radical new way of making structures visible at the nano level has been developed at Johannes Gutenberg University Mainz (JGU). This new method makes it possible to determine with precision the arrangement of atoms and molecules in a diverse range of materials from cement to pharmaceuticals. The procedure, which is still in its infancy, comes from the field of electron microscopy and can resolve the structure of the tiniest crystals. The method was developed by Dr. Ute Kolb's working group at the Institute of Physical Chemistry at Mainz University and is now receiving international attention. In cooperation with researchers from Spain and China, the method has now allowed the structure of a new type of fine-pore zeolite to be established, a study that the journal Science published in the end of August 2011. "We have opened a door to the world of nanostructures," is how Dr. Ute Kolb describes her working group's success.

 

In the age of nanotechnology, science is focusing increasingly on very small particles, which can no longer be captured by way of conventional x-ray structural analysis. For example, an x-ray structural analysis of a single crystal is only possible up to a crystal size of around 1 micrometer, i.e., one thousandth of a millimeter. Below this threshold, in the sphere of nanostructures, electron diffraction tomography or automated diffraction tomography (ADT) allows scientists to make a similar determination of the structure of individual crystallites for the first time. "It is as if we have switched on a light in the world of nanostructures," says Kolb. As is the case with electron microscopy, the method is generally based on the concept of an electron beam being directed at an object and diffracted as a result. The diffraction behavior allows the location of the atoms to be established.

 

Together with her working group, Kolb has developed single-crystal electron diffraction tomography, to give it is full name, over the past 10 years. They had their first major success in 2009 with the determination of the structure of barium sulfate. "Since then, the number of materials whose structure we have been able to uncover has exploded", comments Kolb. The most recent example is the determination of the structure of the zeolite ITQ-43 in cooperation with Spanish and Chinese scientists. Zeolites are crystals that are created from a compound of aluminum and silicate. They have small pores which makes them interesting for the field of energy and environmental technology because of their potential use as adsorbers, ion exchangers or catalysts for example. In water treatment, they can help to filter out heavy metals; in the oil and gas industry, their introduction was like a mini revolution for crude oil cracking. We also encounter them in our everyday lives, in washing powders for instance. Professor Dr. Avelino Corma and his team of researchers from the Technical University of Valencia synthesized a zeolite with small and medium-sized pores, the combination of which acts like a funnel, thereby enhancing its catalytic properties still further. How the complex crystal structure was analyzed using ADT is described by the team of researchers in their recent article in Science.

 

In comparison with conventional electron microscopy characterizations, electron diffraction tomography is considerably faster, more accurate, and more complete. Whereas before, structures were researched for two years, using ADT a result can be obtained within just one day. Even beam-sensitive materials are, in principle, suitable for the method, which Kolb describes as "computer tomography for crystals". ADT also shares a characteristic with computer tomography that has played a major role in its success: the experimental sample under the electron microscope is gradually tipped over in order to gather data from a wide variety of different positions. Using this trick, scientists can avoid the key problem found in this area: the strong interaction of the electron beam with the sample has, up to now, made the electron diffraction much more difficult.