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Xem thêmSynchrotron-like Performance in a Laboratory XAS System
X-ray absorption spectroscopy (XAS) generates the most publications of any synchrotron approach. Because of the technique’s popularity, XAS beamtime can be challenging to acquire, requiring in some cases lengthy proposal submission and evaluation periods. The competitive nature of oversubscribed beamlines mean that even highly meritorious projects rejected. Sigray developed the QuantumLeap products to make it easy to access synchrotron-like XAS performance within your own laboratory, making it possible to complete research otherwise not possible, including those involving many samples or complex in-situ experiments.
Low Atomic Number (Z) Capabilities
The QuantumLeap-V210 is entirely enclosed within a vacuum enclosure capable of evacuated environments reaching 10^-5 Torr. The system also incorporates a load-lock chamber for exchanging samples without breaking vacuum. The vacuum environment enables XAS measurements at energies as low as 1.7 keV, thus providing analysis of important light elements with atomic numbers of Z=15 (phosphorus) and Z=16 (sulfur).
The QuantumLeap-V210 uses a focusing x-ray optic to direct x-rays onto a small spot on the sample. The small spot size enables high resolution chemical microscopy, in which chemical information can be mapped with XANES and/or EXAFS across a heterogeneous sample. Additionally, the small spot size dramatically relaxes the difficulty of sample preparation. In comparison, large spot XAS systems with mm-scale spot sizes require a high degree of sample uniformity that can be challenging to achieve.
Patented QuantumLeap-V210 acquisition scheme. A focusing x-ray optic directs x-rays onto the sample. A downstream crystal separates the transmitted x-rays by wavelengths into different positions on the spatially resolving detector. The resulting “image” by the detector is the XAS spectrum.
Patented Multi-Target Ultrahigh Brightness X-ray Source
The QuantumLeap’s x-ray source features a patented design in which multiple target materials are in optimal thermal contact with diamond, which has excellent thermal conductivity properties. The rapid cooling of diamond enables higher power loading on the x-ray source to produce an intense beams of x-rays. Another key feature of the x-ray source is its motorized x-ray multi-material target, which allows software selection between more than one x-ray target material. This is important for XAS acquisition because switching between target materials allows avoidance of the strong characteristic x-ray energies for a given material that would otherwise contaminate the results.
Mirror Lens: Capillary X-ray Optics
QuantumLeap-V210 is the only micro-XAS system commercially available. Sigray is considered the leading manufacturer of x-ray optics (the company is a key supplier to synchrotron groups around the world), and the QuantumLeap-V210’s design features x-ray optics that relay x-rays from the source to the sample with high efficiency and without chromatic aberrations. The small focused spot on the sample is advantageous for straightforward sample preparation and the ability to analyze heterogeneous samples at high resolution.
Vacuum Enclosure
QuantumLeap-V210 is entirely enclosed in large vacuum chamber capable of environments down to below 10^-5 Torr. The design is critical for enabling XAS of low atomic number elements such as phosphorus and sulfur. This capability is not available even at most synchrotron XAS beamlines due to the complexity of high vacuum instrumentation.
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.
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. Furthermore, the vacuum enclosure of the QuantumLeap-V210 permits analysis of important new battery concepts such as high energy density Li-S batteries by providing access to sulfur chemistry.
Nanoparticles and Nanotubes
The electric, magnetic, and catalytic properties of nanoparticles differ strongly from the same materials in bulk phase. These properties depend on the nanoparticle’s size and shape. Nanoparticles of 1-5nm in size are difficult to characterize with ordinary laboratory techniques such as XRD and TEM. XAS provides information on the distance of atoms, average size of particles smaller than 2nm, and even shape.
