EP3465182A1 - Procédé et appareil de microscopie à rayons x - Google Patents

Procédé et appareil de microscopie à rayons x

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Publication number
EP3465182A1
EP3465182A1 EP17810765.2A EP17810765A EP3465182A1 EP 3465182 A1 EP3465182 A1 EP 3465182A1 EP 17810765 A EP17810765 A EP 17810765A EP 3465182 A1 EP3465182 A1 EP 3465182A1
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EP
European Patent Office
Prior art keywords
ray
micro
beams
detector
array
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP17810765.2A
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German (de)
English (en)
Other versions
EP3465182A4 (fr
Inventor
Wenbing Yun
Sylvia Jia Yun Lewis
Janos KIRZ
Srivatsan Seshadri
Alan Francis Lyon
David Vine
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Sigray Inc
Original Assignee
Sigray Inc
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Filing date
Publication date
Priority claimed from US15/173,711 external-priority patent/US10401309B2/en
Priority claimed from US15/605,957 external-priority patent/US10352880B2/en
Application filed by Sigray Inc filed Critical Sigray Inc
Publication of EP3465182A1 publication Critical patent/EP3465182A1/fr
Publication of EP3465182A4 publication Critical patent/EP3465182A4/fr
Withdrawn legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G01N23/041—Phase-contrast imaging, e.g. using grating interferometers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/201—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
    • G21K1/02—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diaphragms, collimators
    • G21K1/025—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diaphragms, collimators using multiple collimators, e.g. Bucky screens; other devices for eliminating undesired or dispersed radiation
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
    • G21K1/06—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diffraction, refraction or reflection, e.g. monochromators
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K7/00—Gamma- or X-ray microscopes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/611—Specific applications or type of materials patterned objects; electronic devices
    • G01N2223/6116—Specific applications or type of materials patterned objects; electronic devices semiconductor wafer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G01N23/044—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material using laminography or tomosynthesis
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K2207/00—Particular details of imaging devices or methods using ionizing electromagnetic radiation such as X-rays or gamma rays
    • G21K2207/005—Methods and devices obtaining contrast from non-absorbing interaction of the radiation with matter, e.g. phase contrast

Definitions

  • the embodiments of the invention disclosed herein relate to microscopy systems using x-rays, and, in particular, measurement, characterization and analysis systems using a system of periodic micro-beams to illuminate an object to determine various structural and chemical properties of the object.
  • This disclosure presents systems for x-ray microscopy using an array of micro-beams having a micro- or nano-scale beam intensity profile to provide selective illumination of micro- or nano-scale regions of an object.
  • An array detector is positioned such that each pixel of the detector only detects x-rays corresponding to a single micro- beam, allowing the signal arising from the x-ray detector to be identified with the specific, limited micro- or nano-scale regions illuminated. Sampled transmission images of the object under examination at a micron- or nano-scale can therefore be generated while using a detector with pixels having a larger size and scale.
  • the micro- or nano-scale beams may be provided by producing a set of Talbot interference fringes, which can create a set of fine x-ray micro-beams propagating in space.
  • the array of micro- or nano- beams may be provided by a conventional x-ray source and an array of x-ray imaging elements (e.g. x-ray lenses).
  • both the detector and the object are placed within the same defined "depth-of-focus” (DOF) range of a set of Talbot anti-nodes.
  • the object is positioned on a mount that allows translation in the x- and y- directions perpendicular to the direction of x-ray beam propagation, allowing a "scanned" transmission image on a microscopic scale to be assembled.
  • the object is positioned on a mount that allows rotation about an axis at a predetermined angle to the direction of x-ray beam propagation, allowing the collection of data on a microscopic scale to be used for laminographic or tomographic image reconstruction.
  • additional masking layers may be inserted in the beam path to block a selected number of the micro-beams, allowing the use of less expensive detectors with larger pixel sizes for the remaining micro-beams.
  • the use of a masking layer also allows the use of a detector with enhanced detection efficiency for the remaining micro-beams.
  • Such masking layers may be placed in front of the object to be examined, between the object and the detector, or be designed as part of the detector structure itself.
  • FIG. 1 A illustrates a schematic view of an x-ray imaging system providing an array of micro-beams as may be used in some embodiments of the invention.
  • FIG. IB illustrates a cross-section view of the x-ray imaging system of FIG. 1A.
  • FIG. 2 illustrates the use of a Talbot interference fringe pattern from a 1 : 1 duty cycle absorption grating G used as an array of micro-beams for an embodiment of the invention.
  • FIG. 3 A illustrates a schematic view of the micro-beams, object, and detector as used in some embodiments of the invention.
  • FIG. 3B illustrates a schematic cross-section view of the micro-beams, object, and detector of the embodiment of FIG. 3 A.
  • FIG. 3C illustrates a schematic cross-section view of the micro-beams, object, and detector of the variation of the embodiment of FIGs. 3A and 3B, in which portions of the detector array are active elements and other portions are inactive.
  • FIG. 4 illustrates a schematic view of a microscope system using a beam-splitting grating Gj to generate micro-beams from Talbot interference fringes.
  • FIG. 5 illustrates a cross section of a micro-beam intensity pattern as may be formed using certain beam splitting gratings as used in some embodiments of the invention.
  • FIG. 6A illustrates a view of a pair of phase-shifting gratings as may be used in some embodiments of the invention.
  • FIG. 6B illustrates the effective phase shifts that will be produced by the pair of phase-shifting gratings of FIG. 6 A.
  • FIG. 7 illustrates a view of a ⁇ phase shifting grating as may be used in some embodiments of the invention.
  • FIG. 8 illustrates a schematic view of a microscope according to an embodiment of the invention having a mask placed in front of the object under examination.
  • FIG. 9A illustrates a schematic view of the micro-beams, object, and detector of the embodiment of FIG. 8.
  • FIG. 9B illustrates a schematic cross-section view of the micro-beams, object, and detector of the embodiment of FIG. 8.
  • FIG. 10 illustrates a schematic cross-section view of the micro-beams, object, and detector of an embodiment comprising a scintillator detector.
  • FIG. 11 illustrates a schematic cross-section view of the micro-beams, object, and detector of an embodiment comprising a scintillator and a scintillator imaging system.
  • FIG. 12 illustrates a schematic view of a microscope according to an embodiment of the invention having a mask placed between the object under examination and the detector.
  • FIG. 13 A illustrates a schematic view of the micro-beams, object, and detector of the embodiment of FIG. 12.
  • FIG. 13B illustrates a schematic cross-section view of the micro-beams, object, and detector of the embodiment of FIG. 12.
  • FIG. 14 illustrates a schematic cross-section view of the micro-beams, object, and detector of an embodiment comprising a mask at the detector and a scintillator.
  • FIG. 15 illustrates a schematic cross-section view of the micro-beams, object, and detector of an embodiment comprising a mask at the detector and a scintillator and a scintillator imaging system.
  • FIG. 16 illustrates a schematic cross-section view of the micro-beams, object, and detectors for an embodiment comprising multiple detectors.
  • FIG. 17A presents a portion of the steps of a method for collecting microscopy data according to an embodiment of the invention.
  • FIG. 17B presents the continuation of the steps of the method of FIG. 17A for collecting microscopy data according to an embodiment of the invention.
  • FIG. 1 A illustrates a simple embodiment of the invention comprising the formation of an array of micro-beams.
  • An arrayed source 004 comprising an electron emitter 011 that produces electrons 111 that bombard a target 1000 comprising a region 1001 containing structures of x-ray generating materials 704.
  • four material structures 704 that are sub-sources of the x-rays are shown arranged in an array, although the target may comprise any number of source points and, of these source points, any number may be used.
  • these x-rays 888 enter an x-ray optical system 3300 that converts the waveform into focused x-rays 888-F that form an image of the x-ray array region 1001 at a predetermined region 2001 in space.
  • Such an optical system may be a simple x-ray focusing element, such as a capillary with an inner quadric surface, or a more complex multi-element imaging system.
  • the image will comprise four spots 282-F, each having a diameter related to the size of the original x-ray generating source point and the magnification of the optical system 3300, and having a length defined by the depth-of-focus of the optical system, generally related to the x-ray wavelength and the square of the numerical aperture (NA) of the
  • FIG. IB illustrates a cross section view of the converging x-ray field 888- F, showing the formation of micro-beams 888-M at this point in space.
  • the micro-beams 888-M will illuminate the object at specific spatially defined points 282-F, having a diameter of the micro-beam 888-M, which is determined by the size of the original x-ray source point, the x-ray wavelength, and the properties (NA, Magnification) of the optical system 3300.
  • the x-rays detected by each pixel are therefore provided by only one micro-beam.
  • the entire signal generated therefore represents the x-ray transmission of only the much smaller illumination spot 282-F.
  • a detector pixel as large as 25 microns may provide information about only the single micron diameter spot when the pitch between micro-beams is larger or equal to the detector pixel pitch.
  • Such a system will produce a set of arrayed points from the detector representing sample points at each micro-beam. For some applications, this sampling of the x-ray transmission through an object may be sufficient. In other cases, the relative position of the object and the array of micro-beams may be scanned in x- and y- dimensions to produce a scanned "map" of the object. Since each data point represents the information produced by a smaller micro-beam, a high-resolution image using a lower-resolution pixel detector can be achieved. Such scanning techniques for structured illumination have been additionally described in co-pending U.S. Patent Application No.
  • the above example presents one way to form an array of micro-beams using an arrayed x-ray source and imaging optics. Although functional for demonstrating the principle, such an approach is limited by the field of view of the x-ray optical system, and various embodiments of the invention may use any number of techniques that create an array of micro- or nano-scale x-ray beams used for illuminating an object.
  • Talbot interference fringes can be a highly efficient method of directing x- rays into an effective array of micro-beams.
  • the effective lateral dimension of the Talbot anti-nodes (typically defined as regions of constructive interference) can, using the appropriate beam-splitting grating to establish the fringes, be made to be very small, as small as 20 nm, while the overall interference field of the Talbot interference pattern can cover an area of several cm 2 .
  • a Talbot interference pattern when used to illuminate an object under investigation in transmission, provides an array of discrete micro- or nano- probes that can be detected and analyzed using an array detector.
  • each pixel is detecting transmitted x-rays from a single one of the micro-beams. This allows the advantages of decoupling the illumination spot size and the pixel dimension to be achieved, and the Talbot interference phenomenon allows an array of effective micro- beams to be formed over a large area.
  • Talbot interference fringes using a structured x-ray source have been the subject of other Patent Applications by the inventors of the present Application, including Ser. Nos. U.S. 14/527,523, US 14/700, 137, 14/712,917, US 14/943,445, and 15/173,711, all of which are hereby incorporated by reference.
  • Talbot interference has been used for lower resolution imaging, and in particular, for phase contrast imaging, for some time (See, for example, Atsushi Momose, Wataru Yashiro, and Yoshihiro Takeda, "X-Ray Phase Imaging with Talbot
  • Such systems typically use a diffractive grating (often a phase-shifting grating) to produce the Talbot interference pattern, and then analyze the resulting pattern with a second grating and/or an array x-ray detector.
  • a diffractive grating often a phase-shifting grating
  • FIG. 2 illustrates a cross section of representative Talbot interference pattern generated by an absorption grating G having a 50/50 duty cycle with a pitch p when illuminated by a plane wave.
  • the fringes in this illustration are adapted from Fig. 19(a) of section 9.3, "Phase Contrast Imaging", in Elements of Modern X-ray Physics, Second Edition", Jens Als-Nielsen & Des McMorrow (John Wiley & Sons Ltd,
  • interference fringes are generated behind the absorption grating. Self-images of the grating with pitch p and a 50/50 duty cycle occur at the Talbot distances D T , given by
  • n is an integer
  • ⁇ is the x-ray wavelength.
  • the darker regions, where destructive interference occurs, are generally called “nodes” of the interference pattern, whereas the bright regions of constructive interference are generally called “anti-nodes” of the interference pattern.
  • the Talbot interference pattern can, with the suitable selection of a beam-splitting grating with micron-scale features, produce an interference pattern of bright anti-nodes with a corresponding micron-scale for the anti- node dimension.
  • Fringe patterns at various fractional Talbot distances may be inverted in bright and dark fringes, and the size of the bright (anti-node) fringes at various fractional Talbot distances may actually be smaller than the size of the original grating features. These anti-nodes may therefore serve as the multiple micro-beams used for illuminating an object.
  • Placing the object 240-W and the detector 290 having a pixel 291 within this predetermined anti-node region allows the signal from a much larger pixel 291 to represent the transmission of the much smaller region 282 where the anti-node illuminates the object.
  • the pattern shown in FIG 2 represents a non-divergent Talbot
  • the Talbot pattern will be comprise x-rays which are diverging from a common x-ray source.
  • the beam splitting diffraction grating used to form the Talbot pattern may be a phase grating of low absorption but producing considerable x- ray phase shift of either ⁇ 12 or ⁇ radians, or some other specified or predetermined value such as an integer multiple of ⁇ 12.
  • These gratings may also comprise one-dimensional or two-dimensional grating patterns.
  • these probe sizes can be as small as 20 nm with the appropriate selection of a suitably fine beam-splitting grating.
  • x- and y- dimensions allows the micro- or nano-scale probing beams to be moved over the object so that a complete high resolution "map" of the transmission of the object may be obtained with a relatively lower resolution detector.
  • FIGs. 3A and 3B A schematic of an embodiment as may be used with any micro-beam forming system is illustrated in FIGs. 3A and 3B.
  • the object 240 to be examined is illuminated at an array of discrete interaction locations 282 also having pitch p w .
  • the x-ray beam pitch in x- and y- is the same and equal to p w , but other embodiments in which the pitch in x- and y- dimensions are different may also be used. Differences in pitch may also be due to divergence properties of the Talbot pattern.
  • FIG. 3C illustrates the use of a detector 290- A, in which active pixels 291-P and inactive areas 291-A are both present in the detector to select only certain micro-beams for detection.
  • the position of the object can be scanned in x- and y-dimensions perpendicular to the direction of propagation of the micro-beams using a position controller 245, and the transmitted x-rays 888-T resulting from the interaction of the micro-beams and the object can be detected by an array detector 290.
  • the array detector 290 has a pitch p 3 which, in this example, is also equal to p w . This means that the detector will be aligned such that each pixel of the array detector will be positioned to collect only x-rays corresponding to a single micro-beam.
  • p 3 which, in this example, is also equal to p w .
  • the object can then be scanned in x- and y-coordinates. This produces "maps" in parallel of the properties of the object, but the range of motion can be reduced to only correspond to the pitch of the micro-beams (although some overlap between scanned areas may be appropriate to provide a relative calibration).
  • the "maps" generated by each pixel may then be stitched together digitally to produce a large-scale "macro-map" of the object properties, while reducing the corresponding data collection time by a factor related to the number of micro-beams (e.g. up to a factor of 10 4 ).
  • limited angle adjustment of the object may also be added to the motion protocol, as long as the interaction of x-rays with the region of interest in the object as well as the corresponding detector pixel both remain within a region defined by the depth-of-focus for all of the multiple micro-beams.
  • a rotation stage 248 to achieve this purpose has also been illustrated as part of the mount for the object 240 in FIG. 3 A.
  • a 5-axis mount, or a goniometer may be used to allow translation and rotation from the same mounting system.
  • the object may remain stationary, and mechanism forming the Talbot fringes (along with the aligned detector) may be translated or rotated relative to the object.
  • the periodic Talbot pattern may be formed by any of the means as described in the previously cited references and Patent Applications, one innovation that has been shown to enable greater x-ray power employs an x-ray source patterned according to a periodic pattern A 0 .
  • FIG. 4 illustrates an embodiment having the configuration shown in FIGs. 3 A and 3B, but in which the x-ray micro-beam array 888-M is formed using such a periodic x-ray source to generate a Talbot interference pattern.
  • the x-ray source 002 comprises an electron beam 111 bombarding an x-ray target 100 comprising a region 1001 comprising structures 700 comprising x-ray generating material embedded in a substrate 1000.
  • the structures 700 as shown are uniform elements of size a arranged in a periodic 2-D pattern with period po. When bombarded with electrons 111, these produce x-rays 888 in a periodic pattern with period po.
  • the structures 700 comprising x-ray generating material may comprise a plurality of discrete finer microstructures.
  • the x-ray generating structures may typically be arranged in a periodic pattern in one or two dimensions.
  • X-ray sources using such structured targets are described more fully in the U.S. Patent Applications X-RAY
  • the detector 290 is shown as having an array Go with a period ps equal to p w , so that each micro-beam is actually uniquely detected by one detector pixel. However, as discussed above, the detector 290 is aligned such that each detector pixel corresponds to x-rays from only a single micro-beam. To facilitate this, the detector may additionally have a positioning controller 255 to align the detector pixels with the individual micro-beams.
  • the position of the object 240 to be illuminated by the array of micro-beams having a pitch p w is placed at a further distance D from the beam-splitting grating G ⁇ 210-2D.
  • the geometry of the arrangement should satisfy the conditions:
  • This configuration is called the Talbot-Lau interferometer [see Franz Pfeiffer et al., "Phase retrieval and differential phase-contrast imaging with low-brilliance X-ray sources", Nature Physics vol. 2, pp. 258 - 261, 2006; and also Described in US patent 7,889,838 by Christian David, Franz Pfeiffer and Timm Weitkamp, issued Feb. 15, 2011], and has been previously demonstrated using a uniform x-ray source and a masking pattern to create the x-ray source array.
  • the arrayed x-ray source may also be provided in some embodiments using a uniform x-ray material and a masked grating that allows x-rays to emerge only from specific points arranged in an array of dimension a and period p ⁇
  • the arrayed x-ray source disclosed above may have considerable advantages over such prior art systems, as the use of discrete sources allows all generated x-rays to contribute to the image forming process.
  • An arrayed x-ray source may also be provided by selective bombardment of an x-ray generating material using a patterned electron beam. Such sources have been described in more detail in the previously cited U.S. Patent Applications, incorporated by reference herein.
  • the x-ray energy spectrum of the micro-beams may be limited by the use of x-ray filters (or other means known to those in the art) to limit the x-ray bandwidth.
  • the system of FIG. 4 is shown using such a filter 388 to filter the x-rays 888 produced by the x-ray source 002 before they encounter the beam splitting grating 210-2D. This may allow better interference contrast to be achieved.
  • having the average x-ray energy E 0 be between 5 keV and 100 keV, and using an x-ray filter to produce an energy bandwidth of E 0 ⁇ 10% or E 0 ⁇ 15%, may be desired.
  • the contrast between regions of greatest intensity (generally the center of the micro-beams) and the darkest intensity (generally exactly between micro-beams) is preferred to be at least 50%, but signals obtained with a contrast of more than 20%, even 10% in some cases, may be acceptable.
  • FIG. 5 illustrates a simulated example of a portion of a two-dimensional x-ray intensity pattern that may be created using Talbot interference fringes. If the beam- splitting grating has matching periods in x- and y-dimensions, a pattern such as that shown in FIG. 5 can be replicated at the various "depths of focus" regions of the Talbot fringes.
  • the beam-splitting grating may be any number of phase-shifting patterns or, in some embodiments, be formed using a pair of gratings. Typical combinations of phase shifters may use 0, ⁇ /2, or ⁇ radian phase shifts in various regions of the grating. Combinations of 1-D patterns or 2-D patterns may also be used.
  • the grating G ⁇ shown in FIG. 4 may be replaced with a pair of gratings GA and B mounted together.
  • Table I shows the various transmission values and phase shifts that may be used for such a combination of 50/50 duty cycle gratings.
  • the values for t and ⁇ represent the transmission and phase shifts, respectively, for two portions of each grating.
  • a pair of gratings for Option 1 (two crossed ⁇ /2 phase shifting gratings), in which the pitch p a for GA is the same as p > for G B , is shown in FIG. 6A, and the result of the crossed gratings is shown in FIG. 6B.
  • Other options using ⁇ phase shifts can produce Talbot patterns having a pitch at 1 ⁇ 2 the pitch of the ⁇ /2 phase shifting gratings.
  • Some of these configurations may also be fabricated using a single grating.
  • other 1-D or 2-D periodic patterns of ⁇ or ⁇ /2 phase-shifts and/or absorption gratings as described in the previously mentioned patent applications and the other Talbot references mentioned in this Application, may also be used.
  • the distance D between the grating and the object should correspond to one of the fractional Talbot distances, i.e.
  • n is a non-zero integer.
  • the suitable value of n may be different if the grating is an absorption grating, a ⁇ phase-shifting grating, or a ⁇ /2 phase-shifting grating.
  • this distance may be generalized to
  • the detector pitch will be matched to the pitch of the multiple Talbot fringes so that each pixel is positioned to only detect x-rays emerging from the interaction of the object with a single micro-beam, and the cross-talk between pixels due to neighboring micro-beams is minimized. Then, the data collection and final reconstruction of the "map" of the properties of the object may proceed, knowing that the distinct signals from each pixel need not be further deconvolved.
  • detector pitches that are integer fractions of the pitch of the micro-beams (e.g. a 3x reduction in pitch, which would indicate 9 pixels are present to detect the x-rays corresponding to each micro-beam) may also be used. This may offer some advantages if the x-rays being detected have some spatial structure, for example if the desired x-ray signal is related to small-angle scattering from the object. Then, certain pixels of the detector can be aligned to detect only the scattered x-rays, while the non- scattered beam may be collected by a different pixel, or simply blocked by a blocked pixel.
  • a detector pixel that is larger than the pitch of the micro-beam may be used.
  • the detector may therefore be less expensive, and yet still produce a "high resolution" signal (since the spatial resolution is determined by the interaction volume of the Talbot fringe and the object, not the detector pixel size).
  • One disadvantage of this technique is that only 1 out of 4 micro-beams is used for detection, and the other micro-beams are blocked. With a larger pixel, greater detection efficiency may be achieved for the micro-beams that are detected.
  • FIGs. 8 - 15 illustrate the use of larger pixels in some embodiments of the invention.
  • FIG. 8 illustrates a schematic of an embodiment of a system similar to that of FIG. 4, but in which a mask 270 with a number of apertures 272 has been placed in front of the object 240 to block a certain number of micro-beams. As illustrated, 3 out of every 4 micro-beams are blocked, with only 1 beam out of each 4 beams proceeding to illuminate the object and then be detected by the detector. This means that if the pitch of the x-ray beams at the mask is p w , the pitch of the beams illuminating the object is 2p w .
  • the detector pitch p D may therefore be set to be equal to 2p w as well, larger than was used for the configuration in FIG. 4. As illustrated, 3 of 4 beams are blocked, but any number of beams may be blocked according to any number of predetermined patterns for various
  • FIG. 9A and 9B illustrate such an embodiment in more detail, presenting illustrations similar to those of FIGs. 3A and 3B. As can be seen by the comparison with FIGs. 3 A and 3B, because only a certain number of micro-beams are used, the pitch of beams at the detector is substantially larger, and a less expensive detector 290-L with a larger pixel size may be used.
  • the x-ray detector is presented as a direct array detector, generating an electrical signal in response to the absorption of x-rays.
  • Some embodiments may use direct flat panel detectors (FPDs) such as the Safire FPD of
  • CMOS complementary metal-oxide semiconductor
  • Some embodiments may use energy resolving array detectors.
  • the detector may use scintillators that emit visible or ultraviolet light when exposed to x-rays.
  • the active x-ray detection region (the detector sensors) may be defined, for example, by providing a scintillator such as cesium iodide doped with thallium (Csl: Tl) or by providing a detector with a uniform coating of scintillator with a masking layer of high Z material, for example, gold (Au), on top.
  • FIG. 10 illustrates a variation of the embodiment of FIG. 9B, but using a detector 290-S in combination with a fluorescent screen or scintillator 280.
  • the scintillator 280 comprises a material that emits visible and/or UV photons when x-rays are absorbed, and the detector 290-S detects those visible and/or UV photons.
  • Typical scintillator materials comprise a layer of thallium doped Csl, Eu doped Lutetium Oxide (LU2O3 : Eu), yttrium aluminum garnet (YAG), or gadolinium sulfoxylate (GOS).
  • the scintillator efficiency depends upon the fraction of x-rays absorbed by the scintillator and the amount of light produced by the scintillator. For high resolution, the lateral spread of light within the scintillator should be minimized and this often necessitates use of a thin scintillator which may limit x-ray absorption and hence detection efficiency.
  • the spatial resolution is defined by the dimensions of the micro-beams 888-M instead of the detector pixel size. This allows a larger pixel and thereby a thicker scintillator material with higher efficiency to be used, since every photon generated from the larger pixel will be known to have originated from a predetermined micro-beam.
  • FIG. 11 illustrates an additional variation on a system using a scintillator, in which the visible/UV light 890 from the scintillator 280 is collected by a visible/UV optical system 320 and imaged onto a detector 290-SI.
  • the visible/UV optical system may comprise optics with additionally magnify the image of the scintillator.
  • the electronic detector need not comprise a high resolution sensor itself, and less expensive commercial CCD detectors or complementary metal- oxide- semi conductor (CMOS) sensor arrays with, for example, 1024 x 1024 pixels, each 24 ⁇ x 24 ⁇ square, may be used.
  • CMOS complementary metal- oxide- semi conductor
  • Thicker scintillators may also be used in some embodiments having relay optics, increasing sensitivity.
  • detection is limited to the field of view collected by the x-ray optics, which may in some cases be only on the order of hundreds of microns. Collecting data on larger areas can only be accomplished if images are "stitched" together from several exposures.
  • FIGs. 12, 13A and 13B represent an additional embodiment in which a masking structure 297 with apertures 292 is placed between the object 240 and the detector 290-M.
  • a masking structure 297 with apertures 292 is placed between the object 240 and the detector 290-M.
  • all available micro-beams 888-M illuminate the object 240, but a masking layer 297 made of, for example, gold (Au), prevents 3 out of every 4 beams from entering the detector 290-M.
  • This also allows detector 290-M to have a larger pixel, again reducing cost for direct detectors and, for embodiments using scintillators, increasing potential detector efficiency.
  • FIG. 14 illustrates an additional variation of the embodiment of FIGs. 10, 11 A and 1 IB, but with the detection of x-rays achieved using a thicker scintillator 280-S and a visible/UV light detector 290-S.
  • FIG. 15 illustrates an additional variation on a system using a scintillator, in which the visible/UV light 890 from the scintillator 280 is collected by a visible/UV optical system 320 and imaged onto a detector 290-SI.
  • scintillators as illustrated in FIGs. 10, 11, 14, and 15 are shown as comprising uniform layers of scintillator, embodiments using patterned scintillator material, in which scintillator material is placed only over a portion of the pixel, may also be used.
  • the selective placement of scintillator material over portions of the detector may be used as an alternative to the use of a masking layer to select certain micro- beams for detection.
  • Detectors with additional structure within each pixel may also be employed as well. For example, if the typical detector pixel is 2.5 microns by 2.5 microns (an area of 6.25 micron 2 ), but the micro-beam diameter is only 1 micron, a detector pixel with a central "spot" of scintillator material slightly larger than 1 micron and positioned to correspond to the position of the micro-beam may be created. With this configuration, all the x-rays from the micro-beam should be detected, while reducing the detection of scattered or diffracted x-rays that would otherwise cause spurious signals if the full area of the detector pixel were to be used.
  • pixels in which detector structures (such as scintillator material) are only positioned on the outer portion of the pixel, for example, to only detect x-rays scattered at small angles while not detecting the directly transmitted beam, may also be used for some embodiments.
  • the mask 297 in FIG. 13 and 14 is shown as displaced from the scintillator 280, some embodiments may have the mask 297 directly deposited onto the scintillator 280. Other embodiments for patterned scintillators may be known to those skilled in the art.
  • These inactive regions may also be regions transparent to x-rays, allowing the use in some embodiments of multiple detectors.
  • each detector is positioned to detect only a selected number of the x-ray beams. This may be done by using a detector with pixels designed to detect only a predetermined number of the beams, while allowing other beams to pass through the detector.
  • the first detector 290-1 is an array detector with a pixel sized to detect all the transmitted x-rays corresponding to a single micro-beam, transmissive regions between the pixels. Micro-beams incident upon these transmissive regions then pass through the detector 290-1, and fall onto a second detector 290-2 with pixels aligned to detect these alternative x-ray micro-beams.
  • the first detector 290-1 may be transmissive over the entire region to high energy x-rays and the first detector 290-1 is used to detect the lower energy x-rays while the second detector 290-2 is used to detect higher energy x-rays.
  • Such a configuration may include two, three, or more detectors, depending on how many pixels are activated in the first detector and how many micro-beams are allowed to pass through the first detector to be detected or pass through the second detector.
  • the advantage of this approach over the masking approach is that each x-ray micro-beam is eventually detected and can contribute to the final collected data set.
  • FIGs. 17A and 17B The process steps to form an image using micro-beams according to an embodiment are represented in FIGs. 17A and 17B, and are described below.
  • a region of space in which the object will be examined by an array of micro-beams is determined.
  • This region may be a region bounded by the "depth of focus" discussed above for the micro-beams, or may be defined as a region related to a fraction of the Talbot distance D T for a given Talbot pattern, or by any criteria suitable to the measurements desired.
  • an array of micro-beams having a pitch p is formed in the predetermined region.
  • Such micro-beams may be formed by any of the disclosed methods, including by using an x-ray imaging system or by using Talbot interference phenomena.
  • this region may be defined as a region with a length related to a fractional Talbot distance, e.g. l/S D T or 1/16 D T .
  • the micro-beams within this region may have a lateral pattern in the form of an array of circular beams or beams with a square or rectangular profile.
  • the array of micro- beams will generally be propagating in a single direction (generally designated the "z" direction), with a pitch p between micro-beams in the directions orthogonal to the propagation direction (the “x" and "y” directions) being 20-50 micrometers or less.
  • this step may also be used to insert an additional mask that removes some of the micro-beams, as discussed above.
  • the next step 4230 is the placement of a detector having a pixel pitch p d equal to a non-zero integer multiple of the micro-beam pitch p.
  • the detector may be any of the detectors as described above. This sensor portion of the detector is placed in the region selected in the previous step. There is some flexibility in the exact positioning of the detector, as long as each pixel of the detector generates a signal corresponding only to a single micro-beam (without cross-talk between the micro-beams or detector pixels). Generally, a detector will be chosen where every micro-beam has a corresponding pixel or set of pixels; however, in some embodiments, the detector may only detect a subset of the corresponding micro-beams.
  • a region of interest (ROI) of an object to be examined is placed in the selected region comprising micro-beams as well, between the x- ray source and the front of the detector. This will generally be in proximity to the detector, so that the object and detector are both within a "depth-of-focus" region of the micro-beam.
  • the x-ray beam will either be blocked or turned off while the object is positioned and aligned, and the x-rays turned on after the object has been placed.
  • the x-rays transmitted by each micro-beam are detected by the corresponding pixels on the detector, and the corresponding electronic signals are recorded.
  • These signals may represent x-ray intensity in counting detectors and may also include energy in energy-resolving detectors.
  • next step 4256 a decision on how to proceed is made. If only a single set of datapoints are desired, no more data need be collected, and the method proceeds to the step indicated by "B" in FIGs. 17A and 17B. If, on the other hand, additional data need to be collected to build up a 1-D or 2-D "map" of the properties of the object, the decision tree delivers a request for data from additional positions.
  • step 4260 the relative position of the object and the micro- beams is changed by a predetermined distance in x- and/or y-dimensions, and the method reverts to step 4250, in which data is now collected for the new position.
  • the system will loop through this decision tree of steps 4250, 4256, and 4260 until data have been collected for the entire 1-D or 2-D region designated for examination, at which point the method proceeds to the step indicated by "B" in FIGs. 17A and 17B.
  • the system will determine in steps 4266 and 4276 whether only a 2-D "map" is to be constructed, or if additional information is needed to generate a 3-D representation of the object, using algorithms related to either laminography or tomography.
  • the method proceeds to the final analysis step 4290. If data for a ID or 2D map was taken in the previous steps, the accumulated data is then used with various image "stitching" techniques that are generally well known in the art to synthesize a 1-D or 2-D intensity "map" representing the x-ray transmission/absorption of the ROI of the object.
  • step 4276 a decision on how to proceed is made. If additional data is still required to be collected to build up a 3-D dataset of the properties of the object, the decision tree delivers a request for data from additional angles.
  • the method then proceeds to a step 4280 in which the object is rotated by a predetermined angular increment around an axis at a predetermined angle relative to the z axis, and then the method proceeds to the step indicated by "A" in FIGs. 17A and 17B, passing control back to the loop of steps 4250, 4256, and 4260 to collect a set of data from the x-ray detector at this alternative rotation position.
  • the system will loop through these steps 4250, 4256, 4260 and also 4266, 4276, and 4280 to collect x-ray information at a preprogrammed sequence of positions and rotations until a complete set of data is collected. At this point, after all data collection is complete, the system will then proceed to the final analysis step 4290 to take the accumulated data and, in this case, use various image 3-D analysis techniques that are generally well known in the art, to synthesize a 3-D representation of the x-ray
  • Variations on the method described above may also be put into practice. For example, instead of first executing a loop of data collection in x- and y-dimensions at a fixed rotation position, and then changing the rotation setting to collect additional data, embodiments in which the object is rotated while the x- and y-position settings remain fixed may also be executed. Rotation of the object around the z-axis may also provide additional information that can be used in image tomosynthesis. 5. Limitations and Extensions.

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Abstract

La présente invention concerne des systèmes de microscopie à rayons X utilisant un réseau de micro-faisceaux ayant un profil d'intensité de faisceau à échelle micro- ou nanométrique pour produire un éclairage sélectif de régions à échelle micro- ou nanométrique d'un objet. Un détecteur matriciel est positionné de sorte que chaque pixel du détecteur ne détecte que des rayons X correspondant à un micro- ou nano-faisceau unique. Cela permet d'identifier le signal provenant de chaque pixel de détecteur de rayons X avec la région à échelle micro- ou nanométrique limitée spécifique, éclairée, permettant la génération d'une image de transmission échantillonnée de l'objet à une échelle micro- ou nanométrique, en utilisant un détecteur avec des pixels ayant une taille et une échelle plus élevées. Par conséquent, des détecteurs à rendement quantique supérieur peuvent être utilisés, étant donné que la résolution latérale est produite uniquement par les dimensions des micro- ou nano-faisceaux. Les faisceaux à échelle micro- ou nanométrique peuvent être générés au moyen d'une source de rayons X en réseau ou d'un ensemble de franges d'interférence de Talbot.
EP17810765.2A 2016-06-05 2017-06-02 Procédé et appareil de microscopie à rayons x Withdrawn EP3465182A4 (fr)

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US15/173,711 US10401309B2 (en) 2014-05-15 2016-06-05 X-ray techniques using structured illumination
US201662401164P 2016-09-28 2016-09-28
US201662429587P 2016-12-02 2016-12-02
US201662429760P 2016-12-03 2016-12-03
US201762485916P 2017-04-15 2017-04-15
US15/605,957 US10352880B2 (en) 2015-04-29 2017-05-26 Method and apparatus for x-ray microscopy
PCT/US2017/035800 WO2017213996A1 (fr) 2016-06-05 2017-06-02 Procédé et appareil de microscopie à rayons x

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