QuantumLeap-H2000
XAS Spectroscopy System
First lab XAS with both transmission and fluorescence modes
Wide energy from 4.5 to 25 keV
Key Advantages:
- Only laboratory XAS system with synchrotron-like performance
Resolving power of over 6000 and high-quality EXAFS to k=15 - Fluorescence mode XAS
First laboratory fluorescence XAS, enabling routine XAS analysis of less than 1% wt. concentrations - Energy range from 4.5 keV to 25 keV
Range encompasses transition metals such as titanium and platinum… to actinides - Patented design and approach
Design and high throughput acquisition method protected by US Patents 11/215,572, 10/428,651, and 10/416,099
Synchrotron-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 means that even highly meritorious projects are 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 that would otherwise not be feasible, including studies involving many samples or complex in-situ experiments.
Fluorescence-mode XAS for Low Concentration Samples
X-ray absorption spectroscopy (XAS) is measured by the amount of X-rays absorbed by the sample near the absorption edge energy of an element of interest. At this resonance energy, slight differences in X-ray absorption are attributable to variations in the electronic structure (e.g., oxidation state and bond lengths). The most direct way to measure XAS is in transmission mode, in which the number of X-rays transmitted through the sample is used to determine how absorptive the sample is to the X-ray energy. An indirect method is fluorescence mode. Due to the absorption of X-rays, the electrons of atoms of interest are excited. Upon relaxation, fluorescence photons are produced. The total intensity of fluorescence photons is determined by how many X-rays were originally absorbed.
Both transmission and fluorescence modes of XAS produce the same spectral graphs. The difference is that fluorescence mode is superior for low-concentration (<1–5%) samples, while transmission mode is better suited for bulk samples. The QuantumLeap-H2000 can provide results for concentrations as low as 0.1 to 0.5 wt%. Additionally, fluorescence mode XAS is required for samples that are thick or mounted on a thick substrate.
Fluorescence data can be found in our XAS results gallery, including 2–5 wt% Mn and Co in NMC battery samples and 0.5 wt% Pd, Pt, and W in catalysts. A white paper on the QuantumLeap-H2000’s fluorescence mode capabilities can be found here.
Resources:
Download Applications Note on QuantumLeap for LIBs Download Applications Note on QuantumLeap for Co Speciation in NMCs Download White Paper on Sigray Systems for Battery Science
Energy Range from 4.5 to 25 keV
QuantumLeap is the only laboratory system capable of operating at low Bragg angles, enabling the acquisition of a complete EXAFS from a single crystal without requiring the stitching together of multiple datasets. In comparison, systems operating at high Bragg angles (e.g., 55 degrees to near-backscatter at 85 degrees) require multiple crystal analyzers to maintain adequate resolution. Operating at a high 85-degree Bragg angle can provide high energy resolution, but comes with major usability drawbacks. For instance, a crystal rotation of 1 degree will cover only 7 eV at 4.5 keV and 39 eV at 25 keV. The same crystal can be used for the entire EXAFS range only if energy resolution is severely sacrificed. Otherwise, achieving adequate energy resolution requires a very large number of crystal analyzers to cover a 1000 to 2000 eV bandwidth of EXAFS. The use of many crystals is disadvantageous because it prevents straightforward robotic exchange (instead, manual crystal changes are required, which severely slow down acquisition time) and because each acquisition must be stitched and aligned.
Read about QuantumLeap’s high energy XAS capabilities in this applications note.
System Features
- Patented high brightness x-ray source with multiple targets, enabling high throughput in the laboratory and acquisition of the full range of elements
- Photon counting detector for high flux measurements
- Intuitive software for acquisition and analysis. Can output data in CVS files to be read by software such as Athena and Artemis
Patented 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, producing an intense beam of x-rays. In addition, the x-ray source offers customizability for the primary source target material, which is typically chosen in collaboration with the customer based on their applications of interest.
Beyond the benefits of high brightness and a relatively small spot size that enables fluorescence XAS (white paper), the QuantumLeap source is the first to incorporate internal calibration targets. This allows calibration off the spectral line of the x-ray source, rather than the conventional method of using absorption profiles of thin films. Not only is calibration far more accurate when using the spectral line versus absorption profiles (allowing for higher energy resolution), but it also only needs to be performed once and is fully scripted through software. In contrast, calibration using thin foils is frequently required in other laboratory XAS systems, which can be time-consuming and typically requires manual intervention.
Photon Counting Detector in Transmission Mode
QuantumLeap-H2000 uses a patented transmission XAS acquisition approach in which a novel photon-counting detector acquires the XAS spectrum instead of a conventional silicon drift detector (SDD). These detectors have extremely fast readout speeds, allowing them to detect each photon individually and enabling energy thresholding to remove harmonic contamination. Using these detectors instead of SDDs enables count rates of up to 10⁸ (100 million) counts per second—more than 500 times that of SDDs, which are limited to half a million counts per second. Such detectors are necessary for the transmission mode of XAS in the QuantumLeap-H2000 due to the high flux incident upon the sample. For fluorescence-mode XAS, the 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 multiple samples (a sample holder accommodating up to 16 samples with 3″ diameters is provided). Data can be exported as CSV files, which can be easily read into analytical software, including Athena and Artemis.
Applications
Catalysts
Catalysts, which are used to speed up chemical reactions, are estimated to be involved in 90% of all commercially produced chemical products and represent a global market exceeding $30 billion. 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 linking structural motifs with catalytic properties. QuantumLeap provides convenient in-laboratory access to such capabilities without requiring the time and expense of acquiring synchrotron beamtime.
One of the most challenging aspects of acquiring catalyst XAS spectra is the need for 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 can be found here.
Batteries and Fuel Cells
A large number of potential electrode hosts for Li+ are being explored in lithium-ion batteries (LIBs), including different material compositions and various structures ranging from micro-to nano-sized. XAS is commonly used to characterize the structural and electronic properties of electrodes to better understand the 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 in the links below, 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)
The chemistry of high atomic number elements, such as lathanides, is important for nuclear fuel research and catalyst research (e.g., Pt and Pd). One of the powerful advantages of the QuantumLeap-H2000 is its ability to perform high-energy spectroscopy up to 25 keV, as shown in the figures on the right and described in an applications note.
Technical Specifications of the QuantumLeap-H2000
| Parameter | Specification | |
|---|---|---|
| Overall | Energy Coverage | 4.5 to 25 keV |
| XAS Acquisition | Transmission mode Fluorescence mode |
|
| Energy Resolution | 0.7 eV in XANES 5-10 eV in EXAFS (Note that you can also use XANES mode to acquire high resolution EXAFS) |
|
| Beam Path | Helium flight path | |
| Focus at Sample | Line focus: 30-100 μm in one direction; ~300 um - 3mm in other direction | |
| Source | Type | Sigray patented ultrahigh brightness sealed microfocus source |
| Target(s) | Mo standard with calibration (W, Cr, Fe) targets. Others available upon request. |
|
| Power | Voltage | 300W | 20-50 kVp | |
| X-ray Crystals | Type | Up to 5 crystals Base configuration comes with 3 cylindrically curved Johansson crystals. Additional crystals for high energy or for EXAFS optimization are readily available as options. |
| X-ray Detector(s) | Type(s) | Spatially resolving (pixelated detector) for transmission XAS Silicon drift detector (SDD) for fluorescence XAS |
| Count Rate | 10^8 x-rays/s for photon counting detector 500k cps for SDD |
|
| Dimensions | Footprint and Weight | 62" W x 78.5" H x 66" D 4226 lb |
Options
In-situ Cells
QuantumLeap is designed with feedthroughs and baffles for flexibility in designing and executing in-situ and in-operando experiments. We are currently offering an off-the-shelf design for in-situ with the following capabilities:
- Vacuum-compatible sample chamber reaching 10^-7 Torr
- Gate valve for load lock mechanism
- Fluid feedthroughs for Argon and O2
- Feedthroughs for electrical, power, and heating
Downloads
Brochures and Specification Sheets
QuantumLeap-V210 White Paper
(note: V210 is a different model; more information here)
Application Notes
XAS of Batteries (NMC and Pouch Cells)
Speciation of Co in low Co formulations of NMC Batteries
High Energy XAS for Catalysts and Actinides
Fluorescence mode XAS for Challenging Samples, including Low Concentrations or Heavy Matrices
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