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Xem thêmPatented Low Contamination High Brightness X-ray Source with In-built Calibration Targets
The QuantumLeap’s x-ray source is made in-house at Sigray and features a design in which the target material is in optimal thermal contact with diamond, which has excellent thermal conductivity. The rapid cooling of diamond enables higher power loading on the x-ray source to produce an intense beam of x-rays. In addition, the x-ray source has undergone significant processing innovations, to remove problems with spectral contamination that can arise from the use of specific materials for the x-ray tube body and its components (e.g., electron optics, corona guard, anode substrate, etc.). The presence of spectral contamination would otherwise significantly degrade the quality of XAS spectra, particularly for transition metals. Furthermore, the x-ray source target material can be customized based on the customer’s set of applications.
In addition to benefits of high brightness, a relatively small spot size that enables fluorescence XAS (white paper), and a contamination-free spectrum, the QuantumLeap source is the first source to incorporate internal calibration targets. This allows calibrating off the spectral line of the x-ray source, rather than the conventional calibration approach using absorption profiles of thin films. Not only is the calibration far more accurate when using the spectral line vs. absorption profiles (allowing higher energy resolution), but calibration only needs to be performed once.
Photon Counting Detector in Transmission Mode
QuantumLeap-H2000 uses a patented transmission XAS acquisition approach in which a novel photon counting detector is used to acquire the XAS spectrum instead of a conventional silicon drift detector (SDD). These detectors have extremely fast readout speeds to detect each photon individually, enabling energy thresholding to remove harmonic contamination. Using these detectors instead of SDDs enables count rates of up to 10^8 (100 million) counts per second – more than 500X that of SDDs; SDDs are limited to half a million counts per second. Such detectors are necessary for the transmission mode of XAS QuantumLeap due to the high flux incident upon the sample. For fluorescence mode XAS, QuantumLeap-H2000 uses an SDD detector.
Software
QuantumLeap features an intuitive GUI for acquiring data, including the capability to set up recipe-based scans for point-by-point mapping or for multiple samples (a sample holder for up to 16 samples of 3″ diameters is provided). Data can be output as CSV files that can be easily read into analytical software, including Athena and Artemis.
Catalysts
Catalysts, which are used to speed up chemical reactions, are estimated to be used in 90% of all commercially produced chemical products and represent more than a $30B global market. They are used in a vast array of applications, spanning from polymers, food science, petroleum, energy processing, and fine chemicals. Synchrotron-based XAS has become the method of choice for developing novel catalysts and to link structural motifs with catalytic properties. QuantumLeap provides convenient in-laboratory access to such capabilities without requiring the time and expense of acquiring synchrotron beamtime.
Some of the most challenging aspects of acquiring catalyst XAS spectra are that they require high energy resolution to resolve pre-edge peaks of interest (see Rutile example on right) and are often prepared in low concentrations (<1wt%), particularly when the metal is precious. The low concentrations cannot be analyzed using conventional transmission geometry XAS and necessitate fluorescence geometry XAS. QuantumLeap-H2000 is the only commercial XAS system capable of acquiring fluorescence geometry XANES and EXAFS at high SNR and suitable throughputs. An example of overlaid spectra from challenging 0.5wt% to 2wt% Pd samples is shown as an example on the right.
A white paper on the fluorescence geometry XAS capabilities of QuantumLeap-H2000 is found here.
Batteries and Fuel Cells
There are a very large number of potential electrode hosts for Li+ being explored in lithium ion batteries (LIBs), including different material compositions and various structures (micro to nanosized). XAS is commonly used to characterize structural and electronic information of electrodes to obtain understanding of electrochemical mechanisms governing a given battery’s chemistry. Sigray’s QuantumLeap not only enables ex-situ determination of electrocatalyst chemistry, but is also designed with baffles and feedthroughs for optional in-situ cells to study changes in-operando.
An applications note describing the use of QuantumLeap for a set of NMC materials can be found here, and a white paper on the use of fluorescence mode XAS of the QuantumLeap for particularly challenging NMC samples with low concentration elements can be found here.
High Energy XAS (e.g., Lathanides)
Chemistry of high atomic number elements such as lathanides are important to nuclear fuel research and for catalyst research (e.g., Pt and Pd). One of the powerful advantages of QuantumLeap-H2000 is that it can perform high energy spectroscopy up to 25 keV, as shown in the figures on the right and described in an applications note.
