Patent Grant
11056308
This application relates generally to systems and methods for analyzing samples using x-rays, and more particularly, to x-ray sources configured to provide soft and/or tender x-rays selectable across an x-ray energy range.
Conventional laboratory-based x-ray sources generate x-rays by bombarding a target material (e.g., solid anode; liquid metal jet) with an electron beam. The generated x-rays include emission (e.g., fluorescence) x-rays generated by the electron beam creating holes in the inner core electron orbitals of the target atoms, which are then filled by electrons of the target with binding energies that are lower than the inner core electron orbitals, with concomitant generation of emission x-rays. The emission x-rays have discrete energies that are characteristic of the target atoms and that are less than the kinetic energy of the electron beam. In addition, the generated x-rays include Bremsstrahlung x-rays generated by the deceleration of the electron beam within the target material, the Bremsstrahlung x-rays having a continuum of energies from zero to the kinetic energy of the electron beam. Generally, in x-ray analysis applications (e.g., x-ray photoelectron spectroscopy) in which x-rays having a predetermined energy irradiate the sample, the target material of the x-ray source is selected based on the characteristic discrete energies of the emission x-rays.
For example,
In one aspect disclosed herein, a system for x-ray analysis comprises at least one x-ray source configured to emit x-rays. The at least one x-ray source comprises at least one silicon carbide sub-source on or embedded in at least one thermally conductive substrate and configured to generate the x-rays in response to electron bombardment of the at least one silicon carbide sub-source. At least some of the x-rays emitted from the at least one x-ray source comprises Si x-ray emission line x-rays. The system further comprises at least one x-ray optical train configured to receive the Si x-ray emission line x-rays and to irradiate a sample with at least some of the Si x-ray emission line x-rays.
In another aspect disclosed herein, an x-ray source comprises at least one electron source configured to generate at least one electron beam and at least one target. The at least one target comprises at least one thermally conductive substrate and a plurality of sub-sources on or embedded in at least a portion of the at least one thermally conductive substrate. The sub-sources are separate from one another and in thermal communication with the at least one thermally conductive substrate. At least one sub-source of the plurality of the sub-sources comprises silicon carbide and is configured to emit Si x-ray emission line x-rays in response to bombardment by the at least one electron beam.
In another aspect disclosed herein, a method of x-ray analysis comprises bombarding a target material comprising silicon carbide with electrons. The method further comprises emitting Si x-ray emission line x-rays from the target material. The method further comprises irradiating a sample with at least some of the Si x-ray emission line x-rays. The method further comprises detecting x-rays and/or electrons emitted from the sample.
In another aspect disclosed herein, an x-ray illumination system comprises at least one x-ray source comprising at least a first x-ray sub-source and a second x-ray sub-source. The first and second x-ray sub-sources are on or embedded in at least one thermally conductive substrate. The first x-ray sub-source comprises a first material configured to generate first x-rays in response to electron bombardment of the first x-ray sub-source. The second x-ray sub-source comprises a second material different from the first material, the second material configured to generate second x-rays in response to electron bombardment of the second x-ray sub-source. The system further comprises a plurality of x-ray optical trains comprising a first optical train and a second optical train. The first optical train comprises at least one first collimating x-ray mirror, at least one first energy-selective x-ray monochromator or multilayer, and at least one first focusing x-ray mirror. The first optical train is configured to be positioned to direct at least some of the first x-rays emitted from the first x-ray sub-source to irradiate a sample. The second optical train comprises at least one second collimating x-ray mirror, at least one second energy-selective x-ray monochromator or multilayer, and at least one second focusing x-ray mirror. The second optical train is configured to be positioned to direct at least some of the second x-rays emitted from the second x-ray sub-source to irradiate the sample.
In another aspect disclosed herein, an x-ray photoelectron spectroscopy system comprises at least one x-ray source comprising a plurality of x-ray sub-sources on or embedded in at least one thermally conductive substrate. The x-ray sub-sources comprise a plurality of materials configured to generate x-rays in response to electron bombardment. The system further comprises a plurality of x-ray optical trains, each optical train comprising at least one collimating x-ray optical element, at least one energy-selective optical element, and at least one focusing x-ray optical element. The plurality of x-ray optical trains is configured to be positioned to direct at least some of the x-rays emitted from a selected one of the plurality of x-ray sub-sources to irradiate a sample. The system further comprises a sample chamber configured to contain the sample at a sample pressure. The system further comprises a first chamber and a first electrostatic lens contained in the first chamber at a first pressure less than the sample pressure. The sample chamber and the first chamber are separated from one another by a first wall having a first aperture configured to allow at least some photoelectrons from the sample to propagate from the sample chamber to the first chamber. The system further comprises a second chamber and a second electrostatic lens contained in the second chamber at a second pressure less than the first pressure. The first chamber and the second chamber are separated from one another by a second wall having a second aperture configured to allow at least some of the photoelectrons in the first chamber to propagate to the second chamber.
Certain embodiments described herein advantageously provide emission x-rays with energies within the range between the Al Kα x-ray line (1.49 keV) and the Ga Kα x-ray line (9.25 keV). In certain embodiments, these emission x-rays are used to advantageously provide valuable information regarding samples under analysis (e.g., by selecting the emission x-ray energy to optimize the photoelectron cross sections).
Certain embodiments described herein provide a source of soft and/or tender x-rays (e.g., soft x-rays with energies in a range of 0.5 keV to about 1.8 keV; tender x-rays with energies in a range of about 1.8 keV to 6 keV) selectable across a broad energy range for tuning depth sensitivity as well as studying interfaces (e.g., gas/solid; gas/liquid; liquid/solid). The system in certain embodiments is optimized to provide a high flux of monochromatic and focused x-rays. The x-ray source of certain embodiments described herein is mountable on a 4.5″ ConFlat® flange, includes a replaceable window (e.g., Be), and includes a mechanism with sufficient travel (e.g., 50 mm) to move and position the x-ray source relative to the x-ray optical elements without breaking vacuum and without requiring re-alignment.
Certain embodiments described herein provide selectable (e.g., tunable) x-ray energies (e.g., selectable among 1.74 keV, 2.7 keV, and 5.4 keV), thereby advantageously providing selectable probing depths (e.g., from 1 nm to 15 nm) for surface, interface, and bulk analysis, and with optimized sensitivity to selected elements (e.g., Hf; Al; Ti). Certain embodiments described herein provide high x-ray energy resolution (e.g., better than 0.7 eV for all energies), small x-ray focus spot sizes (e.g., in a range from 10 μm to 200 μm; 15 μm or less; 20 μm or less; 100 μm or less) for small spot analysis and imaging, and high flux of monochromatic x-rays (e.g., greater than 2×109 photons/second at 100 μm spot size and 200 W or 300 W electron beam power; up to 5×109 photons/second) for high-speed analysis). Certain embodiments described herein provide in situ, in vitro, and/or in operando analysis in combination with small focus spot sizes and high excitation energies, thereby advantageously enabling near-ambient pressure operation. For example, by using an x-ray spot size of 100 μm, certain embodiments described herein can include electron energy analyzer slit sizes of 100 μm, thereby allowing a pressure in the sample region of about 20 mbar, which is comparable to the vapor pressure of water (e.g., about 17 mbar at 15 degrees Celsius). For another example, by using an x-ray spot size of 10 μm, certain embodiments described herein can include electron energy analyzer slit sizes of 10 μm, thereby allowing a pressure in the sample region of about 100 mbar or even higher (e.g., 1 bar), with concomitant reduced signal strength, which can be advantageously used for the study of catalysis. Certain embodiments described herein provide fully automated selection of excitation energy and/or focus spot size, with no cross-contamination of different x-rays.
While prior systems have included x-ray sources with anodes having a heat dissipation layer comprising silicon carbide, these the x-ray sources have not been configured to emit Si characteristic x-rays (e.g., the Si Kα1 line) generated in the silicon carbide (see, e.g., U.S. Pat. Appl. Publ. No. 2014/0185778). The x-ray source 20 of certain embodiments described herein is optimized to emit the Si characteristic x-rays (e.g., the Si Kα1 line) generated in the silicon carbide sub-source (e.g., to provide the Si characteristic x-rays for use by the system 10).
In certain embodiments, the at least one x-ray source 20 is configured to bombard a selected sub-source 26 with the at least one electron beam 23 (e.g., by moving, relative to one another, one or both of the at least one electron beam 23 and the at least one target 24). For example, the at least one electron source 21 of certain embodiments can be configured to direct the at least one electron beam 23 (e.g., via electric and/or magnetic fields) to bombard at least one selected sub-source 26 of the plurality of sub-sources 26 (e.g., as denoted in
As schematically illustrated by
In certain embodiments, the at least one layer 27a comprises at least one intermediate layer (e.g., W) between the substrate portion 25a and the silicon carbide, the at least one intermediate layer configured to facilitate adhesion of the silicon carbide to the substrate portion 25a and/or to provide a diffusion barrier between the silicon carbide and the substrate portion 25a. While pure, stoichiometric silicon carbide is a semiconductor, in certain embodiments, the silicon carbide can be non-stoichiometric (e.g., containing excess carbon; a molar ratio of carbon to silicon in a range between 1 and 1.45), can be doped, and/or can be coated with a thin metal layer to provide a predetermined electrical conductivity so that the sub-source 26a is configured to be used in the anode of the x-ray source 20.
In certain embodiments, the plurality of sub-sources 26 comprises at least one first sub-source 26a comprising SiC and at least one second sub-source 26b comprising at least one target material different from SiC (e.g., Al, Ag, Rh, Cr, Au, Ti, Fe, and/or Mo). In certain other embodiments, the plurality of sub-sources 26 comprises a plurality of target materials (e.g., 3, 4, or more) selected from the group consisting of: Al, Ag, Rh, Cr, Au, Ti, Fe, and Mo. The at least one target material can be on (e.g., adhered to; affixed to; sputtered onto) or embedded in a single thermally conductive substrate (e.g., diamond) or a plurality of thermally conductive substrates. For example, the at least one target material can be in thermal communication with the at least one thermally conductive substrate 26, thereby providing a heat flow path away from the at least one target material. The emitted x-rays 22 have energies corresponding to one or more characteristic x-ray lines (e.g., x-ray emission lines) of the at least one target material and ultrahigh source brightness. For example, the emitted x-rays 22 can comprise at least one of: Al Kα x-ray emission line x-rays (about 1.49 keV); Ag Lα x-ray emission line x-rays (about 2.98 keV); Rh Lα x-ray emission line x-rays (about 2.70 keV); Cr Kα1 x-ray emission line x-rays (about 5.42 keV); Au Lα x-ray emission line x-rays (about 9.70 keV); Ti Kα x-ray emission line x-rays (about 4.51 keV); Fe Kα x-ray emission line x-rays (about 6.40 keV); Mo Lα x-ray emission line x-rays (about 2.29 keV); Mo Lβ1 and Mo Lβ2 x-ray emission line x-rays (about 2.39 keV and 2.52 keV, respectively).
In certain embodiments, the at least one x-ray source 20 further comprises an x-ray window 28 (e.g., Be) configured to allow at least some of the Si x-ray emission line x-rays 22a to propagate from a first region within the x-ray source 20 and containing the at least one sub-source 27a, through the x-ray window 28, to a second region outside the x-ray source 20.
In certain embodiments, the at least one target 24 comprises an anode disk configured to be rapidly rotated while under vacuum with different regions of the anode disk along a circular track being sequentially irradiated by the electron beam 23, thereby distributing the heat load from the electron beam 23 over the circular track of the anode disk. In certain such embodiments, the anode disk is cooled by coolant (e.g., water) flowing through cooling channels within the anode disk. In certain other embodiments, the at least one target 24 is radiatively cooled. For example, a rotating anode disk of the at least one target 24 can comprise silicon carbide (which can withstand operating temperatures of about 2000 degrees Celsius), and at least one heat sink can be positioned in close proximity to a surface portion of the rotating anode disk in a region of the rotating anode disk that is separate from the region of the rotating anode disk being irradiated by the electron beam 23. While conventional rotating source anodes with cooling channels can be operated with an electron beam 23 having a power of 1000 W in a spot size of about 80 μm×80 μm, certain embodiments described herein (utilizing a rotating anode disk comprising silicon carbide) can be operated with an electron beam 23 having a power of 200 W or 300 W in a spot size of about 5 μm×5 μm, resulting in at least about a 50× improvement in x-ray brightness (80 μm/5 μm×80 μm/5 μm×200 W/1000 W).
Example parameters of the at least one x-ray source 20 include, but are not limited to: variable anode voltage in a range of 5 keV to 30 keV; electron power of up to 300 W, an electron beam footprint on at least one selected sub-source having a user-selectable size (e.g., full-width-at-half-maximum) with a first lateral dimension within a range of 5 μm to 50 μm (e.g., 5 μm to 25 μm; 10 μm to 50 μm; 10 μm to 25 μm; 25 μm to 50 μm) and a second lateral dimension perpendicular to the first lateral dimension, the second lateral dimension within a range of 30 μm to 200 μm (e.g., 30 μm to 150 μm, 30 μm to 100 μm). Examples of the at least one x-ray source 20 comprising a plurality of sub-sources 26 compatible with certain embodiments described herein are disclosed by U.S. Pat. Nos. 9,874,531, 9,823,203, 9,719,947, 9,594,036, 9,570,265, 9,543,109, 9,449,781, 9,448,190, and 9,390,881, each of which is incorporated in its entirety by reference herein.
In certain embodiments, the system 10 comprises one or more of: an x-ray photoelectron spectroscopy (XPS) system, a photoemission electron microscopy (PEEM) system, an angle-resolved photoemission spectroscopy (ARPES) system, an ambient-pressure x-ray photoelectron spectroscopy (APXPS) system, an x-ray fluorescence (XRF) system, an x-ray emission (XES) system, an x-ray phase contrast imaging system, and a computed tomography imaging system. Other types of systems and/or applications of the system are also compatible with certain embodiments described herein. The samples under analysis can comprise one or more biological samples (e.g., tissue samples), one or more semiconductor samples, one or more geological samples, and/or other types of samples.
For trace element analysis of semiconductor and geological samples, the use of the Si Kα1 x-ray emission line x-rays can advantageously reduce the background contribution from the silicon in the samples. Since the energy of the Si Kα1 x-ray emission line x-rays (about 1.74 keV) is lower than the Si K absorption edge energy, the Si Kα1 x-ray emission line x-rays do not generate the background photoelectron and/or fluorescence contributions from Si that would be seen if x-rays above the Si K absorption edge energy were used.
In certain embodiments, as schematically illustrated by
In certain embodiments, the at least one x-ray collimating optical element 34 comprises at least one substrate (e.g., comprising glass or silicon oxide). For example, the at least one substrate can be a single, unitary, hollow, axially symmetric structure (e.g., an axially symmetric tube) comprising an inner surface 36 that extends fully around the longitudinal axis 38 (e.g., encircles the longitudinal axis 38; extends 360 degrees around the longitudinal axis 38). In certain other embodiments, the at least one substrate can comprise a portion of a hollow, axially symmetric structure (e.g., a portion of an axially symmetric tube) extending along the longitudinal axis 38 with a surface 36 that extends only partially around the longitudinal axis 38 (e.g., less than 360 degrees; in a range of 45 degrees to 315 degrees; in a range of 45 degrees to 360 degrees; in a range of 180 degrees to 360 degrees; in a range of 90 degrees to 270 degrees). In certain other embodiments, the at least one substrate comprises multiple portions (e.g., 2, 3, 4, 5, 6, or more) separate from one another (e.g., with spaces between the portions) and distributed around the longitudinal axis 38, with the surface 36 of each portion extending at least partially around and along the longitudinal axis 38. For example, the surfaces 36 of the multiple portions can each extend around the longitudinal axis 38 by an angle in a range of 15 degrees to 175 degrees, in a range of 30 degrees to 115 degrees, and/or in a range of 45 degrees to 85 degrees.
In certain embodiments, at least a portion of the surface 36 has a profile that comprises a portion of a quadric profile in a cross-sectional plane that comprises the longitudinal axis 38. In certain embodiments, the surface 36 comprises multiple portions having cross-sectional profiles (e.g., in a cross-sectional plane that comprises the longitudinal axis 38) comprising corresponding quadric profiles. Examples of quadric profiles compatible with certain embodiments described herein include, but are not limited to: at least one ellipsoid; at least one paraboloid; at least one hyperboloid; or a combination of two or more thereof. In certain embodiments, the surface 36 has a first linear dimension (e.g., length) parallel to the longitudinal axis 38 in a range of 3 mm to 150 mm, a second linear dimension (e.g., width) perpendicular to the first linear dimension in a range of 1 mm to 50 mm, and a maximum linear dimension (e.g., an inner diameter; a maximum length of a straight line segment joining two points on the surface 36) in a range of 1 mm to 50 mm in a plane perpendicular to the longitudinal axis 38, a surface roughness in a range of 0.1 nm to 1 nm, and/or a plurality of surface tangent planes having a range of angles relative to the longitudinal axis 38 in a range of 0.002 radian to 0.5 radian (e.g., in a range of 0.002 radian to 0.4 radian; in a range of 0.002 radian to 0.3 radian; in a range of 0.002 radian to 0.2 radian).
The at least one second x-ray optical element 40 of
The at least one third x-ray optical element 50 of
In certain embodiments, the at least one x-ray focusing optical element 54 comprises at least one substrate (e.g., comprising glass or silicon oxide). For example, the at least one substrate can be a single, unitary, hollow, axially symmetric structure (e.g., an axially symmetric tube) comprising an inner surface 56 that extends fully around the longitudinal axis 58 (e.g., encircles the longitudinal axis 58; extends 360 degrees around the longitudinal axis 58). In certain other embodiments, the at least one substrate can comprise a portion of a hollow, axially symmetric structure (e.g., a portion of an axially symmetric tube) extending along the longitudinal axis 58 with a surface 56 that extends only partially around the longitudinal axis 58 (e.g., less than 360 degrees; in a range of 45 degrees to 315 degrees; in a range of 45 degrees to 360 degrees; in a range of 180 degrees to 360 degrees; in a range of 90 degrees to 270 degrees). In certain other embodiments, the at least one substrate comprises multiple portions (e.g., 2, 3, 4, 5, 6, or more) separate from one another (e.g., with spaces between the portions) and distributed around the longitudinal axis 58, with the surface 56 of each portion extending at least partially around and along the longitudinal axis 58. For example, the surfaces 56 of the multiple portions can each extend around the longitudinal axis 58 by an angle in a range of 15 degrees to 175 degrees, in a range of 30 degrees to 115 degrees, and/or in a range of 45 degrees to 85 degrees.
In certain embodiments, at least a portion of the surface 56 has a profile that comprises a portion of a quadric profile in a cross-sectional plane that comprises the longitudinal axis 58. In certain embodiments, the surface 56 comprises multiple portions having cross-sectional profiles (e.g., in a cross-sectional plane that comprises the longitudinal axis 58) comprising corresponding quadric profiles. Examples of quadric profiles compatible with certain embodiments described herein include, but are not limited to: at least one ellipsoid; at least one paraboloid; at least one hyperboloid; or a combination of two or more thereof. In certain embodiments, the surface 56 has a first linear dimension (e.g., length) parallel to the longitudinal axis 58 in a range of 3 mm to 150 mm, a second linear dimension (e.g., width) perpendicular to the first linear dimension in a range of 1 mm to 50 mm, and a maximum linear dimension (e.g., an inner diameter; a maximum length of a straight line segment joining two points on the surface 56) in a range of 1 mm to 50 mm in a plane perpendicular to the longitudinal axis 58, a surface roughness in a range of 0.1 nm to 1 nm, and/or a plurality of surface tangent planes having a range of angles relative to the longitudinal axis 58 in a range of 0.002 radian to 0.5 radian (e.g., in a range of 0.002 radian to 0.4 radian; in a range of 0.002 radian to 0.3 radian; in a range of 0.002 radian to 0.2 radian).
In certain embodiments, the system 10 further comprises at least one beam stop 80 configured to prevent a non-reflected portion of the x-rays 22 from impinging the at least one second x-ray optical element 40. As schematically illustrated by
In certain embodiments, the system 10 further comprises at least one detector subsystem 70 (e.g., comprising an energy dispersive x-ray energy analyzer and/or an energy dispersive electron energy analyzer) configured to detect x-rays 62 and/or electrons 64 emitted from the sample 60 (e.g., in response to the sample 60 being irradiated by the third x-ray beam 52). For example, for a system 10 selected from the group consisting of an x-ray photoelectron spectroscopy (XPS) system, a photoemission electron microscopy (PEEM) system, and an ambient-pressure x-ray photoelectron spectroscopy (APXPS) system, the at least one detector subsystem 70 can be configured to detect photoelectrons 62 (e.g., with electron energy resolution) emitted from the sample 60 in response to at least a portion of the third x-ray beam 52. For another example, for a system 10 selected from the group consisting of an x-ray fluorescence (XRF) system and an x-ray emission (XES) system, the at least one detector subsystem 70 can be configured to detect emission (e.g., fluorescence) x-rays 64 (e.g., with x-ray energy resolution) emitted from the sample 60 in response to at least a portion of the third x-ray beam 52. In certain embodiments, the at least one detector subsystem 70 comprises a pixel array 72 configured to generate images indicative of a spatial distribution of the elemental distribution of portions of the sample 60 from which the detected electrons 62 and/or detected x-rays 64 are emitted. In certain embodiments, the focused third x-ray beam 52 irradiates a portion of a first surface of the sample 60, and the at least one detector subsystem 70 can be positioned to detect x-rays 62 and/or electrons 64 emitted from at least one of: the same portion of the first surface, a different portion of the first surface, and a second surface of the sample 60 different from the first surface (e.g., the second surface opposite to the first surface). Example detector subsystems 70 compatible with certain embodiments described herein are disclosed by U.S. Pat. Nos. 9,874,531, 9,823,203, 9,719,947, 9,594,036, 9,570,265, 9,543,109, 9,449,781, 9,448,190, and 9,390,881, each of which is incorporated in its entirety by reference herein.
In certain embodiments, each of the x-ray optical trains 90 is mounted to a controllably movable stage 92 (e.g., motorized translation and/or rotation stage) configured to controllably position and select an x-ray optical train 90 for use. For example, as schematically illustrated by
In certain embodiments, a first x-ray optical train 90a is configured to be positioned to receive the x-rays 22 from the x-ray source 20 while a first target material of the x-ray source 20 comprising SiC is emitting x-rays 22a (e.g., including at least some of the Si x-ray emission line x-rays) and a second x-ray optical train 90b is configured to be positioned to receive the x-rays 22 from the x-ray source 20 while a second target material (e.g., Cr) of the x-ray source 20 is emitting x-rays 22b (e.g., including at least some of the x-ray emission line x-rays of the second target material). In certain embodiments further comprising a third x-ray optical train 90c, the third x-ray optical train 90c is configured to be positioned to receive the x-rays 22 from the x-ray source 20 while a third target material (e.g., Rh) of the x-ray source 20 is emitting x-rays 22c (e.g., including at least some of the x-ray emission line x-rays of the third target material).
In certain embodiments, the system 10 is configured to generate a Si Kα (1.74 keV) monochromatic focused third x-ray beam 52 and comprises (i) an x-ray source 20 comprising an anode comprising microstructured SiC; (ii) a first x-ray optical element 30 comprising a collimating parabolic mirror having a silver coating; (iii) a second x-ray optical element 40 comprising a channel-cut quartz or InSb (111) double-crystal monochromator, and (iv) a third x-ray optical element 50 comprising a focusing parabolic mirror having a silver coating. The monochromatic third x-ray beam 52 can have a line width with a full-width-at-half-maximum in a range of 0.5 eV to 0.7 eV, a focused x-ray spot size selectable in a range of 10 μm to 200 μm (e.g., by selecting an electron spot size on the anode; fully automated), and can be optimized for high flux (e.g., at least 2×109 photons/second for a 100 μm spot size at 200 W or 300 W of electron beam power).
In certain embodiments, in addition to being configured to generate a Si Kα (1.74 keV) monochromatic focused third x-ray beam 52 as described above, the system 10 is further configured to generate a Cr Kα (5.42 keV) monochromatic focused third x-ray beam 52 and comprises (i) an x-ray source 20 comprising an anode comprising microstructured chromium imbedded in diamond; (ii) a first x-ray optical element 30 comprising a collimating parabolic mirror having a platinum coating; (iii) a second x-ray optical element 40 comprising a channel-cut Ge (111) or Ge (220) double-crystal monochromator, and (iv) a third x-ray optical element 50 comprising a focusing parabolic mirror having a platinum coating. The monochromatic third x-ray beam 52 can have a line width with a full-width-at-half-maximum of 0.5 eV, a focused x-ray spot size selectable in a range of 10 μm to 200 μm (e.g., by selecting an electron spot size on the anode; fully automated), and can be optimized for high flux (e.g., at least 2×109 photons/second for a 100 μm spot size at 200 W or 300 W of electron beam power).
In certain embodiments, in addition to being configured to generate a Si Kα (1.74 keV) monochromatic focused third x-ray beam 52 as described above, the system 10 is further configured to generate a Rh Lα (2.70 keV) monochromatic focused third x-ray beam 52 and comprises (i) an x-ray source 20 comprising an anode comprising microstructured rhodium imbedded in diamond; (ii) a first x-ray optical element 30 comprising a collimating parabolic mirror having a silver coating; (iii) a second x-ray optical element 40 comprising a channel-cut Ge (111) or Si (111) double-crystal monochromator, and (iv) a third x-ray optical element 50 comprising a focusing parabolic mirror having a silver coating. The monochromatic third x-ray beam 52 can have a line width with a full-width-at-half-maximum of 0.5 eV, a focused x-ray spot size selectable in a range of 10 μm to 200 μm (e.g., by selecting an electron spot size on the anode; fully automated), and can be optimized for high flux (e.g., at least 2×109 photons/second for a 100 μm spot size at 200 W or 300 W of electron beam power).
Depth Selectivity
In certain embodiments, the system 10 is configured to provide depth selectivity by virtue of one or more of the following: the attenuation length within the sample 60 of the excitation third x-ray beam 52 (e.g., the distance that the third x-ray beam 52 propagates within the sample 60 where the intensity of the third x-ray beam 52 has dropped by a factor of 1/e; Iattenuation length/Iincident=1/e); the attenuation length within the sample 60 of the emission (e.g., fluorescence) x-rays 62 (e.g., the distance that the emission x-rays 62 propagate within the sample 60 where the intensity of the emission x-rays 62 has dropped by a factor of 1/e), and/or the inelastic mean free path within the sample 60 of the photoelectrons 64 (e.g., the distance, on average, that the photoelectrons 64 propagate, without loss of kinetic energy, within the sample 60 where the intensity of the photoelectrons 64 has dropped by a factor of 1/e). These attenuation lengths of the x-rays 52, 62 and the inelastic mean free path of the photoelectrons 64 are dependent on the material of the sample 60 and the energies of the excitation x-rays 52, 62 and the kinetic energies of the photoelectrons 64, respectively.
For example,
Example Configurations
As schematically illustrated by
As schematically illustrated by
Example Configuration
Table 1 lists various components of an example configuration of an APXPS system in accordance with certain embodiments described herein. The example configuration can be used in studying various processes and/or phenomena at liquid-solid interfaces (e.g., corrosion of metallic biomaterials, such as medical implants and medical devices; surface chemistry under realistic, ambient pressure environments).
The example configuration compatible with certain embodiments described herein can be characterized by a figure of merit (e.g., for comparison to other APXPS systems. For example, the figure of merit for comparing different APXPS systems for studying solid-liquid interfaces of biomaterials with depth profiling can be expressed as the intensity of the photoelectron peak (Ii) for an element of interest i at a depth (z) from the surface from where photoelectrons are emitted. The intensity Ii is dependent on the photon flux (F) incident on the interface, the average atomic concentration of element i (Ni), the photoelectron cross-section of element i related to the mentioned peak (σi), the inelastic mean free path (Λi) of photoelectrons from element i related to the mentioned peak, and the solid angle of the acceptance (Ω(hv)) of the analyzer (approximately inversely proportional to hv). In the simplest form, Ii=F*Ni*σi*exp(−z/Λi)*Ω(hv) Khv, where Khv corresponds to all other factors (which can be assumed to remain constant for a specific photon energy during the measurement).
In certain embodiments described herein, the example configuration provides five times more flux at the sample than currently marketed APXPS systems. For example, a laboratory-based APXPS system marketed by SPECS Surface Nano Analysis GMBH of Berlin Germany uses Al Kα x-rays at 1.487 keV, which are not suitable for studying solid-liquid interfaces of in-vitro biomaterials (e.g., medical implants) due to the limited IMFP of the photoelectrons. For another example, a Ga Kα (9.3 keV) x-ray source using a Ga liquid jet anode, marketed by Scienta-Omicron GmbH of Taunusstein Germany), suffers from lower cross sections and thus lower detection efficiencies (e.g., by a factor of 6, as compared to using Cr Kα x-rays). In addition, the accepted solid angle of the analyzer for 9.3 keV photoelectrons, as compared to 5.4 keV photoelectrons is about 60% less due to larger retardation used by the analyzer which reduces the solid angle. For still another example, a dual Al Kα and Cr Kα x-ray source marketed as “Phi Quantes” by Ulvac-Phi, Inc. of Kanagawa Japan, utilizes Rowland circle geometry Bragg crystals for monochromatization, which provides high resolution at the expense of lower flux and larger divergence angle.
In certain embodiments described herein, the example configuration provide three different x-ray energies, thereby allowing systematic study of depth profiling and optimizing the performance for signal strength, with a figure of merit about 50 times larger than currently marketed APXPS systems (e.g., equal to about 5 (flux)×6 (cross-section)×1.6 (acceptance solid angle)). As a result, the example configuration can provide higher flux (e.g., by a factor of five) with significantly higher cross sections and the ability for optimization depending on the element of interest and various thicknesses of the liquid and passivation layer of the sample.
Conditional language, such as “can,” “could,” “might,” or “may,” unless specifically stated otherwise, or otherwise understood within the context as used, is generally intended to convey that certain embodiments include, while other embodiments do not include, certain features, elements, and/or steps. Thus, such conditional language is not generally intended to imply that features, elements, and/or steps are in any way required for one or more embodiments.
Conjunctive language such as the phrase “at least one of X, Y, and Z,” unless specifically stated otherwise, is to be understood within the context used in general to convey that an item, term, etc. may be either X, Y, or Z. Thus, such conjunctive language is not generally intended to imply that certain embodiments require the presence of at least one of X, at least one of Y, and at least one of Z.
Language of degree, as used herein, such as the terms “approximately,” “about,” “generally,” and “substantially,” represent a value, amount, or characteristic close to the stated value, amount, or characteristic that still performs a desired function or achieves a desired result. For example, the terms “approximately,” “about,” “generally,” and “substantially” may refer to an amount that is within ±10% of, within ±5% of, within ±2% of, within ±1% of, or within ±0.1% of the stated amount. As another example, the terms “generally parallel” and “substantially parallel” refer to a value, amount, or characteristic that departs from exactly parallel by ±10 degrees, by ±5 degrees, by ±2 degrees, by ±1 degree, or by ±0.1 degree, and the terms “generally perpendicular” and “substantially perpendicular” refer to a value, amount, or characteristic that departs from exactly perpendicular by ±10 degrees, by ±5 degrees, by ±2 degrees, by ±1 degree, or by ±0.1 degree.
Various configurations have been described above. Although this invention has been described with reference to these specific configurations, the descriptions are intended to be illustrative of the invention and are not intended to be limiting. Various modifications and applications may occur to those skilled in the art without departing from the true spirit and scope of the invention. Thus, for example, in any method or process disclosed herein, the acts or operations making up the method/process may be performed in any suitable sequence and are not necessarily limited to any particular disclosed sequence. Features or elements from various embodiments and examples discussed above may be combined with one another to produce alternative configurations compatible with embodiments disclosed herein. Various aspects and advantages of the embodiments have been described where appropriate. It is to be understood that not necessarily all such aspects or advantages may be achieved in accordance with any particular embodiment. Thus, for example, it should be recognized that the various embodiments may be carried out in a manner that achieves or optimizes one advantage or group of advantages as taught herein without necessarily achieving other aspects or advantages as may be taught or suggested herein.
This application claims the benefit of priority to U.S. Provisional Appl. No. 62/728,574 filed on Sep. 7, 2018 and incorporated in its entirety by reference herein.
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| Number | Date | Country | |
|---|---|---|---|
| 20200098537 A1 | Mar 2020 | US |
| Number | Date | Country | |
|---|---|---|---|
| 62728574 | Sep 2018 | US |
