X-ray spectrometer
Inventors
Ullom, Joel • O'Neil, Galen • Avila, Luis Miaja • Silverman, Kevin • Swetz, Daniel • Jimenez, Ralph • Doriese, William Bertrand • Hilton, Gene • Reintsema, Carl • Schmidt, Daniel • Alpert, Bradley K. • Uhlig, Jens • Joe, Young • Fullagar, Wilfred K. • Sundstrom, Villy • Maasilta, Ilari • Fowler, Joseph
Assignees
United States Department of Commerce
Publication Number
US-10914694-B2
Publication Date
2021-02-09
Expiration Date
2038-01-09
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Abstract
An x-ray spectrometer includes: an x-ray plasma source that produces first x-rays; an x-ray optic in optical communication with the x-ray plasma source and that: receives the first x-rays from the x-ray plasma source; focuses the first x-rays to produce second x-rays; and communicates the second x-rays to a sample that produces product x-rays in response to receipt of the second x-rays and second light; and a microcalorimeter array detector in optical communication with the sample and that receives the product x-rays from the sample.
Core Innovation
The invention disclosed is an x-ray spectrometer comprising an x-ray plasma source that produces first x-rays; an x-ray optic in optical communication with the x-ray plasma source that receives these first x-rays, focuses them to produce second x-rays, and communicates these second x-rays to a sample. The sample then produces product x-rays in response to receipt of the second x-rays and second light. A microcalorimeter array detector in optical communication with the sample receives the product x-rays from the sample.
The x-ray spectrometer further includes additional components such as a second light source producing second light delivered to the sample that causes the sample to produce product x-rays, and optionally a first light source producing first light to stimulate the x-ray plasma source. An analyzer electrically communicates with the microcalorimeter array detector to receive detector signals and determine an x-ray spectrum of the sample. Calibration is facilitated by a reference x-ray source and a calibrant target that produces reference x-rays for energy calibration of the microcalorimeter detector array.
The spectrometer addresses challenges in ultrafast time-resolved x-ray emission and absorption spectroscopy, aiming to provide a tabletop-sized, efficient system with time resolution better than 6 picoseconds. The problem being solved is the difficulty of performing time-resolved x-ray emission spectroscopy (TR-XES) with sufficient time resolution and flux on laboratory-scale instruments. Traditional TR-XES is photon-starved due to isotropic emission of secondary x-rays and limited collection efficiency of crystal spectrometers, restricting such measurements to large-scale facilities like synchrotrons and free-electron lasers. The invention advances the art by combining a laser-driven x-ray plasma source with an array of superconducting transition-edge sensor microcalorimeters, enabling high collection efficiency and energy resolution sufficient to perform complex measurements such as spin-state dynamics and ultrafast absorption changes in transition metal complexes.
Claims Coverage
The claims cover an x-ray spectrometer system and a process for performing x-ray spectroscopy including its components and their relationships. The following are the four main inventive features derived from the independent claims.
x-ray spectrometer with x-ray plasma source and focused x-ray delivery to sample producing product x-rays detected by microcalorimeter array
An x-ray spectrometer comprising an x-ray plasma source producing first x-rays; an x-ray optic that receives and focuses the first x-rays into second x-rays; and a sample that produces product x-rays in response to receipt of the second x-rays and second light. A microcalorimeter array detector positioned to receive the product x-rays from the sample. The second x-rays, sample, and second light are coincident in an interaction volume, with the second x-rays and sample copropagating at an acute angle, enabling time-resolved emission and absorption spectroscopy.
integration of second light source for sample excitation to produce product x-rays
The spectrometer further includes a second light source in optical communication with the sample that produces and communicates the second light, enabling the sample to produce product x-rays in response to the combination of second x-rays and second light.
first light source producing first light to drive the x-ray plasma source
The spectrometer further comprises a first light source that produces first light and communicates it to the x-ray plasma source, wherein the plasma source in response produces the first x-rays.
calibration system with reference x-ray source and calibrant target for microcalorimeter detector
The spectrometer includes a calibrant target in optical communication with the microcalorimeter detector that produces second reference x-rays in response to first reference x-rays from a reference x-ray source also in optical communication with the calibrant target, facilitating continuous energy calibration of the microcalorimeter detector.
Together, these inventive features form a system and method enabling high-efficiency, time-resolved x-ray spectroscopy on a tabletop apparatus with synchronized light and x-ray sources, a calibrated detector array, and an optimized geometry for interaction and detection, thus overcoming limitations of prior art in resolution, photon efficiency, and versatility.
Stated Advantages
Provides time-resolved x-ray emission and absorption spectroscopy using a tabletop-sized apparatus with time resolution better than 6 picoseconds.
Increases photon collection efficiency by approximately 660 times compared to conventional crystal spectrometers, enabling measurements with substantially lower radiation doses.
Enables ultrafast studies of spin and electronic states in transition metal complexes with elemental specificity and sensitivity to geometric and electronic structure.
Allows simultaneous measurement of multiple emission lines over a wide x-ray energy range without requiring dispersive elements.
Improves mitigation of radiation damage by reducing the number of x-ray photons delivered to samples during measurements.
Flexible detector positioning enables switching between emission, absorption, radiography, scattering, and diffraction measurement modes.
Documented Applications
Ultrafast time-resolved hard x-ray emission spectroscopy (TR-XES) for investigation of photophysical and photochemical processes in transition metal complexes including spin-crossover behavior.
Studying the quintet spin-state dynamics and lifetime measurement in polypyridyl iron complexes such as [Fe(bpy)3]2+.
Time-resolved x-ray absorption spectroscopy (XAS) of ferrioxalate photolysis to understand oxidation state and bond length changes during photoreduction reactions.
Applications in research related to light harvesting, photocatalysis, energy and data storage, and optical display technologies involving metallic complexes and nanomaterials.
Measurements of radiation-sensitive or dilute specimens where reduced radiation dose is critical.
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