X-RAY ILLUMINATORS WITH HIGH FLUX AND HIGH FLUX DENSITY
20190088381 ยท 2019-03-21
Inventors
Cpc classification
H01J35/14
ELECTRICITY
G01N23/223
PHYSICS
G21K1/067
PHYSICS
G21K1/06
PHYSICS
International classification
G21K1/06
PHYSICS
H01J35/14
ELECTRICITY
Abstract
Systems for x-ray illumination that have an x-ray brightness several orders of magnitude greater than existing x-ray technologies. These may therefore useful for applications such as trace element detection or for micro-focus fluorescence analysis. The higher brightness is achieved in part by using designs for x-ray targets that comprise a number of microstructures of one or more selected x-ray generating materials fabricated in close thermal contact with a substrate having high thermal conductivity. This allows for bombardment of the targets with higher electron density or higher energy electrons, which leads to greater x-ray flux. The high brightness/high flux x-ray source may have a take-off angle from 0 to 105 mrad. and be coupled to an x-ray optical system that collects and focuses the high flux x-rays to spots that can be as small as one micron, leading to high flux density.
Claims
1. An x-ray illumination system comprising: an x-ray source; and at least one x-ray optical subsystem; said x-ray source comprising: a vacuum chamber; a window transparent to x-rays attached to the wall of the vacuum chamber; and, within the vacuum chamber: an anode target comprising: a substrate comprising: a first selected material; and a planar first surface, from which thickness is measured in a direction perpendicular to the first planar surface, and two orthogonal lateral dimensions are measured parallel to the first planar surface; and a plurality of discrete structures embedded into the first planar surface of the substrate such that each of the plurality of discrete structures is in thermal contact with the substrate, the plurality of discrete structures comprising: one or more materials selected for its x-ray generation properties; in which each of the plurality of discrete structures has a thickness of less than 20 microns, and each lateral dimension of said discrete structures is less than 50 microns; and in which at least two of the plurality of discrete structures are arranged on an axis; in which the axis is oriented at a take-off angle relative to the first planar surface of the substrate; in which the axis passes through the first window; and at least one electron beam emitter; and a means of directing electrons emitted by the at least one electron beam emitter onto the at least two arranged discrete structures such that x-rays are generated from each of the at least two arranged discrete structures; in which at least a portion of the generated x-rays propagating along the axis from each of the two arranged discrete structures is transmitted through the window; and said at least one x-ray optical subsystem comprising: an optical axis positioned to correspond to the axis on which the at least two discrete structures are arranged; and in which the at least one x-ray optical subsystem is further positioned to collect diverging x-rays generated by the at least two arranged discrete structures in the anode target and produce an x-ray beam with predetermined beam properties; the at least one x-ray optical subsystem additionally comprising a central beam stop positioned to block x-rays propagating parallel to said optical axis.
2. The x-ray illumination system of claim 1, in which the take-off angle is less than or equal to 105 mrad.
3. The x-ray illumination system of claim 1, in which the plurality of discrete structures are buried into the first surface of the substrate within a thickness of less than 100 microns.
4. The x-ray illumination system of claim 1, in which the plurality of discrete structures are arranged in a linear array.
5. The x-ray illumination system of claim 1, in which the plurality of discrete structures are fabricated to have similar shapes.
6. The x-ray illumination system of claim 5, in which the similar shapes are selected from the group consisting of: regular prisms, right rectangular prisms, cubes, triangular prisms, trapezoidal prisms, pyramids, tetrahedra, cylinders, spheres, ovoids, and barrel-shapes.
7. The x-ray illumination system of claim 1, in which the first selected material is selected from the group consisting of: beryllium, diamond, graphite, silicon, boron nitride, silicon carbide, sapphire, and diamond-like carbon.
8. The x-ray illumination system of claim 1, in which the one or more materials selected for its x-ray generating properties comprises a second material selected from the group consisting of: aluminum, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, gallium, zinc, yttrium, zirconium, molybdenum, niobium, ruthenium, rhodium, palladium, silver, tin, iridium, tantalum, tungsten, indium, cesium, barium, gold, platinum, lead, and combinations and alloys thereof.
9. The x-ray illumination system of claim 1, in which one edge of the substrate consists of a second surface that forms a predetermined angle with said first surface of the substrate, and said at least one of the discrete structures is positioned to be within 500 microns of said one edge of the substrate.
10. The x-ray illumination system of claim 1, in which the plurality of discrete structures of the anode target are aligned such that x-rays generated by a predetermined one of the plurality of discrete structures when exposed to electrons emitted by the at least one electron beam emitter are transmitted through another of the plurality of discrete structures.
11. The x-ray illumination system of claim 10, in which the plurality of discrete structures of the anode target are aligned such that x-rays generated by a predetermined number of the plurality of discrete structures when exposed to electrons emitted by the at least one electron beam emitter are transmitted through one predetermined discrete structure selected from the plurality of discrete structures.
12. The x-ray illumination system of claim 1, in which the at least one x-ray optical subsystem has a reflecting surface comprising a material selected from the group consisting of: boron carbide, silicon dioxide, silicon nitride, quartz, glass, chromium, copper, rhodium, palladium, gold, nickel, iridium, and platinum.
13. The x-ray illumination system of claim 1, in which the at least one x-ray optical subsystem has a reflecting surface comprising multilayers of pairs of materials, said pairs of materials selected from the group of material pairs consisting of: tungsten/carbon (W/C), tungsten/silicon (W/Si), tungsten/tungsten silicide (W/WSi.sub.2), molybdenum/silicon (Mo/Si), nickel/carbon (Ni/C), chromium/scandium (Cr/Sc), lanthanum /boron carbide (La/B.sub.4C), and tantalum/silicon (Ta/Si).
14. The x-ray illumination system of claim 1, in which the at least one x-ray optical subsystem comprises an axially symmetric hollow tube with a smooth inner surface designed for reflecting x-rays.
15. The x-ray illumination system of claim 14, in which at least a portion of the inner surface of the at least one x-ray optical subsystem is shaped in the form of a portion of a quadric surface.
16. The x-ray illumination system of claim 15, in which the quadric surface is selected from the group consisting of: a spheroid, an ellipsoid, a paraboloid, a hyperboloid, an elliptic cylinder, a circular cylinder, an elliptic cone, and a circular cone.
17. The x-ray illumination system of claim 1, in which the plurality of discrete structures of the anode target are arranged in a linear array along said axis; and the at least one x-ray optical subsystem has a predetermined axis of symmetry; and the predetermined x-ray optical subsystem axis of symmetry is aligned to correspond with the axis along which the linear array of the source is arranged.
18. The x-ray illumination system of claim 17, in which the a portion of an inner surface of the at least one x-ray optical subsystem has a form corresponding to a portion of an ellipsoid, and the distance between the x-ray source and the at least one x-ray optical subsystem is set such that x-rays reflected from the ellipsoidal portion of the inner surface are focused at a predetermined position.
19. The x-ray illumination system of claim 17, in which a portion of an inner surface of the at least one x-ray optical subsystem has a form corresponding to a portion of a paraboloid, and the x-ray source is positioned at the focus of the paraboloid such that the x-rays reflected from the paraboloidal portion of the inner surface are collimated by the at least one x-ray optical subsystem.
20. The x-ray illumination system of claim 17, in which the at least one x-ray optical subsystem comprises a Wolter type I optic, in which one of the foci corresponds to a location of x-ray generation, and a second focus of the Wolter Type I optic is at a finite distance from said one of the foci to produce a focused x-ray beam.
21. The x-ray illumination system of claim 17, in which the at least one x-ray optical subsystem comprises a Wolter type I optic, in which one of the foci corresponds to a location of x-ray generation, and a second focus of the Wolter Type I optic is at an infinitely large distance from said one of the foci to produce a collimated x-ray beam.
22. The x-ray illumination system of claim 1, in which the at least one x-ray optical subsystem has an x-ray reflecting surface comprising a material with a mass density greater than 2.5 g/cm.sup.3.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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NOTE
[0093] Elements as shown in the drawings are meant to illustrate the functioning of embodiments of the invention, and should not be assumed to have been drawn in proportion or to scale.
DETAILED DESCRIPTIONS OF EMBODIMENTS OF THE INVENTION
1. A Basic Embodiment of the Invention
[0094]
[0095] Inside the vacuum chamber 20, an electron emitter 11 connected through the lead 21 to the negative terminal of a high voltage source 10, which serves as a cathode and generates a beam of electrons 111, often by running a current through a filament. Any number of prior art techniques for electron beam generation may be used for the embodiments of the invention disclosed herein. Additional known techniques used for electron beam generation include heating for thermionic emission, Schottky emission (a combination of heating and field emission), emitters comprising nanostructures such as carbon nanotubes), and by use of ferroelectric materials. [For more on electron emission options for electron beam generation, see Shigehiko Yamamoto, Fundamental physics of vacuum electron sources, Reports on Progress in Physics vol. 69, pp. 181-232 (2006).]
[0096] A target 1100 comprising a target substrate 1000 and regions 700 of x-ray generating material is electrically connected to the opposite high voltage lead 22 and target support 32 to be at ground or a positive voltage relative to the electron emitter 11, thus serving as an anode. The electrons 111 accelerate towards the target 1100 and collide with it at high energy, with the energy of the electrons determined by the magnitude of the accelerating voltage. The collision of the electrons 111 into the target 1100 induces several effects, including the emission of x-rays 888, some of which exit the vacuum tube 20 and are transmitted through a window 40 that is transparent to x-rays.
[0097] In some embodiments of the invention, there may also be an electron control mechanism 70 such as an electrostatic lens system or other system of electron optics that is controlled and coordinated with the electron dose and voltage provided by the electron emitter 11 by a controller 10-1 through a lead 27. The electron beam 111 may therefore be scanned, focused, de-focused, or otherwise directed onto a target 1100 comprising one or more microstructures 700 fabricated to be in close thermal contact with a substrate 1000.
[0098] Once the x-rays 888 exit the source 80, a portion of the x-rays are collected by a set of x-ray optics, or optical train 840, typically comprising one or more optical elements having axial symmetry. The elements of this optical train 840 reflect x-rays at grazing angles to focus a portion 887 of the x-rays onto the object 240. X-rays that are not collected and focused may be blocked by a beam stop 850.
[0099] Once the focused portion of the x-rays 887 converge onto the object 240, x-ray fluorescence 2888 emitted from the illuminated region of the object 240 are collected by a detector 290. As in prior art systems, the detector 290 converts the detected counts to electronic signals, which may be further processed by signal processing electronics 292 and passed to an analysis system 295, which may comprise a display 298. The detector 290 commonly comprises sensors and electronics that serve as an x-ray spectrometer, analyzing both the number of x-ray fluorescence photons as well as their energy. Translation and rotation stages for the object 240 may also be provided, to allow different positions on the object 240 to be illuminated in a systematic scan or from several angles of incidence.
[0100]
[0101] It should be noted that these illustrations are presented to aid in the understanding of the invention, and the various elements (microstructures, surface layers, cooling channels, etc.) are NOT drawn to scale in these figures.
2. Structured X-ray Source
[0102] One objective of the invention is to provide a system for x-ray fluorescence measurements that is compact and has a high brightness x-ray source. One way to achieve this goal is to use x-ray targets in the system that comprise microstructured regions of x-ray generating material embedded into a thermally conductive substrate.
[0103] Microstructured targets such as those that may be used in embodiments of the invention disclosed herein have been described in detail in the US Patent Application entitled STRUCTURED TARGETS FOR X-RAY GENERATION (U.S. patent application Ser. No. 14/465,816, filed Aug. 21, 2014), which is hereby incorporated by reference in its entirety along with any provisional Applications to which this Patent Application claims benefit. Furthermore, sources using such structured targets are described more fully in the U.S. Patent Applications X-RAY SOURCES USING LINEAR ACCUMULATION (U.S. patent application Ser. No. 14/490,672 filed Sep. 19, 2014, now issued as U.S. Pat. No. 9,390,881), X-RAY SOURCES USING LINEAR ACCUMULATION (U.S. patent application Ser. No. 14/999,147, filed Apr. 1, 2016), and DIVERGING X-RAY SOURCES USING LINEAR ACCUMULATION (U.S. patent application Ser. No. 15/166,274 filed May 27, 2016), all of which are hereby incorporated by reference in their entirety, along with any provisional Applications to which these Patents and co-pending Patent Applications claim benefit. Any of the target and/or source designs and configurations disclosed in the above referenced Patents and Patent Applications may be considered for use as a component in any or all of the methods or systems disclosed herein.
[0104] As described herein and in the above cited pending Patent Applications, the target used in the source of x-rays may comprise a periodic array of sub-sources. Each sub-source may be comprised of a single or multiple microstructures of x-ray generating material in thermal contact with, or preferably embedded in, a substrate selected for its thermal conductivity. When the microstructures are in good thermal contact with a substrate having a high thermal conductivity, higher electron current densities may be used to generate x-rays, since the excess heat will be drawn away into the substrate. The higher current densities will give rise to higher x-ray flux, leading to a higher brightness source. As described in the above co-pending patent Applications, sources with microstructures of x-ray generating material may have a brightness more than 10 times larger than simpler constructions made from the same materials. Additional configurations in which multiple sub-sources are aligned to contribute x-rays on the same axis can multiply the brightness further through linear accumulation of the x-ray sub-sources.
[0105] It should also be noted here that, when the word microstructure is used herein, it is specifically referring to microstructures comprising x-ray generating material. Other structures, such as the cavities used to form the x-ray microstructures, have dimensions of the same order of magnitude, and might also be considered microstructures. As used herein, however, other words, such as structures, cavities, holes, apertures, etc. may be used for these structures when they are formed in materials, such as the substrate, that are not selected for their x-ray generating properties. The word microstructure will be reserved for structures comprising materials selected for their x-ray generating properties.
[0106] Likewise, it should be noted that, although the word microstructure is used, x-ray generating structures with dimensions smaller than 1 micron, or even as small as nano-scale dimensions (i.e. greater than 10 nm) may also be described by the word microstructures as used herein as long as the properties are consistent with the geometric factors for sub-source size and grating pitches set forth in the various embodiments.
[0107] It should also be noted that here that, when the word sub-source is used it may refer to a single microstructure of x-ray generating material, or an ensemble of smaller microstructures that function similarly to a single structure.
[0108] The fabrication of these microstructured targets may follow well-known processing steps used for the creation of embedded structures in substrates. If the substrate is a material with high thermal conductivity such as diamond, conventional lithographic patterning using photoresists can produce micron sized structures, which may then be etched into the substrate using processes such as reactive ion etching (RIE). Deposition of the x-ray generating material into the etched structures formed in the substrate may then be carried out using standard deposition processes, such as electroplating, chemical vapor deposition (CVD), atomic layer deposition, or mechanical pressing.
[0109] The x-ray generating material used in the target should ideally have good thermal properties, such as a high melting point and high thermal conductivity, in order to allow higher electron power loading on the source to increase x-ray production. The x-ray generating material should additionally be selected for good x-ray production properties, which includes x-ray production efficiency (proportional to its atomic number) and in some cases, it may be desirable to produce a specific spectra of interest, such as a characteristic x-ray spectral line. For these reasons, targets are often fabricated using tungsten, with an atomic number Z=74.
[0110] Table II lists several materials that are commonly used for x-ray targets, several additional potential target materials (notably useful for specific characteristic lines of interest), and some materials that may be used as substrates for target materials. Melting points, and thermal and electrical conductivities are presented for values near 300 K (27 C.). Most values are cited from the CRC Handbook of Chemistry and Physics, 90.sup.thed. (CRC Press, Boca Raton, Fla., 2009). Other values are cited from various sources found on the Internet. Note that, for some materials, such as sapphire for example, thermal conductivities an order of magnitude larger may be possible when cooled to temperatures below that of liquid nitrogen (77 K) [see, for example, Section 2.1.5, Thermal Properties, of E. R. Dobrovinskaya et al., Sapphire: Material, Manufacturing, Applications, Springer Science+Business Media, LLC, 2009]
[0111]
[0112] The material of the substrate 1000 may also be chosen to have a high thermal conductivity, typically larger than 100 W/(m C.) at room temperature, and the microstructures are typically embedded within the substrate, i.e. if the microstructures are
TABLE-US-00002 TABLE II Various Target and Substrate Materials and Selected Properties. Material Atomic Melting Thermal Electrical (Elemental Number Point C. Conductivity Conductivity Symbol) Z (1 atm) (W/(m C.)) (MS/m) Common Target Materials: Chromium (Cr) 24 1907 93.7 7.9 Iron (Fe) 26 1538 80.2 10.0 Cobalt (Co) 27 1495 100 17.9 Copper (Cu) 29 1085 401 58.0 Molybdenum (Mo) 42 2623 138 18.1 Silver (Ag) 47 962 429 61.4 Tungsten (W) 74 3422 174 18.4 Other Possible Target Materials: Titanium (Ti) 22 1668 21.9 2.6 Gallium (Ga) 35 30 40.6 7.4 Rhodium (Rh) 45 1964 150 23.3 Indium (In) 49 157 81.6 12.5 Cesium (Cs) 55 28 35.9 4.8 Rhenium (Re) 75 3185 47.9 5.8 Gold (Au) 79 1064 317 44.0 Lead (Pb) 82 327 35.3 4.7 Other Potential Substrate Materials with low atomic number: Beryllium (Be) 4 1287 200 26.6 Carbon (C): 6 * 2300 10.sup.19 Diamond Carbon (C): 6 * 1950 0.25 Graphite || Carbon (C): 6 * 3180 100.0 Nanotube (SWNT) Carbon (C): 6 * 200 Nanotube (bulk) Boron Nitride (BN) B = 5 ** 20 10.sup.17 N = 7 Silicon (Si) 14 1414 124 1.56 10.sup.9 Silicon Carbide Si = 14 2798 0.49 10.sup.9 (-SiC) C = 6 Sapphire Al = 13 2053 32.5 10.sup.20 (Al.sub.2O.sub.3) || C O = 8 * Carbon does not melt at 1 atm; it sublimes at ~3600 C. ** BN does not melt at 1 atm; it sublimes at ~2973 C.
shaped as rectangular prisms, it is preferred that at least five of the six sides are in close thermal contact with the substrate 1000, so that heat generated in the microstructures 700 is effectively conducted away into the substrate 1000. However, targets used in other embodiments may have fewer direct contact surfaces. In general, when the term embedded is used in this disclosure, at least half of the surface area of the microstructure will be in close thermal contact with the substrate.
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[0115] A disadvantage of the target of
[0116] To address this, some targets as may be used in some embodiments of the invention may use a configuration like that shown in
[0117] The depth of penetration for electrons into the target can be estimated by Potts' Law [P. J. Potts, Electron Probe Microanalysis, Ch. 10 of A Handbook of Silicate Rock Analysis, Springer Netherlands, 1987, p. 336)]. Using this formula, Table III illustrates some of the estimated penetration depths for some common x-ray target materials.
TABLE-US-00003 TABLE III Estimates of penetration depth for 60 keV electrons into some materials. Density Penetration Depth Material Z (g/cm.sup.3) (m) Diamond 6 3.5 13.28 Copper 29 8.96 5.19 Molybdenum 42 10.28 4.52 Tungsten 74 19.25 2.41
[0118] As an example, if 60 keV electrons are used, and diamond (Z=6) is selected as the material for the substrate 1000 and copper (Z=29) is selected as the x-ray generating material for the microstructures 700, approximately of the penetration depth in the substrate corresponds to a dimension of 10 microns, and the depth D in the x-ray generating material, which, when set to be (66%) of the electron penetration depth for copper, becomes D3.5 m.
[0119] The majority of characteristic Cu K x-rays are generated within depth D. The electron interactions below that depth typically generate few characteristic K-line x-rays but will contribute to the heat generation, thus resulting in a low thermal gradient along the depth direction. It is therefore preferable in some embodiments to set a maximum thickness for the microstructures in the target in order to limit electron interaction in the material and optimize local thermal gradients. One embodiment of the invention limits the depth of the microstructured x-ray generating material in the target to between one third and two thirds of the electron penetration depth at the incident electron energy. In this case, the lower mass density of the substrate leads to a lower energy deposition rate in the substrate material immediately below the x-ray generating material, which in turn leads to a lower temperature in the substrate material below. This results in a higher thermal gradient between the x-ray generating material and the substrate, enhancing heat transfer. The thermal gradient is further enhanced by the high thermal conductivity of the substrate material.
[0120] For similar reasons, selecting the depth D to be less than the electron penetration depth is also generally preferred for efficient generation of bremsstrahlung radiation, because the electrons below that depth have lower energy and thus lower x-ray production efficiency.
Note
[0121] Other choices for the dimensions of the x-ray generating material may also be used. In targets as used in some embodiments of the invention, the depth of the x-ray generating material may be selected to be 50% of the electron penetration depth. In other embodiments, the depth of the x-ray generating material may be selected to be 33% of the electron penetration depth. In other embodiments, the depth D for the microstructures may be selected related to the continuous slowing down approximation (CSDA) range for electrons in the material. Other depths may be specified depending on the x-ray spectrum desired and the properties of the selected x-ray generating material.
Note
[0122] In other targets as may be used in some embodiments of the invention, a particular ratio between the depth and the lateral dimensions (such as width W and length L) of the x-ray generating material may also be specified. For example, if the depth is selected to be a particular dimension D, then the lateral dimensions W and/or L may be selected to be no more than 5D, giving a maximum ratio of 5. In other targets as may be used in some embodiments of the invention, the lateral dimensions W and/or L may be selected to be no more than 2D. It should also be noted that the depth D and lateral dimensions W and L (for width and length of the x-ray generating microstructure) may be defined relative to the axis of electron propagation, or defined with respect to the orientation of the surface of the x-ray generating material. For normal incidence electrons, these will be the same dimensions. For electrons incident at an angle, care must be taken to make sure the appropriate projections are used.
[0123] Up to this point, targets that are arranged in planar configurations have been presented. These are generally easier to implement, since equipment and process recipes for deposition, etching and other planar processing steps are well known from processing devices for microelectromechanical systems (MEMS) applications using planar diamond, and from processing silicon wafers for the semiconductor industry.
[0124] However, in some embodiments, a target with a surface with additional properties in three dimensions (3-D) may be desired. As discussed previously, when the electron beam is larger than the electron penetration depth, the apparent x-ray source size and area is at minimum (and brightness maximized) when viewed parallel to surface, i.e. at a zero degree (0) take-off angle. As a consequence, the apparent brightest x-ray radiation occurs when viewed at 0 take-off angle. The radiation from within the x-ray generating material will accumulate as it propagates at 0 through the material.
[0125] With an extended target of substantially uniform material, the attenuation of x-rays between their points of origin inside the target as they propagate through the material to the surface increases with decreasing take-off angle, due to the longer distance traveled within the material, and often becomes largest at or near 0 take-off angle. Reabsorption may therefore counterbalance any increased brightness that viewing at near 0 achieves. The distance through which an x-ray beam will be reduced in intensity by 1/e is called the x-ray attenuation length, and therefore, a configuration in which the generated x-rays pass through as little additional material as possible, with the distance selected to be related to the x-ray attenuation length, may be desired.
[0126] An illustration of a portion of a target as may be used in some embodiments of the invention is presented in
[0127] The thickness of the bar D (along the surface normal of the target) is selected to be between one third and two thirds of the electron penetration depth of the x-ray generating material at the incident electron energy for optimal thermal performance. It may also be selected to obtain a desired x-ray source size in the vertical direction. The width of the bar W is selected to obtain a desired source size in the corresponding direction. As illustrated, W1.5D, but could be substantially smaller or larger, depending on the size of the source spot desired.
[0128] The length of the bar L as illustrated is L4D , but may be any dimension, and may typically be determined to be between to 3 times the x-ray attenuation length for the selected x-ray generating material. The distance between the edge of the shelf and the edge of the x-ray generating material p as illustrated is pW, but may be selected to be any value, from flush with the edge 2003 (p=0) to as much as 1 mm, depending on the x-ray reabsorption properties of the substrate material, the relative thermal properties, and the amount of heat expected to be generated when bombarded with electrons.
[0129] An illustration of a portion of an alternative target as may be used in some embodiments of the invention is presented in
[0130] In this target as may be used in some embodiments of the invention, the total volume of x-ray generating material is the same as in the previous illustration of
[0131] However, as shown in
[0132] Likewise, the distance between the edge of the shelf and the edge of the x-ray generating material p as illustrated is pW, but may be selected to be any value, from flush with the edge 2003 (p=0) to as much as 1 mm, depending on the x-ray reabsorption properties of the substrate material, the relative thermal properties, and the amount of heat expected to be generated when bombarded with electrons.
[0133] For a configuration such as shown in
[0134] The bars may be embedded in the substrate (as shown), but if the thermal load generated in the x-ray generating material is not too large, they may also be placed on top of the substrate.
[0135] Microstrutures may be embedded with some distance to the edges of the staircase, as illustrated in
[0136] An alternative target as may be used in some embodiments of the invention may have several microstructures of right rectangular prisms simply deposited upon the surface of the substrate. In this case, only the bottom base of the prism would be in thermal contact with the substrate. For a structure comprising the microstructures embedded in the substrate with a side/cross-section view as shown in
With a small value for D relative to W and L, the ratio is essentially 1. For larger thicknesses, the ratio becomes larger, and for a cube (D=W=L) in which 5 equal sides are in thermal contact, the ratio is 5. If a cap layer of a material with similar properties as the substrate in terms of mass density and thermal conductivity is used, the ratio may be increased to 6.
[0137] The amount of heat transferred per unit time (Q) conducted through a material of area A and thickness d given by:
where is the thermal conductivity in W/(m C.) and T is the temperature difference across thickness din C. Therefore, an increase in surface area A, a decrease in thickness d and an increase in T all lead to a proportional increase in heat transfer.
[0138] Other target configurations that may be used in embodiments of the invention, as has been described in the above cited U.S. patent application Ser. No. 14/465,816, are microstructures comprising multiple x-ray generating materials, microstructures comprising alloys of x-ray generating materials, microstructures deposited with an anti-diffusion layer or an adhesion layer, microstructures with a thermally conducting overcoat, microstructures with a thermally conducting and electrically conducting overcoat, microstructures buried within a substrate and the like.
[0139] Other target configurations that may be used in embodiments of the invention, as has been described in the above cited U.S. patent application Ser. No. 14/465,816, are arrays of microstructures that may comprise any number of conventional x-ray target materials (such as copper (Cu), and molybdenum (Mo) and tungsten (W)) that are patterned as features of micron scale dimensions on (or embedded in) a thermally conducting substrate, such as diamond or sapphire. In some embodiments, the microstructures may alternatively comprise unconventional x-ray target materials, such as tin (Sn), sulfur (S), titanium (Ti), antimony (Sb), etc. that have thus far been limited in their use due to poor thermal properties.
[0140] Other target configurations that may be used in embodiments of the invention, as has been described in the above cited U.S. patent application Ser. No. 14/465,816, are arrays of microstructures that take any number of geometric shapes, such as cubes, rectangular blocks, regular prisms, right rectangular prisms, trapezoidal prisms, spheres, ovoids, barrel shaped objects, cylinders, triangular prisms, pyramids, tetrahedra, or other particularly designed shapes, including those with surface textures or structures that enhance surface area, to best generate x-rays of high brightness and that also efficiently disperse heat.
[0141] Other target configurations that may be used in embodiments of the invention, as has been described in the above cited U.S. patent application Ser. No. 14/465,816, are arrays of microstructures comprising various materials as the x-ray generating materials, including aluminum, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, gallium, zinc, yttrium, zirconium, molybdenum, niobium, ruthenium, rhenium, rhodium, palladium, silver, tin, iridium, tantalum, tungsten, indium, cesium, barium, gold, platinum, lead and combinations and alloys thereof.
[0142] The embodiments described so far include a variety of x-ray target configurations that comprise a plurality of microstructures comprising x-ray generating material that can be used as targets in x-ray sources to generate x-rays with increased brightness. These target configurations have been described as being bombarded with electrons and generating x-rays, but may be used as the static x-ray target in an otherwise conventional source.
[0143] It is also possible that the targets described above may be embodied in a moving x-ray target, replacing, for example, the target in a rotating anode x-ray source with a microstructured target as described above and in the cited co-pending patent applications to create a source with a moving microstrucutred target in accord with other embodiments of the invention.
[0144] Although the targets may be aligned to radiate x-rays using a zero degree take-off angle, as discussed above, some embodiments may use near-zero degree take off angles using source configurations as presented in, for example, U.S. patent application Ser. No. 15/166274, filed May 27, 2016 by the inventors of the present Application and entitled DIVERGING X-RAY SOURCES USING LINEAR ACCUMULATION, which is hereby incorporated by reference into the present Application in its entirety.
[0145]
[0146] For the target 1100-T as illustrated, there is a local surface in the area of the x-ray generating elements that has a surface normal n. This defines an axis for the dimension of depth D into the target for determining the depth of the x-ray generating materials. This axis is also used to measure the electron penetration depth or the electron continuous slowing down approximation depth (CSDA depth).
[0147] For the target as illustrated, there is furthermore a predetermined take-off direction (designated by ray 88-T) for the downstream formation of an x-ray beam. This take-off direction is oriented at an angle .sub.T relative to the local surface, and the projection of this ray onto the local surface (designated by ray 88-S) in the plane that contains both the take-off angle and the surface normal is a determinant of the dimension of length L for the target. The final dimension of width W is defined as the third spatial dimension orthogonal to both the depth and the length directions.
[0148] As illustrated in
3. X-ray Optical System
[0149] Once x-rays are generated by a high-brightness x-ray source, a portion of the x-rays can be collected by an optical system, to be subsequently collimated and/or focused onto the object to generate fluorescence.
[0150]
[0151] The generated x-rays 888 will be diverging from the source, and after passing from the source through an x-ray transparent window 1040 to exit the vacuum chamber (not shown in
[0152] These optical elements 3000 will typically be mounted such that a portion of the x-rays experience total external reflection from the inner surface, as was described above. The reflected x-rays 887 may be focused to a point (as illustrated), or collimated, or some other diverging or converging configuration.
[0153] By placing an object 240 to be examined where it will be illuminated by the reflected x-rays 887, x-ray fluorescence 2888 is generated. A suitable detector 290 (not shown in
[0154] Note that these figures are not drawn to scale, but drawn to illustrate the principle more clearlysuch detectors often have much larger dimensions than the x-ray optics, but such a scale drawing would have obscured the source and optical elements in this three-dimensional illustration.
3.1. Ellipsoidal Optics
[0155]
[0156]
[0157] In some embodiments, as illustrated in
3.2. Paraboloidal Optics
[0158]
[0159]
[0160] Once collimated, a second optical element 3022 with a tube-shaped topology and paraboloidal inner surface, as shown in
[0161] Although the illustration shows a second paraboloidal optical element 3022 of the same size and shape as the initial paraboloidal optical element 3020, these need not be the same dimensions, but may have paraboloid surfaces with different curvature and relative focus positions.
[0162] In some embodiments, as illustrated in
[0163] Using structured targets for x-ray generation allows the use of multiple materials for x-ray generation, and the characteristic lines of several different materials may be generated by the source in some embodiments of the invention. These multi-material targets have been discussed in more detail in the co-pending Patent Applications mentioned above.
[0164]
[0165] As illustrated in
[0166] As in the previously described embodiments, a beam stop 1852 may be used to block the on-axis un-collimated x-rays. As shown in
[0167] As illustrated in
[0168] It should also be noted that this dual-wavelength optical system may be used even if the target comprises microstructures of a single x-ray generating material. Rhodium (Rh, Z=45) has two characteristic lines (L.sub.1=2.835 keV and K.sub.1=20.216 keV) that may be used to excite fluorescence from different elements. Bombarding rhodium targets with electrons having energy great enough to generate x-rays at both these lines would produce a polychromatic x-ray spectrum, and a dual wavelength optical system such as that illustrated in
[0169] It should also be noted that assembly of embodiments with such dual wavelength optical systems may entail mounting the optical elements in mounts that allow the fine adjustment of position and rotation, so that the sets of optical elements for the different wavelengths can be made to be coaxial with each other and also with the x-rays generated, especially if an x-ray target is used that features one-dimensional linear accumulation of x-rays.
3.3. Wolter Optics
[0170]
[0171] By configuring the inner surfaces of two tube-shaped optical elements 3030 and 3040 to have a hyperboloidal and ellipsoidal surfaces, and designing the optical system so that the angle of incidence for the x-rays is smaller than the critical angle (critical angles may be made larger through use of a coating for the reflecting portions; see Table I), total external reflection is achieved. Then, at least a portion of the x-rays generated by a source placed at the focus F.sub.h1. will emerge as a collimated beam of x-rays. A two-component x-ray optical system of this kind is known as Wolter Type I optics [see H. Wolter, Spiegelsysteme streifenden Einfalls als abbildende Optiken fr Rntgenstrahlen, Annalen der Physik vol. 10 (1952), pp. 94-114].
[0172]
[0173] Once collimated, a second set of optical elements 3042 and 3032 with a tube-shaped topology and hyperboloidal and ellipsoidal inner surfaces, as shown in
[0174] Although the illustrations of
[0175] In some embodiments, as illustrated in
[0176] It should be noted that, although the variation of Wolter optics as shown in
[0177] It should also be noted that a dual wavelength source as was illustrated in
[0178] As in the paraboloidal system previously illustrated in
3.4. Polycapillary Optics
[0179] Another prior art x-ray optical element is illustrated in
[0180] A larger scale optical element may be fabricated by combining many of these capillary tubes into a bundle that collects x-rays and then redirects them to a point, effectively focusing the x-rays. Such bundled capillary tubes may comprise hundreds or even thousands of glass tubes, and are called polycapillary optics. Polycapillary optics may be used as optical elements in various embodiments of the invention.
[0181]
[0182]
3.5. Other X-ray Optics
[0183] Another prior art x-ray optical element is illustrated in
[0184] As with the capillary tubes described above, these conical optical elements are often long and thin, with lateral dimensions on the order of millimeters or smaller and length on the order of several centimeters, and are constructed of glass filled with air. They are also typically designed to accept collimated beams as input, with the smaller output aperture of the tube causing convergence of the x-rays. These may therefore be used in embodiments of the invention as illustrated in
[0185] The optical elements described above may be fabricated of any number of optical materials, including glass, silica, quartz, BK7, silicon (Si), Ultra-low expansion glass (ULE), Zerodur or other elemental materials.
[0186] The reflective coatings used for the various optical elements used in embodiments of the invention as described above may be a single elemental material, to take advantage of the total external reflection for angles of incidence smaller than the critical angle, and preferably may be coated with a layer of higher mass density material (greater than 2.5 g/cm.sup.3) at least 25 nm thick. Or, the reflective coatings may be multilayer coatings, with alternating periodic layers of two or more materials, that provide constructive interference in reflection for certain wavelengths. The reflection efficiency depends on the wavelength and angle of incidence of the x-rays, and the thickness of the alternating layers, so this has limited use as a broad band reflector, but may be used if specific wavelengths are desired. Combinations that may be used for multilayer reflectors may be tungsten/carbon (W/C), tungsten/tungsten silicide (W/WSi.sub.2), molybdenum/silicon (Mo/Si), nickel/carbon (Ni/C), chromium/scandium (Cr/Sc), and lanthanum/boron carbide (La/B.sub.4C), and tantalum/silicon (Ta/Si), among others. The surface may also be a compound coating comprising an alloy or mixture of several materials.
[0187] Kirkpatrick-Baez optics may also be used in some embodiments of the invention. These are illustrated in
[0188] Embodiments with multiple sets of such optical elements stacked to collect additional x-rays, as illustrated in
[0189] Other optical elements, such as Fresnel Zone Plates, cylindrical Wolter optics, Wolter Type II optics, Wolter Type III optics, Schwarzschild optics, Montel optics, diffraction gratings, crystal mirrors using Bragg diffraction, hole-array lenses, multi-prism or alligator lenses, rolled x-ray prism lenses, lobster eye optics, micro channel plate optics, or other x-ray optical elements may be used or combined with those already described to form compound optical systems for embodiments of the invention that direct x-rays in specific ways that will be known to those skilled in the art.
3.6. X-ray Optics with Monochromators
[0190] For applications in which the spectral purity of the x-rays is important, embodiments of the invention that comprise an optical system that provides spectral purity by the incorporation of a monochromators may be used.
[0191] Such a system is illustrated in
[0192] The optical system in the embodiment shown in
[0193] The once-reflected x-rays 889-1 then propagate to a second crystal diffraction element 3056 that is designed to again reflect efficiently the same wavelength as the first crystal diffraction element 3054. The twice-reflected x-rays with a narrowed spectral bandwidth 889-2 then propagate as a collimated beam towards the object 240. Before reaching the object, however, another paraboloidal optical element 3021 is encountered that takes the collimated x-rays and creates a converging beam of x-rays 887. The x-rays focus to a spot on the object 240 that emits x-ray fluorescence 2888 detected by a detector 290.
[0194] The mount for the first crystal diffraction element 3054 may be an adjustable mount that allows translation and rotation, to maximize the reflective efficiency of the crystal, or may be fixed at a predetermined angle relative to the paraboloidal optical element 3026. Likewise, the mount for the second crystal diffraction element 3056 may be an adjustable mount that allows translation and rotation, to maximize the reflective efficiency of the crystal, or may be fixed at a predetermined angle relative to the first crystal 3054 and the paraboloidal optical element 3026. The crystal diffraction Miller index is selected to obtain the energy resolution required. In some embodiments, the x-ray energy bandwidth may be as small as 10 eV. The double crystal monochromator will typically comprise one or more rotary stages with rotation axis that is parallel to the crystal diffraction plane and perpendicular to the x-ray beam propagation direction.
[0195] Some typical crystals used for these diffractive monochromators are quartz (SiO.sub.2), lithium fluoride (LiF), sapphire (Al.sub.2O.sub.3), calcite (CaCO.sub.3), topaz (Al.sub.2(F,OH).sub.2SiO.sub.4), aluminum (Al), silicon (Si), germanium (Ge), and indium antimonide (InSb), among others. Crystal reflection efficiencies as large as 90% or higher may be achieved.
[0196] As shown, two optical elements are used to provide spectral purity, but embodiments that use only one diffractive element in reflection may also be designed. Likewise, other embodiments employing multiple elements to enhance spectral purity may be designed.
[0197] Reflectors that comprise ordered multilayers of materials, such as Mo/Si, as previously described above, can also provide wavelength selective reflection. The configuration used may be similar to that illustrated in
[0198] For more on crystal or multilayer reflectors, see James H. Underwood, Multilayers and Crystals, Section 4.1 of the X-ray Data Booklet, which may be downloaded at: xdb.lbl.gov/Section4/Sec_4-1.pdf.
4. Detectors
[0199] Several detectors may be used to detect the fluorescence generated by a object under examination in embodiments of the invention, and many of these prior art detectors are well known to those skilled in the art.
[0200] Fluorescence tends to be emitted uniformly, and therefore a larger detector collecting emitted fluorescence x-rays over a larger collection angle will produce a better signal-to-noise ratio. Such a configuration was illustrated in the general illustration of
[0201] There are three types of x-ray detectors having energy resolution (also known as spectrometers) that may be used to detect the fluorescent x-rays generated by a object under examination.
[0202] The first type, known as energy dispersive x-ray spectrometer (EDS), uses a semiconductor device to measure the energy of the detected x-ray photons. When an x-ray is absorbed by the detector, it creates a number of electron-hole pairs, with the number of electrons liberated depending on the energy of the x-ray photon. The electrons are drawn to the anode, and become a pulse of current exiting the detector. The measurement of the transient current from each pulse by a charge sensitive pre-amplifier and pulse processing electronics allows an estimation of the individual x-ray photon energy. Counts of electron bursts at different energies allow the quantitative determination of the spectrum of fluorescence x-rays. The silicon PIN photodiode (SiPIN) is a simple and low cost class of EDS spectrometer that typically has the lowest performance in terms of energy resolution.
[0203] The lithium drifted silicon (Si(Li)) or germanium (Ge(Li)) spectrometer is another class of EDS with significant better energy resolution than SiPIN, but has a count rate limited typically to less 30,000 counts per second and requires deep cooling down to liquid nitrogen temperature. A silicon drift detector (SDD) offers significant higher count rate (>10) than Si(Li) or Ge(Li) DES and requires modest cooling. Typically, an EDS can simultaneously measure x-ray spectra over a wide energy range, i.e., parallel detection. An EDS is generally preferred for fast measurement of fluorescence x-rays over a wide energy range.
[0204] The second type, known as wavelength-dispersive x-ray spectrometer (WDS), uses a wavelength-dispersive component with x-ray wavelength selection property such as a crystal or multilayer optic and an x-ray counter that receives and counts the x-rays selected by the wavelength dispersive component. Typically, a WDS has an energy resolution better than an EDS but requires sequential (serial) measurement of x-ray spectra over a wide wavelength (energy) range. A WDS is generally preferred to measure a single x-ray fluorescence line with high sensitivity and high speed or measure trace elements.
[0205] The third type, known as an x-ray microcalorimeter spectrometer (XMS), uses typically a superconductor circuit to measure change of the electric response from absorption of an x-ray photon. An XMS can provide energy resolution comparable to that of WDS and simultaneous measurement over a wide energy range, but its count rate is typically limited, requires cooling of the superconductor down to liquid helium temperature, and has a higher cost than EDS and WDS.
[0206] Additional configurations may involve additional filters (e.g. thin foils containing the appropriate element(s)) along the beam path before the detector to preferentially attenuate some unwanted x-rays from arriving at the spectrometer to reduce the background due to the detection of the x-rays scattered from the object or reduce total x-ray flux entering by the spectrometer to avoid saturation. Multiple spectrometers of the same type or combination of two or more types can be used simultaneously or interchangeable to utilize their respective strength individually or collectively. In a Si(Li) or SDD spectrometer, often multiple detector elements are packaged together as a single detector unit to increase the solid angle of collection, to increase the overall count rate, of a combination thereof
[0207] Fluorescent x-rays tend to be emitted isotropically. For some applications, a spectrometer collecting emitted fluorescence x-rays over a larger collection angle will produce a better signal-to-noise ratio is preferred. Such a configuration is illustrated in the general illustration of
[0208] If the working distance between the last optical element and the object under examination is too small to conveniently place a detector between them, a more conventional configuration such as that illustrated in
[0209] In some other configurations, such as illustrated in
[0210] Other detector geometries and arrangements for x-ray fluorescence may be known to those skilled in the art. For more on x-ray detectors, see Albert C. Thompson, X-Ray Detectors, Section 4.5 of the X-ray Data Booklet, which may be downloaded at: xdb.lbl.gov/Section4/Sec_4-5.pdf.
5. Other Source Configurations
[0211] A source for use in embodiments of the invention with the optical elements as described above is not limited to a target with microstructures embedded in one surface of the substrate. A target with may be coated on two sides, with electron beams bombarding both sides, as has been described in more detail in the above mentioned co-pending Patent Applications. The x-rays generated from both spots may be aligned to produce linear accumulation of x-rays propagating towards the optical system, increasing brightness and flux.
[0212] Multiple targets may also be aligned within the source to increase linear accumulation of x-rays. Shown in
[0213] In this embodiment, the four x-ray generating spots are aligned with an aperture 184 in a screen 84 to appear to originate from a single point of origin. An alignment procedure as discussed above for the case of a two-sided target, except that now the four electron beams 1231, 1232, 1241, and 1242 are adjusted to maximize the total x-ray intensity at a detector placed beyond the aperture 184.
[0214] As discussed above, the targets 2203 and 2204 may be rigidly mounted to structures within the vacuum chamber, or may be mounted such that their position may be varied. In some embodiments, the targets 2203 and 2204 may be mounted as rotating anodes, to further dissipate heating. The rotation of the targets 2203 and 2204 may be synchronized or independently controlled.
[0215] The thickness of the coatings 2231, 2232 and 2241, 2242 can be selected based on the anticipated electron energy and the penetration depth or the CSDA estimate for the material. If the bombardment occurs at an angle to the surface normal, as illustrated, the angle of incidence can also affect the selection of the coating thickness. Although the tilt of the targets 2203 and 2204 relative to the electron beams 1231, 1232 and 1222 is shown as 45, any angle from 0 to 90 that allows x-rays to be generated may be used.
[0216] Although only two targets with four x-ray generating surfaces are illustrated in
[0217] Likewise, the coatings themselves need not be uniform materials, but may be alloys of various x-ray generating substances, designed to produce a blend of characteristic x-rays. These may be used in embodiments that comprise the dual-wavelength optical systems described above.
[0218]
[0219] Between each of the x-ray generating targets, x-ray imaging mirror optics 2821 and 2831 are positioned to collect x-rays generated at wider angles and redirect them to a focus at a position corresponding to the x-ray generating spot another x-ray target. These optical elements 2821 and 2831 may comprise single reflectors, or multiple reflectors comprising quartic surfaces as described in the embodiments above. As illustrated, the focus is set to be the x-ray generating spot in the adjacent target, but in some embodiments, all the x-ray mirrors may be designed to focus x-rays to the same point, for example, at the final x-ray generating spot in the final (rightmost) x-ray target.
[0220] These imaging mirror optics 2821, 2822, 2831, 2832 may be any conventional x-ray imaging optical element, such as an ellipsoidal mirror with a reflecting surface typically fabricated from glass, or surface coated with a high mass density material, or an x-ray multilayer coated reflector (typically fabricated using layers of molybdenum (Mo) and silicon (Si)) or a crystal optic, or a combination thereof. The selection of the material and structure for an x-ray optic and its coatings may be different, depending on the spectrum of the x-rays to be collected and refocused. Although illustrated as cross sections, the entire x-ray optic or a portion thereof may have cylindrical symmetry.
6. Limitations and Extensions
[0221] Other uses for the high flux and high flux density illuminators described here for use in an x-ray fluorescence system may be known to those skilled in the art. For example, the sources as described according to the invention and the optical systems that collimate x-rays may be used for x-ray diffraction, crystallography, spectroscopy and small-angle scattering applications.
[0222] Illustrated in
[0223] With this application, several embodiments of the invention, including the best mode contemplated by the inventors, have been disclosed. It will be recognized that, while specific embodiments may be presented, elements discussed in detail only for some embodiments may also be applied to others. Also, details and various elements described as being in the prior art may also be applied to various embodiments of the invention.
[0224] While specific materials, designs, configurations and fabrication steps have been set forth to describe this invention and the preferred embodiments, such descriptions are not intended to be limiting. Modifications and changes may be apparent to those skilled in the art, and it is intended that this invention be limited only by the scope of the appended claims.