Electron Energy Loss Spectroscopy with a hybrid-pixel detector: pros, no cons!
A 10-minute read
As a new player on the electron microscopy (EM) marketplace, our collaboration with NION—a word-class developer of advanced electron-optical instruments—was monumental. Our work together started a couple of years ago with the testing of a prototype hybrid-pixel electron detector, now known as the DECTRIS ELA. Today, we are proud to present a summary of this endeavour’s results.
Introducing a near-ideal electron detector for EELS
What started in 2018 as a coffee break chat at M&M in Baltimore turned out to be a success story: a nearly ideal electron detector for 20-200 keV electron energy loss spectroscopy (EELS). In a joint publication, NION and DECTRIS tested and characterized DECTRIS ELA, a hybrid-pixel electron detector, and its application potential. In this article, we will summarize some of the core findings. These were recently published in Ultramicroscopy1, and discussed in our latest webinar.
Zero-loss peak and direct electron detection
One of the main challenges for a direct electron detector used in combination with an EEL spectrometer is the significant intensity difference between the zero-loss peak (ZLP) and the low-energy features present in the spectrum. Usually, the microscopist must decide to either expose for the ZLP or to shift the spectrum to avoid saturation and to expose for the features at lower energy. A radiation-hard, high-dynamic range electron-counting detector eliminates this dilemma. The setup of a NION IRIS spectrometer and DECTRIS ELA allowed for the simultaneous acquisition of ZLP and core levels, thus covering the full spectrum. Figure 1 showcases an example of such acquisitions. A hexagonal Boron Nitride (h-BN) spectrum with an intensity range spanning over seven orders of magnitude, a one-pixel point spread function and a negligible background noise shows very accurate features at every energy value.
Figure 1: h-Boron Nitride spectrum at 60 keV, 105 pA, 100 s exposure.
Detector sensitivity
Thanks to DECTRIS hybrid-pixel technology, the ELA demonstrates optimal sensitivity for electron detection at the typical energies used in commercial TEM/STEM machines. Short dark exposures result in images with zero counts due to the absence of readout noise. However, with longer exposures on the order of several tens of seconds, the electron detector records the cosmic background radiation at the rate of about four counts per frame per second. Being far below any expected EELS signal, this background noise is irrelevant for practical applications and does not affect the electron detector’s performance.
Advantages for multi-pass spectral imaging
Long acquisition times are detrimental for the quality of the experimental data, because of mechanical instabilities and degradation of the sample due to prolonged irradiation. An electron detector with a fast readout, a high framerate, absent dark current, and high dynamic range presents significant benefits in this regard. The energy-filtered images shown in Figure 2 were obtained as a sequence of shorter acquisitions, aligned, and summed. With this approach, the total radiation dose absorbed by the sample can be determined in post processing, any sample drift during the acquisition can be corrected, and even faint high-loss features are effectively visualized.
Figure 2: 128 x 128 spectral images (SI) of an STO/BTO/LMSO multilayer, acquired as 32 separate SIs of 8 s each, aligned and summed (4.3 min total).
Near-ideal detection quantum efficiency (DQE)
The data collected by NION during electron detector testing have shown that in the 30-100 keV energy range the detection efficiency of a silicon sensor is nearly ideal, and the point-spread function remains below two pixels up to 200 keV. The measured DQE at zero Nyquist is above 0.8 for 60 keV electrons, and the modulation transfer function chases the theoretical limit in a wide interval of frequencies.
Sub-pixel accuracy
DECTRIS ELA is a 2D electron detector with 1024 x 512 pixels, each of 75 x 75 µm. Since the NION IRIS spectrometer can focus the ZLP into a single pixel, a sub-pixel averaging technique has been developed, to increase the accuracy with which each feature can be resolved. Figure 3 shows an application of such technique, where several acquisitions with a ¼ pixel shift are combined to obtain richer data and to improve peak-fitting accuracy.
Figure 3: EELS of hexagonal boron nitride with E0 = 60 keV, beam current = 105 pA, 100 s exposure.
Acquisition time
The characterization of the detector was not limited to its performances. NION has used the electron detector to reproduce the results of several experiments thus illustrating the benefits of the technology. For example, the fast framerate allows revising existing techniques and giving them new life. One significant example is energy-momentum mapping of the phonon dispersion in two-dimensional systems. The NION team replicated the impressive results previously obtained by Senga et al.2, acquiring well-defined optical and acoustic phonon branches from an h-BN sample, with a significantly reduced acquisition time – from eight hours to eight minutes.
FAQs
Virtual pixels between chips and data acquisition?
DECTRIS ELA is made up from eight separate readout chips with 256x256 75 μm pixels each. The assembly with a continuous semiconductor sensor is aided by the presence of three columns of double-sized pixels. From an application point of view, the quality of the final data is not compromised, but the user should pay attention not to locate important features at the corresponding energy channel.
Radiation hardness?
Hybrid pixel technology is inherently radiation hard. Extended periods of irradiation of the silicon sensor with 80kV electrons did not generate features or undesirable artifacts.
4D-STEM and other applications?
The high dynamic range and high framerate accessible with DECTRIS ELA bring advantages to more than just electron energy loss spectroscopy experiments. 4D-STEM is the natural candidate for the use of this novel class of fast detectors, and it is already showing impressive preliminary results.
Software integration?
DECTRIS provides for ELA a complete and documented application programming interface, usable with most programming languages. The integration of the electron detector in any modern data pipeline, or electron microscopy suite, is straightforward. In this work, NION used the powerful open-source application NionSwift.
Electron detector compatibility?
Please, contact the manufacturer of your spectrometer for questions regarding DECTRIS ELA compatibility and integration options.
Browse our electron detector product page for more details. Or, if you have any other questions about ELA detector or its application, do not hesitate to reach out.
1. Hybrid pixel direct detector for electron energy loss spectroscopy, Ultramicroscopy, Volume 217, 2020
2. Position and momentum mapping of vibrations in graphene nanostructures, Nature 573, 247–250, 2019
