New microscope captures nanoscale structures in dazzling 3D

April 19, 2012
Lithium Ion

This 3D reconstruction of a lithium-ion battery electrode, composed of 1,441 individual images captured and aligned by the TXM, reveals nanoscale structural details to help guide future energy research (credit: Brookhaven National Laboratory)

A new x-ray microscope probes the inner intricacies of materials smaller than human cells and creates unparalleled high-resolution 3D images at 25 nm.

By integrating unique automatic calibrations, scientists at the U.S. Department of Energy’s Brookhaven National Laboratory are able to capture and combine thousands of images with greater speed and precision than any other microscope.

The direct observation of structures spanning 25 nanometers will offer fundamental advances in many fields, including energy research, environmental sciences, biology, and national defense.

This innovative full field transmission x-ray microscope (TXM) was developed at Brookhaven Lab’s National Synchrotron Light Source (NSLS), which provides the x-ray source needed to capture images on the nanoscale.

Building an extra dimension

Wang’s team examined, for example, a 20-micrometer electrode from a lithium-ion battery — as thin around as a human hair. The internal interaction of pores and particles determines the energy performance of the battery, and examining that activity requires precise knowledge of the nanoscale structure.

Wang’s team took 1,441 2D pictures of the electrode as a machine rotated the tiny material specimen to capture every possible angle. The challenge then becomes converting those separate images into a single 3D structure — one in which every nanometer makes a difference. On this scale, the usual one-micron wobbles are similar in scale to taking a portrait and having the subject leap several feet to either side.

Before this new system, scientists had to manually align every single image or use software to slowly interpret the shifts. This had two major limiting effects on the process: first, the sample has to have sharp internal features or be marked to provide guidelines, which can limit material types; and second, manual alignment demands so much time that the total image count peaks in the hundreds. Brookhaven’s TXM changes that.

For the first time, the specimen is mounted on top of a platform with three sensors that measure nanometer shifts in any direction as the battery rotates and the microscope takes pictures. The computer recording the images, after calibration using a gold sphere, then automatically compensates for any shifts and accurately assembles the images into the final three-dimensional construct. The entire process takes only four hours, and that owes more to the x-rays available from NSLS than the microscope or computer.

The future of 3D imaging

Brookhaven’s National Synchrotron Light Source II (NSLS-II), scheduled to come online in 2015, will exploit the capabilities of this TXM on an even more radical scale. Imaging that lithium-ion battery took 10,000 seconds on NSLS, but with the new light source’s higher beam flux, or x-ray brightness, it will be 1,000 times faster, dropping that time to only 10 seconds.

In addition to direct structural observation, the TXM will also advance elemental and chemical understanding of materials. Maintaining constant magnification during spectroscopic imaging, which examines the unique ways that matter interacts with radiation, scientists will be able to identify the individual chemical configurations within samples. Research is currently under way by Wang’s team to demonstrate this capability.

While the focus for the new TXM will likely be on alternative energy fuels and storage solutions, the fundamental insights have already been applied to plant root structures, catalysts, and advanced electronics. The demonstrated success of the 3D imaging system has already attracted the interest of commercial users, with major corporations such as UOP and IBM scheduling time at the TXM. The Defense Advanced Research Projects Agency (DARPA) also plans to use the new microscope to probe the intricate structures of imported microchips in the interest of national security.

Ref.: Jun Wang, et al., Automated markerless full field hard x-ray microscopic tomography at sub-50 nm 3-dimension spatial resolution, Applied Physics Letters, 2012; [DOI:10.1063/1.3701579]