Nuclear Instruments and Methods in Physics Research A 347 (1994) 170-176 North-Holland

NUCLEAR INSTRUMENTS & METHODS IN PHYSICS RESEARCH
Section A

The future of X-ray holography
1. McNulty
Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439, USA X-ray holography is a promising technique for high resolution study of biological, microelectronics and materials science specimens . It offers absorption and phase contrast, it is amenable to flash sources, and it is capable of three-dimensional imaging when coupled with tomography . Soft X-rays are suited to microscopy of thin organic specimens and wet biological objects such as subcellular organelles . Major advances in X-ray sources, optics, and detectors have made possible Gabor and Fourier transform holography with 50 to 60-nm transverse resolution using 350-600 eV photons; 100-nm depth resolution by holographic tomography has recently been demonstrated . X-ray holography at higher energies (1-4 keV) may be feasible soon using third-generation synchrotron sources. These methods might profitably be used to investigate denser objects than are accessible to soft X-rays, for example defects in microcircuits and adsorbates in zeolites . The future is likely to see progress in X-ray holography over an increasing range of photon energies, with elemental and chemical specificity, and with three-dimensional resolution below one micron . 1. Introduction The last decade has seen X-ray holography progress from proof-of-principle experiments disappointingly shy of expectation, to dramatic results with biological and artificial test objects at an order of magnitude better resolution than those obtainable using visible light. This progress has largely taken place with soft X-rays in the "water window" between the oxygen K-edge at 532 eV and the carbon K-edge at 284 eV [1]. Soft X-rays offer suboptical resolution and lower radiation dose than electron probes for hydrated biological objects, and thus are well suited to the study of thick, unstained and possibly living specimens under physiologically natural conditions [2]. High brightness undulators at the newly-commissioned third-generation Advanced Light Source (ALS) storage ring [3] will enable soft X-ray holography experiments to be performed at higher resolution, with the potential for time-resolved experiments . In the near future, third-generation sources of higher energy X-rays at the APS, ESRF and SPRing-8 storage rings [4] will, for the first time, allow X-ray holography in the intermediate energy (1-4 keV) region . These more penetrating photons are likely to be useful for imaging denser, thicker microelectronics and materials sciences specimens, and for phase contrast imaging of biological objects [5]. Holographic imaging involves two steps. A recording is first made of the interference pattern that results when a reference wave is mixed with the wave scattered by an illuminated object. The object wave is then reconstructed from the interference pattern or hologram. The hologram intensity I is the squared sum of the complex amplitudes of the object and reference waves I = a. a* + a, a* + a, a* + a, a* , where a. and a r are the object and reference wave amplitudes . Re-illumination of the hologram by a, produces image terms proportional to ao and a** , and two noise terms representing the diffraction patterns of the object and the reference source. Reconstructing the object wave from the image-forming terms with minimal added noise is the challenge in refining a particular holographic technique from a novel demonstration to a practical tool . Holography is a coherent process in which the object wave amplitude is, in principle, fully recoverable . This feature resolves the famous phase problem of crystallography, enables image formation by both absorption and phase contrast, and is the basis for three-dimensional (3D) wavefrom reconstruction. Elemental specificity is possible in the X-ray region due to the existence of absorption edges at the electronic binding energies of atoms [1]. Chemical selectivity in the vicinity of absorption edges is also possible ; chemical contrast has been shown in recent X-ray microscopy experiments [6]. Phase contrast, which is sensitive to the real part of the object's refractive index, can be exploited to obtain information about membranes, interfaces and regions of anomalous dispersion that are inaccessible to methods based solely on absorption . The thrust of this paper is to review the origins, current status, and methods of X-ray holography and to extrapolate some of the directions it will take in the near future . These include techniques for obtaining 3D information, extension to higher energies, and the use of flash sources. 2. Historical background The first X-ray hologram, of a thin wire, was unintentionally recorded by Kellstr6m with Al-K (1 .5 keV) X-rays

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in Phys. Holography was unknown until Gabor invented it in 1948 as a lensless means of high resolution imaging in order to circumvent the aberrations of electron optics of the day [8]. a plane wave both illuminates the object and provides the reference wave [8]. tunable x-radiation available. It became evident that synchrotron-based sources could provide the requisite coherent flux [19.I. El-Sum was able to reconstruct Kellstr8m's hologram with visible light [10] . 1.17. thin film deposition and precision metrology. surface polishing.1 % BW) Fig. Soft X-ray bending magnet and undulator sources at the Photon Factory. Currently.6-nm X-rays and 200-ps exposures [28] . but it required a strong point reference source. 100 lasers held promise for the future [21] . and others [11-14] subsequently explored the theoretical foundations for high resolution X-ray holography . the brightest continuous sources of partially coherent. Winthrop. Historically. but a fine-grained detector was necessary to obtain high resolution images . and high resolution detectors did not yet exist. The spatial frequencies of the Fresnel fringes in a Gabor hologram extend to the frequency limit of the object . The two approaches are complementary and offer a different mix of capabilities . at least until XRLs become competitive. The resolution of this technique depends on the detector resoluVl . NSLS and LURE have since been used to record Gabor and Fourier transform X-ray holograms [2227]. Progress in two-dimensional imaging resolution by X-ray holography (circles) as a function of estimated source brightness. X-ray Gabor holograms are recorded on high resolution X-ray resists. The Fourier transform holography geometry [12.1% bandwidth. McNulty /Nucl. Extension of Gabor's approach to the X-ray region had the advantage of not requiring X-ray optics. The Livermore XRL was used to make Gabor holograms with 20 . The most significant work has been realized using undulators.Ô O 001 - Source Brightness (ph/s/mm 2/mrad2 /0 . In the Gabor geometry. because bright enough X-ray sources.20] and that short-pulse Fig. The next few years saw modest results by Giles [15] and Bjorklund [16] with vacuum-ultraviolet light. If this trend is extrapolated to a resolution of 10 nm. Res. then reconstructed optically with ultraviolet light or numerically by computer . 105 107 109 10 11 1013 10 15 1017 1019 1021 . 2) . State of the art Sub-100-nm holography has been demonstrated with soft X-rays using both the Gabor in-line and the Fourier transform methods (Fig . Instr. Baez envisioned using shorter wavelength radiation and proposed ways to construct a holographic X-ray microscope [9]. have a spectral brightness of 10 17 to 10 18 photons/ s/mm 2 / mrad2 per 0. Progress was slow. COHERENCE ô ô fN w . efficient wide-aperture X-ray optics. the resolution has improved approximately with the fourth power of the brightness (dashed-line fit to data). from 1952 to the present [10. such as the X1 soft X-ray undulator at the NSLS and undulators planned for the ALS and APS storage rings. 1 shows the downward trend in imaging resolution by X-ray holography with increasing source brightness. the brightest soft and hard X-ray sources. it appears that one would require a time-averaged source brightness of 10 21 (in these units)! 3. Undulators. This situation changed dramatically with the advent of high brightness X-ray sources on synchrotron storage rings and demonstration of the first X-ray lasers (XRLs) . Gabor in-line (a) and Fourier transform (b) holography geometries . there still was no X-ray source with sufficient coherent flux to form holograms with a resolution beyond that obtainable with visible light. Leith. Concurrently. since El-Sum . 2 . Consequently.13] was hailed as the solution because it decoupled the hologram resolution from the detector resolution. Although Gabor's experiments were conducted in the optical region. are still the sources of choice for X-ray holography experiments . however. then Reuter and Mahr [18]. X-ray energies used in the work shown are between 300 and 1500 eV . Stroke. A 347 (1994) 170-176 in 1932 [7]..22-281 . About this time.18. Fig. magnified by atomic force or transmission electron microscopy (TEM). many of the difficulties of making diffraction-limited diffractioe and reflective X-ray optics were overcome by advances in microfabrication technology. Significant advances were not made until Aoki and Kikuta [17]. and Meth. This progress was paralleled by the introduction of sensitive electronic array detectors and high resolution resists for X-rays . recorded and reconstructed X-ray holograms to a resolution of a few microns. In both cases.

20].27]. Because the object wave has approximately the same curvature as the reference wave. fabricated by the same method. Joyeux and Polack recorded Gabor holograms of diatoms with 10 nm X-rays at LURE and optically reconstructed them to submicron resolution [24] . demanding considerable dynamic range of the detector. Jacobsen and others obtained Gabor holograms at the NSLS of dry rat pancreatic zymogen granules. Res.27]. Effective use can thus be made of a multimode beam . Considerable effort must be invested to achieve the necessary stability for good fringe visibility . This avoids the twin-image problem. However. whereby the out-of-focus object image from the last term in Eq. provided that the object and reference are sufficiently separated such that the reconstruction of the first and last two terms in Eq . Because the lower spatial frequencies in the object are encoded near the hologram center. TEM hologram readout requires coating of the resists with metal for contrast. and Meth. one to either side of the optic axis . As the spatial coherence width must only be as large as the object under study. A CCD camera was used to record holograms of the test patterns . which slows the turnaround from hologram recording to reconstruction . the field of view can be as large as the beam size. In Fourier transform X-ray holography. a spherical reference wave originating from a point near the object is made to interfere with the illumination scattered by the object [12. In high resolution Fourier transform holography. this beam-splitting geometry was suggested as a way to generate a strong reference wave adjacent to the object [14. lending a high-pass-filtered appearance to the reconstruction . In X-ray experiments. fabricated by e-beam lithography. McNulty/Nucl. Lindaas [30] has built a wide-field. The imaging resolution is limited by the precision with which the reference wavefront is known and the angular extent over which the hologram is recorded . A 347 (1994)170-176 tion and means of readout. scanning atomic force microscope to read out the exposed resists directly without the need for metallization. Although soft X-ray zone plates with finest zone widths of 25 nm have now been made [31]. Being spatially separated. which permits additional development if desired and should reduce aberrations. this limit will probably not decrease significantly over the next few years. in Phys . The object was situated a few microns from the first-order focus of the zone plate such that it was illuminated by the zeroth and other diffraction orders . and hydrated fixed hippocampal cells with 2. PMMA resist was used to record the holograms. Moreover. This provides a swift route to numerical reconstruction .13]. a monochromaticity of a few hundred). The reference wave and object illumination were derived with a Fresnel zone plate in Fourier transform holography experiments with 3.0 to 2. optical distortions in the TEM used to read them are believed to have limited the reconstructed resolution . these may be blocked by the stop. The NSLS X1 undulator provided the coherent X-ray beam . The CCD (a 576 X 384 array of 23 p. Instr. detector size. Because of the low fringe frequencies. A disadvantage is that the intensity is very strong at the center and weak near the hologram periphery. which were numerically reconstructed to a resolution of 60 nm [25. the Fourier transform geometry is ideal for digital hologram recording with coarse-grained electronic detectors such as CCDs . no prefocusing.m-square pixels) was cooled with liquid nitrogen for low dark current and was coated with a thin phosphor layer to convert incident X-rays to visible light for better quantum efficiency . critical-point dried Chinese hamster ovarian cells. the hologram fringes are of low spatial frequency at the expense of object field of view . the relative strength of the object and reference waves can also be balanced for optimum fringe contrast . no optics. and optical path differences will permit . and minimal alignment are required in the recording step . was made of gold and had a finest zone width of 50 nm . the specimen position in relation to the reference source must be . it is usually necessary to employ a beam stop to attenuate this bright central peak (principally the zerothorder beam) to avoid detector saturation . leading to better image resolution . Gold patterns with 50-125 nm features. One must also deal with the "twin-image" inherent to in-line holography. this geometry may be best for high power sources due to the large area over which the hologram intensity is distributed.172 I. The digitally-recorded Fourier transform holograms were reconstructed by computer to the 60-nm diffraction limit of the zone plate lens that formed the reference source . it should be possible to improve the resolution by extended source compensation [13] and by accounting for nonplanarity of the object illumination in the reconstruction . the reference source size limits the resolution by this technique. The point reference source can be formed with a focusing optic or by a point scatterer. On the other hand. Gabor holography is the most well developed and applied in the X-ray region .4-nm soft X-rays by McNulty [26. off-line processing is necessary to enlarge and read out the hologram. The zone plate. Due to the off-axis location of the reference source with respect to the object. The main advantage of Gabor holography is simplicity : apart from a monochromator to provide sufficient temporal coherence (typically. (1) does not overlap. Twin-image effects can be alleviated by iterative phase retrieval [29] . were used as test objects.5-nm undulator radiation. Information down to 20 nm is indicated in the exposed resists. both primary and conjugate images of the object are reconstructed. (1) overlaps the primary image in the reconstruction . Mechanical and thermal stability of the apparatus during the recording step is crucial in view of the minutes-long exposures currently necessary to obtain X-ray holograms with synchrotron sources. Typical exposure times are several minutes using the X1 soft X-ray undulator. leaving no opportunity for further development. At present. high linearity.

scattered and transferred momenta satisfy Bragg's law k = kmc . much work in optical. Vl. acoustic and microwave holography. (2) to the product of the hologram intensity and a numerical representation of the reference wave . (b) Use of three different incidence angles in holographic tomography to cover wider range in kr to obtain better depth resolution. [22]). The object wave amplitude at the detector is represented in the Fresnel approximation by e . wide-aperture hologram [35] . Although this approach to 3D imaging is well known [36. i. A 347 (1994) 170-176 173 maintained to a precision comparable to the desired resolution. By recording an ensemble of holograms from various angles of incidence. Indeed. Instr. making it difficult to achieve a numerical aperture of more than .l. it will be necessary to go beyond the Fresnel approximation to reconstruct them . has been one. X-rays are scattered weakly at large angles. But because of the small cross-section in matter for coherent scattering. COHERENCE . (a) View in reciprocal space (k x and k. k=2. Holography may be regarded as a scattering process in which the incident. HT can help eliminate speckle that may degrade reconstructions of successive depth planes from a single. If substantially wider-aperture holograms are recorded to reach better resolution. 4. the depth resolution depends on the inverse-square of the numerical aperture of the optical system. the object is sampled over a wider spatial frequency range. Three-dimensional X-ray holography Holography is not by definition a three-dimensional form of imaging despite its popular reputation . (3) limits the range of spatial frequencies that are accessible to the hologram.0. the 3D capability of holographic methods is both tantalizing and opportune. 3a. y) a. as for X-rays. as well as in other types of imaging. This procedure. Reconstructions of digitized 512 X 512-pixel holograms can now be performed by this method in less than a minute on a fast RISC workstation computer .37] and its application to Fig. 3b). easily and rapidly implemented with a fast Fourier transform algorithm. axes shown) indicating the range of accessible spatial frequencies (shaded region) for the scattenng angle NA . respectively. has been successfully used to reconstruct X-ray Gabor and Fourier transform holograms to a numerical aperture of about 0. the largest angle over which fringes in the hologram are recorded .e .or two-dimensional (a notable exception can be found in ref. McNulty/Nucl. "!) = i. y) is the object transmittance. therefore.ks ao(x. (x.tz Az ff 2z [(x-6)2+(y-n)2I) dx dy. in Phys. where a o (x. This limitation can be overcome by recording several holograms of the object from various directions then reconstructing them according to hmographic principles with the effects of diffraction included [34] . The object transmittance is reconstructed by applying the inverse of Eq . as well as nearly all work in the X-ray region. Numerical reconstructions of X-ray holograms to date have mostly been based on digital implementations of the Fresnel-Kirchhoff diffraction integral [32] .I. high depth resolution with a single X-ray hologram .y) and (6. the object and detector must stay stable to within this limit. the object scatters predominantly in the forward direction.kscat' The scattering angle defined by Eq .1 and. giving a larger effective numerical aperture and better depth resolution (Fig. In holography. i7) are space coordinates in the object and hologram planes. In the Gabor case. as shown in Fig.( e. In addition. Nonetheless. This is particularly useful in cases which. One possibility is to use the limited basis set algorithm of Haddad [33] .05. Res. and Meth .rr/. 3. A potential advantage of holographic tomography (HT) over conventional projection tomography is that fewer views should be required because each hologram contains some depth information about the object. and z is the distance from the object plane to the detector .

z) . gallium and arsenic. 130 nm wide and 90 nm thick). Tomographic X-ray analysis of composites is already an active field [43] . z) [40] . At an energy of 3 keV and bandwidth of 0. high resolution optics have also become available for harder X-rays . the APS U5 . with natural elemental and chemical absorption contrast for the heavier elements and phase contrast for the lighter elements.g . zeolites). For instance. L. less dose and through thicker specimens [5]. A 347 (1994) 170-176 the X-ray region has been suggested before [20. Res. and registry of the holograms used in the reconstruction determine the resolution attainable by HT . Instr. copper. although a substantially smaller number of views may be sufficient for sparse objects. The object. Bionta fabricated zone plates made by the sputtered/ sliced tech- and therefore its 3D index of refraction n(x. holography could be used to pinpoint microdefects in 100-nm-wide aluminum interconnects sandwiched between micron-thick layers of silicon within a microcircuit. . there must be enough coherent flux available to record the tomographic ensemble. we can expect enough signal with a beamline efficiency of several percent to record holograms of a 10-micron-cube volume with 10 3 coherent photons/s per 50-nm resolution element. which becomes more restrictive at higher photon energies . y.174 I. We performed a demonstration experiment to explore the feasibility of HT [39]. Using coherent 3 . Intermediate energy X-rays are potentially useful for holographic microscopy of microstructures important to the materials sciences and to the microelectronics sector. Object complexity and the number. The CAD drawing that would necessarily accompany an integrated circuit is such an example. was oriented normal to the beam and rotated such that the bars were in various depth planes . In addition to brighter sources. 100 views to image a 10-wm diameter volume with a depth resolution of 50 nm). it has not been tested with X-rays until recently. phase-shifted by the difference in depth (the other bar served as the reference source). Three-dimensional phase recovery and inverse Fourier transformation were used to recover the object scattering potential F(x. The 1-4 keV range is also attractive for holography of biological specimens. y. The interaction lengths of such X-rays are suited to investigation of dense microscopic objects. The bar is localized in the reconstructions to better than 100 nm in both the transverse and longitudinal directions . Biological structures can have significant phase-shifting yet relatively weak absorptive effects on intermediate energy X-rays . For fixed temporal coherence length 1. these energies could permit imaging with better phase contrast. When the depth resolution per view is insignificant. without disturbing its mechanical or electrical integrity. Misregistration of the holograms due to object rotational errors can be partially corrected a posteriori by aligning the images to an identifiable feature in the object . Holographic tomography may be a practical approach to 3D imaging provided the number of holograms needed to achieve satisfactory depth resolution with an acceptable signal-to-noise ratio and radiation dose can be determined for a given class of objects.1%.5 p. aperture. Numerical reconstructions of a 1-wm segment of one bar were obtained from seven holograms covering an angular range of -45° to +45°. McNulty/Nucl. figure prominently in environmental cleanup research [44] . especially those containing aluminum. Clearly this is impractical for a radiation-sensitive specimen (e . By comparison to soft X-ray and charged-particle probes. 4. incorporation of a priori information about the object into the reconstruction could drastically reduce this number. X-rays coherently scattered by the bars interfered to produce a Young's fringe pattern that is the hologram of one bar. Nondestructive in-situ imaging of imbedded microcircuits is another potential application . nickel.m apart. Fc decreases even more swiftly with A according to F~ =BA3/41C .4] is illustrated in Fig. X-ray holography at these energies might be feasible for the first time . noteworthy for the wide variety of elements in the middle of the periodic table whose K. _ AZ/t> A and the brightness B per unit bandwidth. the number of views required for a densely packed object is equal to the object radius divided by the desired depth resolution . We have shown that the depth resolution can approach the transverse resolution in simple objects with a small number (. we recorded Fourier transform holograms of a microfabricated test object from various illumination angles. and Meth..5 undulator will deliver an anticipated coherent flux of 5 X 10' ° photons/s.10) of holograms provided that the angular coverage approaches 90 °. Additionally.g . the 1-4 keV intermediate energy region has seen comparatively few spatially resolved applications .1] (4) 5. This energy range. y. in Phys. For example. We have also applied an algebraic reconstruction technique [41] that effectively reduces artifact arising from using a limited hologram set. The coherent flux Fc = B(A/2) Z expected at intermediate X-ray energies using several of the brightest existing and planned undulators [3. silicon. z) = . Moreover. Molecular sieves (e . and M absorption edges fall within it. consisting of two parallel gold bars (2. has attracted increasing attention in the past few years [42] ..2-nm X-rays and a CCD camera. used extensively for shape-selective catalysis and adsorption.38]. Owing to the unprecedented coherent flux that will be available from undulators on third-generation storage rings.k2 [ n'(x. Higher energies By contrast to the soft and hard X-ray regions. where B is the spectral brightness per bandwidth t1 A/A.

and Meth . the short pulse duration could allow biological X-ray microscopy that is truly free of radiation damage artifact . Res. is one of the most exciting future prospects. development of 3D flash holography with 10-nm resolution would have dramatic implications for structural biology.1% bandwidth) XRL would make possible an array of X-ray holography experiments that could never be attempted with an undulator. These optics have been used in scanning transmission and fluorescence microscopy experiments near 8 keV [47]. A 347(1994)170-176 175 m 10 12 10 11 1010 _ n=3 NSLS X1 n=5 ALS U3 9 n=5 ô â fn d 9 108 050 10 15 20 25 30 35 40 Photon energy (KeV) Fig. Radiation dose increases like S-z" with the imaging dimension n and resolution 8 [2]. Flash sources Perhaps the greatest challenge facing application of X-ray holography to the life sciences is the problem of radiation damage . Flash sources potentially offer the greatest reward in this regard . Grazing incidence Wolter and multilayer Schwartzschild mirrors. The time for radiation damage to be manifest in living specimens following exposure is much greater. Certainly. Coherent flux at 1-4 keV produced by the NSLS X1 (8 .9 devices must be used because of the lower storage ring energy (2 .L McNulty /Nucl. is around the corner . previously well behind diffractive optics in achieving theoretical resolution limits. and holographic lithography [54] . 3D X-ray holography may be possible with this source if means can be found to record several simultaneous holograms of the specimen with a single pulse. There are sure to be many interesting developments to come . Higher energies are attractive in view of the third-generation X-ray sources due to come on-line soon . their coherent output is still too limited for submicron X-ray holography . To a lesser degree. as compared to 7 GeV for the APS). Down the line. if realizable. The immense number of coherent photons per pulse. The richest rewards of X-ray holography will likely be realized in combination with other methods. Moreover.5 GeV for the NSLS and ALS respectively. suggesting that use of these sources for holography. are now competitive with zone plates in the soft X-ray region and show promise for extension to higher energies . This extremely short pulse (150 fs). ALS U3. Synchrotron sources do not posses the peak brightness necessary to record high resolution flash holograms. To reach above 1 keV. Synchrotron sources are invaluable for developing these applications and for refining the techniques that will be needed to utilize high brightness XRLs . The key to flash X-ray holography will lie in the ability of the source and beam transport optics to deliver sufficient coherent flux to the experiment in a short enough time . high resolution.5 and 1 . a holographic snapshot of the specimen must be captured with low incident intensity in less time than it takes the damage to appear. [49] .0 cm period). 4. Even at this juncture. Nevertheless. but they could be adapted to work at lower energies . While XRLs have steadily improved in brightness and exhibited significant gain at water-window wavelengths [501 since their inception in 1985. 10 14 . it is clear that holography has just begun to find application in the X-ray domain. COHERENCE 6. on millisecond or longer scales . therefore bright XRLs are the only alternative. VI . Yun demonstrated submicron focusing with near-ideal diffractive efficiency using phase zone plates made by X-ray lithography [46] . in Phys. or with high incident intensity in less time than hydrodynamic blurring occurs . Future outlook The potential of X-ray holography has only recently been explored and the many uses to which it could be put are clearly far from exhausted. Instr. To avoid artifact due to irreparable radiation damage.9 and APS U5 . The proposed Stanford soft X-ray free-electron laser [52]. the higher harmonics of the X1 and U3 . An intriguing possibility is atomic resolution by X-ray fluorescence holography with a local reference source [55] . Onset of hydrodynamic blurring scales as the inverse third power of the resolution and is of order 100 ps for a resolution of 50 run [48] . direct-imaging experiments have been conducted with 4. when they become bright enough. for example the gate electrode of a working MOS field-effect transistor. is four orders of magnitude greater than that currently needed to form a single high resolution Gabor [25] or Fourier transform X-ray hologram [26] . high peak brightness (1031 photons/s/mm2/mrad2 per 0.5 undulators [3. nique [45] .41. 7. Other possible applications include interferometric and microdifferential holography [53]. development of holographic optical elements.48-nm X-rays from the Livermore XRL [51]. radiation damage may complicate holography of inanimate but fragile objects.

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