Nanoscale under gigapressure

Research team led by DESY and MAX IV scientists adapts important X-ray analysis method for use with difficult-to-move samples

Sometimes a change of perspective can make a world of difference. A team of scientists from DESY and MAX IV as well as University of Bayreuth has rearranged the method in which one can use an X-ray beam to image a sample without using high-quality lenses. The method, called ptychography, has been widely used at synchrotrons and free-electron lasers to analyse the inner workings of materials quickly enough while avoiding major damage to the sample by the X-rays. The team has turned the standard method of ptychography on its head: Instead of moving the sample around the X-ray beam, they have figured out how to move the X-ray beam itself in a way that does not alter the properties of the X-rays while still accomplishing the effect of ptychographic analysis. Moreover, they have tested the method on a sample that is in and of itself difficult to move – short-lived states of matter under extreme conditions of pressure and temperature. The team has published their findings in the Proceedings of the U.S. National Academy of Sciences (PNAS).

X-ray ptychography has become, in recent years, a standard technique in the toolbox of researchers using X-ray light sources. In a wide variety of fields, including biology and geology, the technique has been critical for imaging the interiors of samples up to atomic-scale detail non-destructively, revealing details on a scale that methods of light and electron microscopy cannot reach. Up to now, ptychography has been accomplished by using extremely precise sample movers that would change the position of the sample relative to the X-ray beam by tiny lengths – sometimes to the nanometre level – creating a grid pattern of sequentially imaged spots that eventually revealed the full image. Called high-resolution phase-contrast imaging, it has provided insights into the nanoscale structures of tiny biological structures, mineral deposits, computer chips and much more.

Read more on the DESY website

Image: Two views of an extreme-states experiment: To the left is an X-ray micrograph of the sample set up, which consisted of a piece of elemental iron surrounded by solid oxygen, itself surrounded by a rhenium gasket within a diamond anvil cell creating intense pressure. To the right is a ptychographic reconstruction of the area of the sample hit by X-rays, shown with a green circle. In that area using their new ptychographic method, the team could reconstruct the oxidation of the iron being melted by the intense pressure. An extreme-states experiment of this kind has not before been imaged in this way.

Credit: Tang Li, DESY

New X-ray world record: Looking inside a microchip with 4 nanometre precision

n a collaboration with EPFL Lausanne, ETH Zurich and the University of Southern California researchers at the Paul Scherrer Institute PSI have used X-rays to look inside a microchip with higher precision than ever before. The image resolution of 4 nanometres marks a new world record. The high-resolution three-dimensional images of the type they produced will enable advances in both information technology and the life sciences. The researchers are reporting their findings in the current issue of the journal Nature.

Since 2010, the scientists at the Laboratory of Macromolecules and Bioimaging at PSI have been developing microscopy methods with the goal of producing three-dimensional images in the nanometre range. In their current research, a collaboration with the EPFL and the ETHZ, the Swiss Federal Institutes of Technology in Lausanne and Zürich, and the University of Southern California, they have succeeded for the first time in taking pictures of state-of-the-art computer chips microchips with a resolution of 4 nanometres, i.e. 4 millionths of a millimetre – a world record. Instead of using lenses, with which images in this range are not currently possible, the scientists resort to a technique known as ptychography, in which a computer combines many individual images to create a single, high-resolution picture. Shorter exposure times and an optimised algorithm were key to significantly improving upon the world record they themselves set in 2017. For their experiments, the researchers used X-rays from the Swiss Light Source SLS at PSI.

Between conventional X-ray tomography and electron microscopy

Microchips are marvels of technology. Nowadays, it is possible to pack more than 100 million transistors per square millimetre into advanced integrated circuits – a trend that continues to increase. Highly automated optical systems are used to etch the nanometre-sized circuit traces into silicon blanks in clean rooms. Layer after layer is added and removed until the finished chip, the brains of our smartphones and computers, can be cut out and installed. The manufacturing process is elaborate and complicated, and characterising and mapping the resulting structures proves to be just as difficult.

While scanning electron microscopes have a resolution of a few nanometres and are therefore well suited to imaging the tiny transistors and metal interconnects that make up circuits, they can only produce two-dimensional images of the surface. “The electrons don’t travel far enough into the material,” explains Mirko Holler, a physicist at SLS. “To construct three-dimensional images with this technique, the chip has to be examined layer by layer, removing individual layers at the nanometre level – a very complex and delicate process which also destroys the chip.”

However, three-dimensional and non-destructive images can be produced using X-ray tomography, because X-rays can penetrate materials much further. This procedure is similar to a CT scan in a hospital. The sample is rotated and X-rayed from different angles. The way the radiation is absorbed and scattered varies, depending on the internal structure of the sample. A detector records the light leaving the sample and an algorithm reconstructs the final 3D image from it. “Here we have a problem with the resolution,” explains Mirko Holler. “None of the X-ray lenses currently available can focus this radiation in a way that allows such tiny structures to be resolved.”

Read more om PSI website

Image: The sample, an extract from a commercial computer chip, is supported by the gold-coloured pin in the centre of the picture. Less than 0.000 005 metres in diameter (about 20 times smaller than the width of a human hair), it was cut out of the chip using a focused ion beam and placed on the pin.

Credit: Paul Scherrer Institute PSI/Mahir Dzambegovic

Enhancing FEL imaging resolution with OAM and ptychography

The broad research fields of microscopy and computational imaging actively seek higher resolution, better quality, faster acquisition, versatile and easy-to-operate instrumentation to accommodate as many scientific applications as possible. Ptychography is one of the computational microscopy techniques based on diffraction imaging principles, where algorithms are used to reconstruct a high-fidelity image of the sample without the use of magnifying lenses. While powerful, ptychography’s effectiveness can, however, be limited by the characteristics of the probing light, particularly in the case of samples exhibiting a high degree of symmetry.

In this study, researchers at the DiProi beamline explored the use of Extreme Ultraviolet light carrying Orbital Angular Momentum (OAM), often referred to as “twisted light” to enhance ptychographic imaging resolution. Unlike conventional (Gaussian) beams, OAM light has a helical phase structure, which combined with the structured illumination of the beam profile, allows for a selective amplification of high-frequency spatial component in the diffraction process. The net effect is an increase in the amount of information (spatial resolution) that can be captured about the sample.

The experiments were conducted using the FERMI seeded free-electron laser (FEL) source, which provides a highly coherent and intense beam of light. By pairing state-of-the-art ptychography reconstruction algorithms designed by the Scientific Computing Team with the high-quality characteristics of the source, the researchers were able to reliably use the OAM beam to improve the spatial resolution of the reconstructed images.

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