METHOD OF GENERATING A MULTI-DIMENSIONAL IMAGE OF A SAMPLE, METHOD OF CREATING A THREE-DIMENSIONAL V

专利摘要:
dual imaging method and system for generating a multidimensional image of a sample. The present invention relates in part to a method for generating a multidimensional image of a sample that combines different image capture modalities with data analysis capability to identify and integrate the more accurate image features captured by each respective modality for provide reconciled image data of highest accuracy and consistency. a system that can be used to run the method is also included.
公开号:BR112014009093B1
申请号:R112014009093-9
申请日:2012-10-11
公开日:2021-08-17
发明作者:Gustavo Carpio；Timothy Cavanaugh；Boaz Nur；Michael Suhrer
申请人:Ingrain, Inc；
IPC主号:

专利说明:

FUNDAMENTALS OF THE INVENTION
[001] The present invention relates to a method for generating a multidimensional image of a sample. The present invention also relates to a system for generating the multidimensional image of a sample.
[002] Three-dimensional data acquisition and volume visualization through the application of FIB (Focused Ion Beam) cutting has recently emerged as a potential method to acquire, interrogate, and display multidimensional images for various substrate materials. For example, in US Patent No. 6,855,936 and US 7,750,293 B2, certain systems are described that can be used for FIB-SEM (scanning electron microscope) three-dimensional imaging methods. The FIB system can act as a nanoscale scalpel to remove very thin slices of material from a sample, while SEM captures images of the sample structure in each slice. Factors that may limit the widespread use of FIB-SEM-based three-dimensional imaging methods include challenges in implementing fast and accurate image data analysis and image volume generation methods for the images captured with these devices.
[003] In the field of digital rock physics, devices generating computer tomographic (CT) images of rock samples, such as drill chips, have become available and used to analyze rock samples. Such CT imaging devices have been used to produce two-dimensional grayscale images of rock samples. Two-dimensional images can be stacked within a three-dimensional volume. Such grayscale images have been used, for example, as part of an analysis to obtain estimates of petrophysical parameters of the rock sample formed with image, for example, porosity, permeability, shear and volume modulus, and resistivity factor of formation.
[004] The present investigators recognized that it would be beneficial to generate ultra-high resolution multidimensional images of rocks or other materials in combination with powerful automated analytical capabilities for alignment and image corrections to enable accurate and consistent nanoscale analysis of hydrocarbon deposits in rock or other samples. This development can allow quick and accurate understandings of a rock sample, such as in terms of geological phase content and distribution for any individual two-dimensional slices and the three-dimensional volume as a whole without the need for laboratory analysis of the sample and with reduced dependence or need for human or manual analysis as part of the methodology. The present investigators further recognized that there is a need for unique digital image capture and analysis methods that can provide accurate understandings in a short period of time for "tight" or unconventional fine-grained rocks. Tight formations can have extremely low permeability unlike more typical sandstones or other more porous rocks that have been analyzed using digital rock physics. SUMMARY OF THE INVENTION
[005] One aspect of the present invention is to provide a method for generating a multidimensional image of a sample, which includes capturing multiple two-dimensional substrate images of a surface region of the sample with different image capture modalities having different accuracy, and generating a image adjusted using the different images captured.
[006] Another feature of the present invention is to provide a method of creating a three-dimensional volume by simultaneously capturing dual sets of surface electron two-dimensional substrate images and backscatter two-dimensional electron substrate images, and generating a three-dimensional substrate volume from the surface electron two-dimensional substrate images using the alignment of the plurality of backscatter two-dimensional electron substrate images.
[007] A further aspect of the present invention is to provide a method for generating a three-dimensional volume of a sample that includes scanning a surface of a sample containing multiple phases by a primary electron beam generated by an electron source, and recording image data separated based on detected surface electrons and backscattered electrons emitted by the sample during scanning and storing the image data as a double set of image data associated with the scanned surface, remove a slice from the sample and repeat the image capture a plurality of times, and then correcting at least one phase in the images based on detected surface electrons using tags from a different phase that are identified in the images based on detected backscattered electrons emitted by the sample during scanning.
[008] Another feature of the present invention is to provide a method for generating a three-dimensional volume of a sample that includes scanning a surface of a sample comprising kerogen, porosity, and minerals in which pixels are relocated from kerogen to porous space in an analyzed two-dimensional image that was captured based on surface electrons detected using a first mask, and pixels are reallocated from mineral to kerogen on the basis of the analyzed two-dimensional image using a second mask.
[009] Another feature of the present invention is to provide a system for implementing the indicated methods.
[010] Additional features and advantages of the present invention will be set forth in part in the description that follows, and in part will be apparent from the description, or may be learned by practicing the present invention. The objectives and other advantages of the present invention will be realized and attained by means of the elements and combinations particularly pointed out in the description and appended claims.
[011] To achieve these and other advantages, and in accordance with the purposes of the present invention, as embodied and broadly described herein, the present invention relates in part to a method for generating a multidimensional image of a sample wherein the method includes capturing a first two-dimensional substrate image of a surface region of the sample with a first image capture mode, wherein the locations of at least one material in the surface region are captured. A second two-dimensional substrate image of the surface region is captured with a second image capture modality that is different from the first image capture modality. The second image capture modality can provide greater accuracy with respect to the locations of at least one material in the surface region than the first image capture modality. The first two-dimensional substrate image is spatially aligned based on the second two-dimensional substrate image, and then a corrected first two-dimensional substrate image can be generated based at least in part on the locations of the at least one material in the second substrate image. two-dimensional. As an option, the corrected first two-dimensional substrate image comprises a first material content determined by the second modality which is not obscured by loading problems with regard to identifying this first material than when measured with the first modality, and a Porosity content of the sample is determined by the first modality which has greater accuracy with respect to the identification of porosity in the first two-dimensional image than in the second modality. As another option, the corrected two-dimensional substrate image is provided by altering the first two-dimensional substrate image with at least one digital mask where the locations of at least one sample porosity and the organic content determined for the first two-dimensional image by the first modality is corrected using at least one mask formed with reference to one or more of the locations of organic content identified in the second two-dimensional substrate image.
[012] The present invention further relates in part to a method of creating a three-dimensional volume wherein the method includes capturing a plurality of surface electron two-dimensional substrate images and a plurality of backscatter two-dimensional electron substrate images. An alignment of the plurality of backscatter electron substrate images is determined to generate a three-dimensional volume. A three-dimensional substrate volume is generated from the surface electron two-dimensional substrate images using the alignment of the plurality of backscatter two-dimensional electron substrate images.
[013] The present invention further relates in part to a method for generating a three-dimensional digital image of a sample, wherein the method has steps that include a) scanning a surface of a sample comprising kerogen, porosity and mineral by a primary electron beam generated by an electron source, and (i) recording first image data based on detecting surface electrons from the sample and storing the first image data as a first two-dimensional image comprising an allocated gray scale value each of a plurality of pixels in the image, and (ii) recording second image data based on detecting backscattered electrons emitted by the sample during scanning and storing the second image data as a second two-dimensional image comprising an allocated gray scale value each of a plurality of pixels in the image. The first and second two-dimensional images provide a double set of image data associated with the scanned surface. In step b), a layer is removed from the sample by an ion beam directed at the sample to provide a different exposed surface on the sample. In a step c), the different exposed surface of the sample is scanned by the primary electron beam, and steps a) (i) and a) (ii) are repeated to provide a double set of image data associated with the exposed surface different. In a step d), steps b) and c) are repeated a plurality of times. In a step e), a plurality of the double sets of image data obtained from steps a) and d) are stacked by placing the respective first and second two-dimensional images in the same sequential order as obtained from the sample. In a step f), the first two-dimensional images are aligned with reference to the second two-dimensional images. In a step g), the first and second two-dimensional images from the plurality of dual sets of image data are analyzed with allocation of the pixels to porous space, kerogen, or mineral to form first and second analyzed two-dimensional images. In a step h), pixels allocated to kerogen in the first analyzed two-dimensional images that are not allocated to kerogen in the second analyzed two-dimensional images are identified in the double set of image data. In a step i), the pixels identified in step h) are relocated to porous space in the first analyzed two-dimensional images associated with the double set of image data.
[014] The present invention further relates in part to a method for generating a three-dimensional digital image of a sample wherein the method includes the steps indicated a)-f) below, and the additional steps g)-j) wherein double masks are generated and used to correct the first two-dimensional images. In step g) of the present method, the first two-dimensional images from the plurality of dual sets of image data are base analyzed comprising segmenting the pixels into porous, kerogen, or mineral space to form first base analyzed two-dimensional images. In a step h), the second images of a plurality of dual sets of two-dimensional image data are first analyzed comprising selecting only pixels that have grayscale values exceeding a preselected grayscale threshold value for kerogen to define a first mask. In a step i), the second images from a plurality of dual sets of two-dimensional image data are further analyzed comprising selecting only pixels that have grayscale values below a preselected grayscale threshold value for a mineral to define a second mask. In a j) step, the first two-dimensional images analyzed from the base are changed by the first mask and the second mask. Pixels are reallocated from kerogen to porous space in the first two-dimensional images analyzed from baseline using the first mask, and pixels are reallocated from mineral to kerogen in the first two-dimensional images analyzed from baseline using the second mask.
[015] The present invention further relates in part to a system for generating a three-dimensional digital image of a sample including a charged particle microscope, first and second signal processing systems, and a computer. The charged particle microscope includes a scanning electron beam column comprising an electron source for generating a primary electron beam, an ion beam column for generating a focused ion beam through a sample to successively remove a thin layer. of the same in the direction of sample thickness and expose a different surface of the sample for scanning by primary electron beam, a first charged particle detector to detect sample surface electrons when scanning with the primary electron beam, and a second detector. charged particle to detect electrons backscattered by the scanned sample. The first signal processing system is operable to record first image data based on sample surface electrons detected by the first charged particle detector and store the first image data as a first two-dimensional image comprising an allocated gray scale value. for each of a plurality of pixels in the image. The second signal processing system is operable to record second image data based on electrons backscattered by the sample during scanning which are detected by the second charged particle detector and store the second image data as a second two-dimensional image comprising a value of gray scale allocated to each of a plurality of pixels in the image. The first and second two-dimensional images provide a double set of image data associated with the different exposed surface. The computer has at least one processor operable to execute a computer program capable of performing the calculations to create a three-dimensional digital representation of the sample. The calculations comprise i) stacking a plurality of double sets of image data obtained by the first and second processing systems by placing the respective first and second two-dimensional images in sequential order as obtained from the in-line sample, ii) analyzing the base the first two-dimensional images of the plurality of dual image data sets comprising allocating the pixels to porous, kerogen, or mineral space to form base analyzed first two-dimensional images, iii) first analyzing the second two-dimensional images of the plurality of dual image data sets comprising only selecting pixels that have grayscale values exceeding a preselected grayscale threshold value for kerogen to define a first mask, (iv), second analyzing the second two-dimensional images from the plurality of dual image data sets comprising selecting only pixels that have grayscale values below a pre-selected grayscale threshold value for mineral to define a second mask, and (v) change the first two-dimensional images analyzed from baseline by the first mask and the second mask, comprising relocating pixels from kerogen to porous space in the first two-dimensional images analyzed from baseline using the first mask and reallocate pixels from mineral to kerogen in the first two-dimensional images analyzed from baseline using the second mask.
[016] It is to be understood that both the above general description and the following detailed description are only exemplary and explanatory and are intended only to provide a further explanation of the present invention as claimed.
[017] The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate some of the embodiments of the present invention and together with the description serve to explain the principles of the present invention. Drawings are not necessarily drawn to scale. Like numbers in the drawings refer to like elements in the various views. BRIEF DESCRIPTION OF THE DRAWINGS
[018] Figure 1 is a schematic representation of a system according to an example of the present invention.
[019] Figure 2 is a schematic illustration of secondary electrons and backscatter electrons generated by a primary electron beam that is directed over a surface of the sample.
[020] Figures 3A and 3B show two-dimensional grayscale images captured on a rock sample surface with an electronic backscatter scan (also referred to herein as an "select energy backscatter" scan ("ESB scan") or scan backscatter electronics ("BSE" scan) and a surface electron scan (also referred to herein as a secondary electron scan ("SE2")), respectively, of the same sample slice, according to an example of the present invention.
[021] Figures 4A and 4B show kerogen phase segmentations for both the ESB and SE2 of the slices in Figures 3A and 3B, respectively, according to an example of the present invention.
[022] Figures 5A and 5B show segmented captured images generated from a method including a dual signal processing technique in which kerogen segmentation from ESB data is shown in Figure 5A and pore segmentation from ESB data SE2 is shown in Figure 5B, in accordance with an example of the present invention.
[023] Figure 6 is a block diagram showing several steps of a method according to an example of the present invention.
[024] Figure 7A shows an image of SE2 and Figure 7D shows an image of ESB that were acquired simultaneously for the same surface region of a sample and are spatially aligned. Figures 7B and 7C are images which are enlarged regions marked in Figure 7A with corresponding shapes. Figures 7E and 7F are images which are magnified regions marked in Figure 7D with corresponding shapes, in accordance with an example of the present invention.
[025] Figures 8A-8F include Figures 8A-8C corresponding to Figures 7A-7C and Figures 8E-8F show the images after a base segmentation is performed on the images. Some of the pore spaces (black) that are erroneously labeled as kerogen (grey) in the SE2 data are indicated by the arrow pointing in the upper left direction in Figures 8A, 8B, 8D, and 8E, and some of the kerogen (grey) that are erroneously labeled as mineral (white) are indicated by the arrow pointing horizontally to the left in Figure 8A, 8C, 8D and 8F, in accordance with an example of the present invention.
[026] Figures 9A-9B include Figure 9A which corresponds to Figure 7D, and Figure 9B shows an example of a mask created to relabel kerogen as a pore at locations where the signal is being read from inside the pore. The ESB in Figure 9A is segmented so that all values and only values above those representing real kerogen in the SE2 image are selected, which is indicated by the "sea" areas in Figure 9B, according to an example of the present. invention.
[027] Figures 10A-10B include Figure 10A which corresponds to Figure 7D, and Figure 10B shows an example of a mask created to relabel mineral as kerogen in locations where the kerogen has charged. The ESB in Figure 10A is segmented so that all values and only values below those representing actual mineral in the SE2 image are selected, which is indicated by the added shading in Figure 10B, in accordance with an example of the present invention.
[028] Figures 11A-11I include three sets of images that show the effect of the two masks created from the ESB image on the resulting segmentation. The SE2 data defined in Figures 11A-11C corresponds to Figures 8A-8C, Figures 11E-11F corresponds to Figures 8D-8F, and the base segmentation modified by two masks is shown in Figures 11G-11I, and the arrows indicate the same erroneously labeled phases as indicated above in Figure 8A-8F, in accordance with an example of the present invention.
[029] Figures 12A-12C are three enlarged views of the pore space near the arrow shown in Figure 11B, 11E and 11H, respectively, in which the SE2 dataset is shown in Figure 12A, the base segmentation in Figure 12B, and the base segmentation after correction of the two masks in Figure 12C, according to an example of the present invention.
[030] Figure 13 includes a Table 1 showing results for determination of kerogen and porosity content for scanned FIB-SEM slices of shale samples using a method according to an example of the present invention and a comparison method including manual analysis of image content. DETAILED DESCRIPTION OF THE PRESENT INVENTION
[031] The present invention relates in part to a method for generating a multidimensional image of a sample that combines different image capture modalities having the ability to analyze data for identification and integration of the most accurate image characteristics captured by each respective modality to produce reconciled image data of greater accuracy and consistency than possible from any modality alone. The method of the present invention can be particularly useful, for example, for generating digital images of samples that contain different phases that are not imaged at the same levels of precision by a single high-resolution imaging modality. Recognizing this problem, a method of the present invention includes simultaneous capture of dual sets of image data for the same surface of a sample using different image capture modalities. The different image capture modalities are part of a dual signal digital image generation, acquisition, analysis and display system. As an option, at least one of the modalities can provide superior identification accuracy for at least one image feature compared to the other image capture modality or modalities. Corrected images can be generated from the identifications of different characteristics with the corresponding modality that provides the superior identification accuracy for the given characteristic. Rock samples, for example, can have one or more types of solid materials (eg, inorganic material, organic material, or combinations of these phases) and possibly porous space. When multiphase materials are viewed under a scanning electron microscope or other high resolution image capture device, for example, a SEM surface electron or secondary electron detector, for example, can generate signals that provide images Two-dimensional grayscale displays that can display pore space with high accuracy at the given slice level. These scans can also capture solid material signals within the pore space at a location that belongs to a subsequent or deeper slice of the sample, which can create misidentifications for the image. Unless corrected by a present method, solid material misidentified from the deepest slice may deceptively appear in the two-dimensional image as occupying space in the same two-dimensional slice as the pore through which it is detected. In addition, some organic rock contents, such as kerogen, can also carry over to the mineral phase during SEM scanning and become misidentified as a mineral in the two-dimensional image. Thus, reliance on captured surface electron imaging can result in incorrect determinations of pore space and solid material or materials for a sample slice. When two-dimensional images are stacked in a single three-dimensional volume, these identification errors can be compounded if not corrected by the present method. The present method can provide such correction modes in highly automated routines that are more accurate, faster and more repeatable than reliance on manual image analysis and processing.
[032] As an option, a method of the present invention can determine phase distribution content in rock containing organic content in which a corrected two-dimensional substrate image can be generated that comprises organic content of interest determined by a modality having greater accuracy in terms of with respect to organic content, and any porosity content is determined by a different modality having greater accuracy with respect to porosity in a two-dimensional image that has been aligned using the second two-dimensional substrate image. As another option, a method of the present invention provides a second imaging modality that can include at least one type of solid material with a high level of accuracy at the same slice level, and these more accurate identifications can be used to correct for by. minus one of the solid material misidentifications in the first image which are actually porous space and solid material misidentifications as a different type of solid material.
[033] The present method can be applied for the generation and correction of individual two-dimensional images. The method can also be applied for generating and correcting multiple two-dimensional images that are obtained from successive slices of a sample, and the stacked alignment corrected images provide a high-precision simulation of the three-dimensional volume of the scanned portion of the sample.
[034] As indicated, the present method can be implemented in a highly automated way in a relatively short period of time. The present method can avoid the need to correct slices by hand one slice at a time. A manual process can be very time-consuming, non-repeatable, and inaccurate as shown in the examples included here. Also, with manual marking corrections, results can highly depend on the individual making manual corrections. The present method reduces the opportunity for such errors to arise and adversely affect simulated image results.
[035] As an option, a method of the present invention relates to creating a three-dimensional display of the volume of a sample wherein the different indicated image capture modalities comprise an modality for capturing a plurality of two-dimensional electron substrate images of surface, and a different embodiment which may comprise an embodiment for capturing a plurality of backscatter two-dimensional electron substrate images that are used to correct the two-dimensional surface electron substrate images. After determining the alignment of both sets of images based on the plurality of backscatter electron substrate images, a three-dimensional substrate volume formed by corrected images can be generated from the two-dimensional surface electron substrate images including corrections made. for features misidentified with reference to the backscatter electron substrate images. Optionally, the different embodiment may comprise capturing a plurality of energy dispersive spectrometer (EDS) substrate images.
[036] As an option, a method for measuring porosity and organic content in rocks or mineral specimens is provided that can integrate three-dimensional slice-by-slice image data acquisition capabilities with powerful image analytic capabilities in a highly automated manner. To determine porosity and kerogen or other fractions of organic content in a rock sample, a charged particle microscope equipped for various signal detection modalities can be used to generate three-dimensional sample data such as dual sets of image data. Dual image datasets can provide different levels of accuracy to image different sample characteristics, where dual datasets can be aligned, analyzed and merged or integrated into current methods to produce high-precision single images and consistency for the sample. A rock or mineral material, for example, that can be analyzed by this method is not necessarily limited. The rock can be, for example, shale, mudstone, siltstone, claystone, porcelain, dolomite, or a combination thereof. Shale is mentioned in some descriptions provided herein by way of illustration and not limitation. The method can be applied, for example, to unconventional rocks and minerals or "tight" fine grain formation. Tightly formed materials can have very low permeability, such as less than about 0.1 milliDarcy absolute permeability, or they may not have porous networks of flow paths at all. The rock may include mineral material, such as solid crystalline or mineral material. Optionally, organic content can include kerogen. Kerogen is a mixture of organic chemical compounds that form a portion of the organic matter in some rocks, such as sedimentary rocks. Kerogen typically is insoluble in normal organic solvents because of the very large molecular weight (eg, above 1000 Daltons) of its component compounds. When heated, some types of kerogen can release crude oil or natural gas. In one option of the present method, the rock can be slice-scanned by a FIB-SEM device that simultaneously generates multiple signals that can be processed and transformed into separate sets of grayscale images that produce different results for mineral identification (by eg grain), organic content (eg kerogen) and any pore space content of the rock slices or other swept sample.
[037] As an option, to determine the locations and fractions of different phases of a sample, such as a rock sample, a focused ion-beam scanning electron microscope (FIB-SEM) equipped for various detection modalities can be used. to produce two-dimensional (2D) images on different sample slices at a very high resolution. A charged particle beam system 100 is shown in Figure 1 to illustrate a FIB-SEM system that can be used for this option. The charged particle beam system 100 comprises a scanning electron beam column 101 and a focused ion beam column 201. As shown in Figure 1, the optical axis 102 of the electron beam column 101 and an optical axis 202 of the focused ion beam column 201 intersects substantially in the plane defined by the flat surface 302 of a sample 301. In this illustration, the optical axis 202 of the focused ion beam column 201 extends approximately perpendicularly to that plane of the sample 301 and the beam of ions therefore collide orthogonally on this surface in this example. The angle at which the electron beam traveling along the optical axis 102 of the SEM 101 column collides with the surface 302 of the sample 301 in this configuration can be a conventionally used value, such as about 30° to about 40°, or any other suitable values. In the scanning electron beam column 101, a primary electron beam can be generated by an electron source 103, such as a Schottky field emitter, and an anode 104. The emitted electrons can also be passed through an extraction electrode 105 disposed between the electron source 103 and the anode 104. The accelerated electron beam then can pass through a hole in the bottom of the anode 104 and is substantially collimated by a collimator system 107 and then passes by an opening stop 109 and an interior space 111 of the electron beam column 101. The system described thus far may comprise components shown in a system such as in US Patent No. 7,770,293 B2, which is incorporated herein by reference. with regard to these and other details of the design of the electron optical system and the ion optical system. A detector 112 for secondary or surface electrons and a separate detector 114 for backscattered electrons are disposed in interior space 111 through which the accelerated electron beam passes. Following the beam direction of the electrons, an objective lens 116 can then be provided which may be a combination of a magnetic lens and an electrostatic lens, which may have characteristics such as those described in the above incorporated patent. The focused ion beam column 201 can comprise an ion source 203 and other components, as described in the above-incorporated patent, capable of generating an ion beam that can also be impinged on the surface 302 of the sample 301.
[038] On the left side of Figure 1, some control elements 15 of system 100 are shown. A scan control 1 can generate a scan signal that is applied to electron beam column 101 and the same or a separate scan control (not shown) can generate a scan signal that is applied to FIB column 201. Scan control signal 1 can also be applied to data memory 2 and can drive data memory 2. Data memory 2 can have a suitable capacity to store a plurality of simultaneously captured dual image data sets. Secondary and backscattered electrons emitted by sample 301 because of the primary electron beam can be accelerated by objective lens components 116 of scanning electron beam column 101 in the direction of the optical axis of electron beam column 101 and can be detected by detectors 112 and 114. The separate signals detected by detectors 112 and 114 can be amplified or otherwise enhanced by the respective signal processing units 3A and 3B, and stored in the data memory 2 in combination with the designated information from the control Scanning 1. Thin slices can be removed from the sample 302 using focused ion beam column 201. By deflecting the focused ion beam, for example, in a direction perpendicular to the plane which is defined by the optical axis of the beam column. electrons 111 and optical axis of ion beam column 201, using scan control 1, thin slices can be removed from sample 302. Simul Similarly, image data is generated using the scanned electron beam and detecting secondary and backscattered electrons with detectors 112 and 114, respectively. The image data generated by the electron beam column within the time a slice is removed defines a set of image data, and each detector 112 and 114 captures signals for a respective set of image data. By repeatedly removing one slice after another and continuously generating image data a plurality of double sets of image data are recorded and stored in memory 2. For scanning electron microscopes (SEM), scanners typically emit two-dimensional arrays of values that represent the grayscale values from the scanner. In a further step, the plurality of image data sets stored in memory 2 are evaluated in an image data analysis and adjustment unit 4. In relation to image analysis and adjustment, reference is made to Figures 3-13 here . After the image analysis and adjustment has been carried out, the results can be stored in memory 2 and enough information can be available to generate high resolution 3D image previews of the results in a view 5, including according to usual viewing methods and known are available.
[039] As indicated, a feature of this option is the ability to simultaneously detect secondary or surface electrons and backscatter electrons to produce respective dual signals for capturing and generating dual sets of image data based on each detection mode . A secondary electron detector, for example, can be used to detect signals that result from electron beam interactions with atoms on or near the surface of the sample. As illustrated in Figure 2, primary electrons from a primary electron beam ("PE") impinging on a sample surface at a beam point can release secondary electron by an inelastic interaction, which may be referred to as "SE1" . Primary electrons can also penetrate the sample, undergo plural elastic interactions within a so-called interaction volume very close to the sample surface, and emerge from the sample at a distance from the beam point as backscatter electrons, which can be referred to as "BSE" or "ESB". In addition, secondary electrons can be released from the sample just as backscattered electrons emerge from the sample, which can also emerge from the sample at a distance from the beam point, and these secondary electrons can be referred to as " SE2". Backscattered electrons can collide with the outside of the SEM lens, for example, to release additional secondary electrons, sometimes referred to as "SE3" (not shown in Figure 2). The concepts of BSE, and SE1, SE2 and SE3 types of secondary electrons are generally known. These BSE typically have higher energy level and other differences with respect to secondary electrons, and these differences can be exploited to detect them separately. As an option, the detection of secondary electrons in methods of the present invention refers to the detection of "SE2" secondary electrons". In this option, dual image data sets can be based on signal detection for BSE and SE2 electrons. The scattering process and mechanisms taking place in the interactive volume very close to the sample surface may be different for different materials and may depend, for example, on the composition and structure of the material. As indicated, simultaneous detection of secondary and backscattered electrons is provided in a present method so that dual sets of image data can be captured for each sample slice.
[040] Furthermore, as indicated, after double sets of images are captured for a given slice of the sample, the focused ion beam of the FIB-SEM can be used to remove a thin layer from the surface of the sample and another double set of data from image can be captured on the newly exposed surface. The thin layer removed with the FIB can be, for example, from about 1 nm to about 30 nm, or between about 1 nm to about 20 nm, or between about 1 nm to about 15 nm, or between about 1 nm to about 10 nm, or between about 1 nm to about 5 nm, or between about 2 nm to about 4 nm, or other values. A FIB-SEM system that can be adapted for use in the indicated method can be obtained commercially, for example, as a model referred to as the AURIGA® CROSSBEAM® FIB-SEM workstation from Carl Zeiss SMT AG (Oberkochen, Germany). As an alternative, one of the indicated surface electron and backscatter electron detectors can be replaced with a detector to detect X-ray signals emitted by the sample, such as an energy dispersive spectrometer ("EDS"), and store the data from image as an alternative set of image data in addition to the surface electron-based image data or the backscatter electron-based image data.
[041] Many images can be obtained sequentially in these methods and then combined by stacking and aligning them in the correct position, to create a preliminary three-dimensional (3D) volume. The raster image output produced by an SEM scanner can be a 3D numeric object including a plurality of 2D slices or sections of the formed image sample. Each 2D slice can include a grid of values each corresponding to a small region of space defined within the grid plane. Each such small region of space is referred to as a "pixel" and assigned a number that represents the intensity of the image (or, for example, the density of the material as determined by the CT scanning procedure).
[042] The process by which two-dimensional images are stacked and aligned is not trivial. Grayscale images can be stacked and aligned, for example, with data analysis and visualization software adapted for use in the present methods. Stacking can be done, for example, sequentially by positioning the slice images in the order they were taken from the sample. Alignment can be based on processing techniques that identify the correct lateral position of one slice relative to the next in the same stack. As an option, the two-dimensional substrate image or images obtained based on surface electron detection can be aligned with reference to the two-dimensional substrate image or images obtained using backscatter electron detection. For example, kerogen locations in a two-dimensional substrate image obtained with electron backscatter detection can be highly accurate and can be used to align the two-dimensional substrate image or images obtained from electron backscatter detection and also captured simultaneously two-dimensional substrate image or images obtained from a surface electron detection on the scanned sample. Backscatter electron data typically contains fewer artifacts for rock samples such as shale, and these two-dimensional images can be used to more easily align the slices and create a three-dimensional volume. For example, since kerogen sites can be presented more accurately in backscatter electron substrate images captured in rock samples and, more than in surface electron substrate images, kerogen sites in backscatter images Backscatter electron substrate can be used to align the counterpart surface electron substrate image that was captured at the same time with the FIB-SEM system. With alignment determined from backscatter electron data, surface electron data can be manipulated identically. The identified kerogen locations can be used to laterally align (X-Y directions) a two-dimensional substrate image of the sample that was simultaneously acquired by surface electron detection. Where a three-dimensional volume of images must be generated based on successive scans and capture of double set of image data on each slice, alignment can also be based on the kerogen sites identified in the two-dimensional substrate images captured from a detection of backscatter electron for each slice where nanoscale or other very small thicknesses are used to generate the two-dimensional image stacks for successively scanned slices of a sample. Using thin slices, kerogen sites that propagate through adjacent slices of the images obtained from an electron backscatter detection can be identified and used as a reference point or points for aligning this pile and the separate pile of slices comprising images obtained with surface electron detection. Kerogen locations in images obtained by electron backscatter detection can be used to laterally align images captured simultaneously with each other, and images of adjacent slices. This alignment process can be performed slice by slice for a stack of successively acquired double sets of images for the sample. Using the present alignment method, surface electron images can be aligned without the additional processing that would otherwise be required. As another option, physical registration or reference marks can be created on the surface of the sample having the image formed for alignment purposes, as described, for example, in US Patent No. 7,750,293 B2.
[043] For the purposes described here, "segmentation" means a process of partitioning a digital image into several segments (sets of pixels). Image segmentation is commonly used to locate objects and borders (lines, curves, etc.) in images. In porous rock segmentation, for example, it can be used to allocate porous space and one or more non-porous phase regions and their boundaries. Image segmentation is the process of allocating a label to pixels in an image such that pixels with the same labels share certain visual characteristics. The result of image segmentation is a set of segments that collectively cover the entire image, or a set of contours extracted from the image. Each of the pixels in a region can be similar with respect to some computed characteristic or property, such as color, intensity, or texture. Adjacent regions are different with regard to the feature(s). General purpose algorithms and techniques have been developed and used for image segmentation in the field of digital image processing. For example, a digital image of a rock sample can be segmented into its composition classes. The term "composition classes" can encompass, for example, open pores, mineral(s), optionally other types of materials, or any combinations thereof. Members of a single composition class must have the same composition and general structure relative to other composition classes so that they influence to a similar extent rock properties. As is known in the art, there can be ambiguity in the segmentation of X-ray attenuation images (to use the X-ray tomography example) into composition classes of similar mineralogy because different rock minerals can have similar X-ray attenuations. Segmentation can be greatly facilitated if previous information about the mineral composition of the sample limits the number of possibilities for each pixel. As is also known, where there is no prior information, x-ray diffraction can be used to determine mineralogy. If two classes of composition have equal or nearly equal x-ray attenuations, it may be necessary to use structural patterns to distinguish them as will be understood by those skilled in the art. Grayscale is a non-limiting example. These and other targeting methods and techniques can be applied or adapted for use in a method and system of the present invention.
[044] As an example, after alignment, dual image datasets can be analyzed to assign or segment pixels in the two-dimensional grayscale images to different phases (eg, porous space, kerogen, or mineral, in some samples of rock) to form two-dimensional images of the analyzed base. The value assigned to each pixel of the 2D slices is typically an integer which can range, for example, between zero and 255, for example, where 0 is, for example, pure black, and 255 is pure white. Such an integer is commonly referred to as a "greyscale" value. In the example given, 0 to 255 can be associated, for example, with eight digital bits in a digital word that represents the gray scale value in each pixel. Other grayscale ranges may be associated with longer or shorter digital words in other implementations, and the range from 0 to 255 is not intended to limit the scope of the invention. As an option, in order to simulate a process using such a numerical object (the gray scale) for a rock sample, pixel allocation can comprise the allocation of pixels in the images to porous space, kerogen, or mineral, by determining whether the pixels meet preselected threshold criteria based on preselected grayscale values for porous space, kerogen, or mineral, respectively. The numerical object can be processed, for example, so that all pixels allocated to the empty space of a rock sample (pores) are represented by a common numerical value, for example, just zeros, and all pixels associated with the Rock minerals or kerogen are represented by different (higher) numerical values, eg a gamma value or value much closer to 255 for mineral, and an intermediate value or gamma value between this for minerals and pore for kerogen. A routine that can be used for allocation can be, for example, data visualization and analysis software adapted for the present method.
[045] For rocks such as shale, for example, there may be a great complexity in the characteristics of the images. Images may also contain artifacts from the acquisition process that are not present in the actual sample. Thus, creating a stack of three-dimensional images of a sample can be technically difficult without the present method. For example, where images are obtained from a surface electron detector used in a FIB-SEM to create a three-dimensional volume from which porosity and kerogen or other organic content is quantified, the images created using the detector data Surface electron detectors alone can provide sharper edges in porous spaces (porosity) than, for example, from electron backscatter detector data. However, it has been found that there are typically more artifacts in the surface electron data that make three-dimensional alignment and quantification of kerogen or other organic content more difficult than when using a different modality, eg, backscatter electron data. For accurate determination of porosity, then additional processing steps are required to deal with the digital artifacts that may be present in the surface electron data. As indicated, manual corrections, however experienced in how particular a human image interpreter can be, are usually time-consuming and require visual interpretation and personal judgment. The present method can overcome these problems associated with reliance on manual interpretation of images.
[046] As an option, in the method of the present invention, kerogen fraction can be determined from the backscatter electron data and porosity fraction can be determined from surface electron data that have been aligned using the backscatter image stack. backscatter electron by any of the simultaneously captured two-dimensional images captured from the double dataset acquired in the FIB-SEM. An illustration of the different results that can be obtained based on surface electron scans and backscatter electron scans of the same rock sample surface with a FIB-SEM device, and the calculation of a corrected image result with The basis on this different data is shown, for example, in Figures 3A-3B, 4A-4B and 5A-5B. Figures 3A and 3B show two-dimensional grayscale images that were captured simultaneously on a rock sample surface (ie, a shale surface) with an electron backscatter (ESB) scan) and a surface electron scan (secondary electron scan (SE2)), respectively, of the same sample slice using an AURIGA ® CROSSBEAM ® FIB-SEM workstation obtained from Carl Zeiss NTS GmbH. Figures 4A and 4B show separate ESB and SE2 segmentation images of the slices of Figures 3A and 3B, respectively. At this stage of the data analysis, the calculated results for the ESB scan of Figure 3A are 1.8% porosity, 22.1% kerogen, and 0 ND absolute permeability, and for the SE2 scan of Figure 3B, they are porosity 5.6%, kerogen 16.6%, and absolute permeability 36/0/15 nD (x, y, z axis). Thus, the results of the ESB and SE2 scans do not match. These results show that ESB and SE2 scans can have significantly different capabilities to distinguish kerogen pores in shale or other rock. Figures 5A and 5B show segmented captured images from a present method including a dual signal processing technique where kerogen segmentation from ESB data is shown in Figure 5A and pore segmentation from SE2 data is shown in Figure 5B. As an option, the kerogen content of the sample slice can be determined from the kerogen segmentation only from the electron backscatter (ESB) data (Figure 5A) and the porosity can only be determined from the kerogen segmentation. pore from the surface electron data (SE2) (Figure 5B) that was aligned using the backscatter electron image stack. If this option is used, the calculated and merged results for these two types of images acquired for the same sample slice are 5.6% porosity as a function of determining higher porosity resolution from surface electron data, kerogen 22 .1% as a function of determining high resolution kerogen from electron backscatter data, and 36/0/15 nD absolute permeability (x, y, z axis). The absolute permeability of the sample was determined by numerical simulation. Using the present method on a plurality of simultaneously captured two-dimensional images indicated from the dual dataset acquired at FIB-SEM for a given scanned sample, kerogen volume fractions, porosity, and for other phases of a rock can be more accurately determined . The method can also be applied to other types of samples, and is not limited to rock or mineral. Data processing and segmentation time can be reduced by this method. Another advantage of the method is that it is much faster, more consistent and more accurate than a methodology using manual analysis.
[047] FIB-SEM (SE2) images, for example, can become increasingly difficult to segment as the pore space becomes larger and signals are captured from solid material within the pore space from one location that belongs to a subsequent slice. An uncorrected segmentation used to segment computer tomography (CT) datasets typically labels this material as kerogen (or, in a worse case, as mineral for materials that have carried or oriented nearly parallel to the ground surface) when it should be labeled as porosity. Kerogen, for example, can be erroneously labeled as a mineral when charging during scanning by a FIB-SEM device. Without the present method, these misidentifications would have to be manually corrected one slice at a time. As indicated, a manual process is very time-consuming, non-repeatable and imprecise. Results can highly depend on the individual making the manual corrections.
[048] As another option, a method of the present invention can correct images captured as surface electron two-dimensional substrate images with at least one mask that can be developed from backscatter two-dimensional electron substrate images that are captured simultaneously in each slice. In this option, pixels can be relocated from kerogen to porous space in surface electron two-dimensional substrate images using a first mask. Additionally or alternatively, pixels can be relocated from mineral to kerogen in the surface electron two-dimensional substrate images using a second mask. To correct pores misidentified as kerogen in surface electron two-dimensional substrate images, such as where material within a deeper slice pore appears in a gray scale band of kerogen, inspection of an electron dataset Simultaneous acquired backscatter imaging can be used to reveal areas in surface electron two-dimensional substrate images where the pore is misnamed as kerogen. For example, backscatter electron data that is taken simultaneously with and aligned with surface electron data reveals that in areas where pores have been mislabeled as kerogen in surface electron data than backscatter electron data have a significantly higher grayscale value than areas labeled kerogen that are correct. This indicates that these areas have higher gray scale values than would be expected from real kerogen. For example, with the first mask, real pore can be assigned a high gray scale value as it appears white relative to real kerogen in backscatter SEM images (eg, about 190-240). The second kerogen mask that was loaded and erroneously labeled as mineral can be assigned a low grayscale value relative to the mineral phase as kerogen may appear as a lower grayscale relative to the mineral phase in backscatter SEM images (for example, about 0 to 115). A surface area in the surface electron data that appears significantly darker in the shadow and has a gray scale value significantly greater than the actual kerogen in the backscatter electron data can be identified by comparing the kerogen identified in the data. surface electron with this in the backscatter electron data. For example, the backscatter electron dataset may reveal pore areas that were incorrectly identified as kerogen in surface electron two-dimensional substrate images that have grayscale values that are higher than the areas correctly labeled as kerogen in the two-dimensional backscatter electron substrate images. This difference can be exploited to correct for porosity misidentified as kerogen in the surface electron two-dimensional substrate images while leaving real kerogen sites unaffected. To correct kerogen misidentified as mineral at locations on surface electron two-dimensional substrate images where kerogen has been charged in the mineral grayscale range during scanning (eg charged kerogen appears much lighter than normal on images ), the same backscatter electron dataset used to correct porosity can be used to make these corrections. For example, there may be areas of the segmented mineral phase in the surface electron dataset that should be identified as kerogen, but this is not because these areas have a grayscale value that is above the grayscale range assigned to kerogen . These areas mislabeled as mineral in the surface electron data are found to have a significantly lower grayscale value in the backscatter electron dataset than the areas classified as mineral that are correct. These areas in the surface electron dataset appear significantly darker than the actual mineral areas in the backscatter electron dataset. For example, the backscatter electron dataset may reveal areas of kerogen misidentified as mineral in surface electron two-dimensional substrate images that have grayscale values that are lower than areas correctly labeled as minerals in images two-dimensional backscatter electron substrate patterns. This difference can be exploited to correct for kerogen mislabeled as a mineral in the surface electron two-dimensional substrate images leaving the real mineral unaffected.
[049] In the block diagram of Figure 6, the main process steps of a current method using double masks to correct the double set of image data are shown. In step 101, a surface of the sample is scanned, such as with a FIB-SEM, as shown here. In step 102, dual sets of SEM image image data signals that are captured by various detectors, as indicated herein, are recorded (e.g., during a two-way scanning of the electron beam of the optical column of electrons in two directions. perpendicular to its optical axis and detect secondary and backscattered electrons). In a consecutive step 103, this double set of image data is stored in an image memory. During the time that the image dataset is recorded in step 103, a slice can be removed from the sample in step 104, for example, by dry etching or spraying the sample by the focused ion beam. These steps 101 to 104 are repeated a certain number of times, which is designated by recursive arrow 104A until a desired plurality of dual sets of image data are stored in memory. After the desired amount of dual sets of image data is recorded at step 103, the dual sets of images are stacked at step 105 and then aligned at step 106. At step 107, the images are analyzed (e.g., segmented ) to preliminarily allocate phase locations in the images, such as, for example, for pore, kerogen, and minerals for some rock samples. In steps 108 and 109, masks are developed to correct pore space that has been misallocated to kerogen and kerogen that has been misallocated to mineral. In step 110, changes or corrections are made to one of the image sets using the masks. After the above steps have been performed, enough information to generate high resolution 3D image display according to usual and known display methods is available.
[050] An example of a double mask method of correcting digital images of a method of the present invention is provided with reference to Figures 7-13. In this illustration, a shale rock is swept with an AURIGA® CROSSBEAM® FIB-SEM workstation from Carl Zeiss SMT AG (Oberkochen, Germany). Other combinations of different scanning modalities can be used, including those indicated in this document. In this example, dual signals are simultaneously acquired with an SE2 detector and ESB detector that are used with the FIB-SEM device. Image data is recorded based on surface electrons detected in the sample and stored as a two-dimensional image comprising a gray scale value allocated to each of a plurality of pixels in the images. A separate set of image data is recorded based on the detected backscattered electrons emitted by the sample during scanning and stored as two-dimensional images comprising a gray scale value allocated to each of a plurality of pixels in the images. Two-dimensional images provide a dual set of image data associated with the scanned sample. The two-dimensional images obtained based on surface electron detection and double backscatter electron each can be stacked and aligned in the aforementioned shape or shapes. The dual image datasets can then be analyzed to allocate pixels in the two-dimensional grayscale images to pore space, kerogen, or mineral to form two-dimensional base-analyzed images. Commercial data visualization and analysis software can be adapted to perform the analysis, such as a computerized segmentation routine. The segmentation routine can be, for example, a tool or a module of a data analysis and visualization software adapted to carry out the analysis indicated here.
[051] As an option, routines are provided using the ESB data as a second image set to increase the accuracy of the pore and kerogen phases labeled in the SE2 data as a primary image set. Two masks are created from the ESB data for two purposes. As a purpose, kerogen is relabeled as pores in places where material within the pore from a deeper slice appears in the gray scale range of kerogen. Closer inspection of the ESB data, which is taken simultaneously with and aligned with the SE2 data, reveals that in areas that the pore was mislabeled as kerogen, the ESB data has a significantly higher grayscale value than the areas labeled as kerogen which are correct. As indicated, this difference is exploited to correct porosity mislabeled as kerogen while leaving real kerogen unaffected. For another purpose, mineral is relabeled as kerogen in places where kerogen has been loaded into the gray scale range of mineral during scanning, such as by a FIB-SEM device. As indicated, the same ESB dataset used to correct for porosity can be used to correct for kerogen, where the segmented mineral phase that must be kerogen has a significantly lower gray scale value in the ESB dataset than the areas classified as mineral that are correct. Kerogen erroneously labeled as a mineral in the surface electron data is corrected while leaving the real mineral unaffected.
[052] For example, Figure 7A shows an image of SE2 and Figure 7D shows an image of ESB that were acquired simultaneously for the same sample surface region and are spatially aligned. Figures 7B and 7C are images which are enlarged regions marked in Figure 7A with corresponding shapes. Figures 7E and 7F are images that are magnified regions marked in Figure 7D with corresponding shapes. The SE2 dataset is segmented using data visualization and analysis software to produce the base segmentation. The ESB dataset is also segmented to produce the two masks that will be used to change the base segmentation produced from the SE2 dataset.
[053] Figures 8A-8F include Figures 8A-8C corresponding to Figures 7A-7C and Figures 8E-8F show the images after base segmentation is performed on the images. Some of the pores (black) were erroneously labeled as kerogen (grey) because of SE2 data being acquired within the pore space (for example, see the arrow pointing at an angle to the upper left direction in Figures 8A, 8B, 8D and 8E) and that part of the kerogen (grey) was erroneously labeled as mineral (white) because it was loaded during sweeping (for example, see arrow pointing in the horizontal direction towards the left side of the figure in Figures 8A, 8C, 8D, and 8F).
[054] Figures 9A and 9B are an example of a method for creating a first mask to relabel kerogen as a pore in places where the signal is being read from the interior of the pore. Figure 9A corresponds to Figure 7D, and Figure 9B shows an example of the created mask. The ESB shown in Figure 9A is analyzed so that all pixels that have grayscale values and only grayscale values above those that represent real kerogen in the SE2 image are selected, which are indicated as areas of " sea" in Figure 9B. Sites where the signal is being acquired from within the pore have higher gray scale values than sites where real kerogen is present so it is possible to relabel these areas as pores without relabeling those areas that are real kerogen. For example, only pixels that have a grayscale value greater than a preselected grayscale threshold value for real kerogen are selected when defining a first mask.
[055] Figures 10A-10B include Figure 10A which corresponds to Figure 7D, and Figure 10B shows an example of a second mask created to relabel mineral as kerogen in locations where kerogen loaded in grayscale values different than actual kerogen in response to the FIB-SEM scanning process. The order of creation of the first and second masks indicated is not limited. The ESB data in Figure 10A is analyzed so that all grayscale values and only grayscale values below those representing actual mineral in the SE2 image are selected, which is indicated by the added shading in Figure 10B . For example, analysis of two-dimensional ESB images from the plurality of dual sets of image data can be done by selecting only those pixels that have grayscale values below a preselected grayscale threshold value for mineral to define the second mask. Since loading is not as much of a problem in the ESB dataset compared to the SE2 dataset, it is possible to select kerogen loaded areas in the ESB dataset that cannot be segmented as kerogen in the dataset of SE2. However, as the boundaries of the ESB datasets can be somewhat confusing and the resolution lower, the kerogen phase from the ESB dataset can be used, but it may not be the optimal solution. For example, boundaries can be segmented from the SE2 dataset, such as using the indicated data analysis and visualization software, while ESB data can only be used to fill in the loaded areas within these boundaries.
[056] Figures 11A-11I include three sets of images that show the effect of the two masks created from the ESB image on the resulting segmentation. The SE2 dataset in Figures 11A-11C corresponds to that in Figure 8A-8C, and those in Figures 11D-11F correspond to Figures 8E-8F. The base segmentation modified by two masks is shown in Figures 11G-11I. The angle and horizontal arrows indicate the same regions as discussed earlier in Figures 8A-8F. In Figure 11H, kerogen within the porous space near the angled arrow was correctly relabeled as pores, and in Figure 11I, the mineral near the horizontal arrow was properly relabeled as kerogen. The analyzed base two-dimensional image based on the SE2 image data is thus altered and corrected by the first mask and the second mask. Pixels are reallocated from kerogen to porous space in the base two-dimensional image analyzed based on the SE2 data using the first mask and pixels are reallocated from mineral to kerogen in the base two-dimensional images analyzed based on the SE2 data using the second mask.
[057] Figures 12A-12C are three enlarged views of the pore space near the arrow shown in Figure 11B, 11E and 11H, respectively, where the SE2 dataset is shown in Figure 12A, the base segmentation in Figure 12B, the base segmentation corrected by the two masks in Figure 12C.
[058] Table 1, which is shown in Figure 13, presents a comparison of the results obtained between a comparison method in which experienced analysts are used to manually analyze the images to segment FIB datasets and the present method indicated in terms of total porosity and kerogen volume fractions. Kerogen values increase or decrease depending on the nature of the sample. As shown in the results, in some cases, the manual method seriously underestimates the total porosity of the sample and at least by one degree in all cases.
[059] Although for the sake of simplification of the present illustration, it only shows images captured and corrected for single slices of a sample, it should be noted that the indicated FIB-SEM workstation can be used to remove successive layers from the sample by an ion beam directed at the sample to provide a different exposed surface on the sample, and the different exposed slice can be scanned and double sets of image data can be captured for each slice for alignment, analysis and correction as shown here . A 3D volume can be created with the resulting stack of corrected images. A system of the present application may include at least one device for displaying, printing or storing scan results, processed images, corrected images, or other results. For example, the resulting 3D volume can be viewed (eg, on an LED screen, LCD screen, CRT screen, HD screen, plasma screen, or other screens), stored in memory, printed with a printer ( eg in strip form), or any combinations thereof.
[060] The indicated analyzes and corrections made to the image datasets provided in the present methods can be performed in a highly automated manner. A program module or modules can be programmed into the data visualization and analysis software, for example, to perform this operation. A program product may be stored on a non-transient computer-readable medium, which, when executed, allows a computer infrastructure to perform at least the indicated stacking, alignment, analysis, and image correction steps. The computer-readable medium may include the program code embodied in one or more articles of portable storage of manufacture (eg, memory card, flash memory, DVD, CD, magnetic disk, a tape, etc.), on one or plus data storage portions of a computing device, such as memory and/or other storage system, and/or as a data signal traveling across a LAN or internet network (eg during electronic distribution with / wireless from the program product). To this end, deployment of the program product may include one or more of the following: (1) installing a program code into a computing device, such as a computer, from a computer-readable medium; (2) the addition of one or more computing devices to the computer infrastructure; and (3) incorporation and/or modification of one or more existing computer infrastructure systems to enable computer infrastructure to carry out the processes of the invention. Program code can be embodied as one or more types of program products, for example as a software program / application, component software / a function library, an operating system, a basic I/O system / controller for a particular computing / or I/O device, and the like.
[061] The technical advantage of the present method can be more precise segmentations and, therefore, more precision in all resulting 2D and 3D image products. Threads themselves can be repeatable and can be more consistent across multiple users. Segments are less likely to lose porosity and kerogen in rock samples, for example, and may be more repeatable because of the reduced or avoided need for manual labeling of materials. The resulting quality of computed properties can be improved. The segmentation process can be shorter than manual methods and therefore more efficient. An economic benefit of the present method can be more consistent, higher quality results in a short period of time. More samples can be completed using the same human resources. More projects can be completed by a given time using the same human resources as the present method can reduce the time required to segment FIB datasets, reducing the need for manual labeling phases of a sample image.
[062] The present invention also includes the following aspects/modalities/features in any order and/or in any combination:1. The present invention relates to a method for generating a multidimensional image of a sample, comprising: capturing a first two-dimensional substrate image of a surface region of the sample with a first image capture mode, wherein locations of at least one material in the surface region are captured; capturing a second two-dimensional substrate image of the surface region with a second image capture modality that is different from the first image capture modality, wherein the second image capture modality provides greater accuracy with respect to the locations of at least one material in the surface region than the first image capture mode; spatially align the first two-dimensional substrate image based on the second two-dimensional substrate image; generate a corrected first two-dimensional substrate image based at least in part on the locations of the at least one material in the second sub image. two-dimensional stratum.2. The method of any previous or next modality / feature / aspect, wherein the corrected first two-dimensional substrate image comprises a first material content determined by the second modality having greater accuracy with respect to the identification of this first material than when measured with the first modality, and a sample porosity content is determined by the first modality having greater precision with respect to the identification of porosity in the first two-dimensional image than in the second modality. The method of any preceding or following modality/resource/aspect, wherein generating comprises: identifying locations of at least one material in the first two-dimensional substrate image that correspond with locations of the at least one material in the second two-dimensional substrate image; and correcting the locations of the at least one material in the first two-dimensional substrate image that correspond to the locations of the at least one material in the second two-dimensional substrate image to generate the corrected first two-dimensional substrate image. The method of any previous or next modality / feature / aspect, further comprising: a) removing a layer of the sample in the surface region after capturing the first and second two-dimensional substrate images to expose a different surface region of the sample; b ) capturing a first two-dimensional substrate image at the different surface region with the first image capture mode; c) capturing a second two-dimensional substrate image at the different surface region with the second image capture mode; d) repeating the steps a), b), and c) a plurality of times; e) spatially align the first two-dimensional substrate image based on the second two-dimensional substrate image; f) identify, for each different surface region, the locations of the at least one material in the first two-dimensional substrate image that correspond with the locations of the at least one material in the second two-dimensional substrate image; g) correct, for each of the different surface regions, the locations of the at least one material in the first two-dimensional substrate image that correspond to the locations of the at least one material in the second two-dimensional substrate image to generate a corrected second two-dimensional substrate image; h) generate a three-dimensional substrate volume with the corrected two-dimensional substrate images.5. The method of any previous or next modality / feature / aspect, wherein the generation comprises determining a substrate porosity based on the corrected surface electron two-dimensional substrate image by comparison with the backscatter electron substrate image.6. The method of any previous or next modality / feature / aspect, wherein the first image capture modality comprises scanning said sample surface region by a beam of charged particle and recording first image data by detecting secondary electrons (surface) emitted by the sample and storing the first image data as a first set of image data corresponding to the first two-dimensional substrate image, and wherein the second image capture mode comprises: i) scanning the surface region of the sample by the beam of charged particle and recording second image data by detecting backscattered electrons emitted by the sample and storing the second image data as a second image data set corresponding to the second two-dimensional substrate image or ii) scanning the surface region of the sample by the beam of charged particle and record second image data by detecting X-rays emitted by the sample with an energy dispersive spectrometer and store the second image data as a second image data set.7. A method of creating a three-dimensional volume, comprising: capturing a plurality of surface electron two-dimensional substrate images; capturing a plurality of backscattering two-dimensional electron substrate images; determining an alignment of the plurality of electron backscatter substrate images to generate a three-dimensional volume; generating a three-dimensional substrate volume from the two-dimensional surface electron substrate images using the alignment of the plurality of two-dimensional electron backscatter substrate images. 8. The method of any previous or next modality/feature/aspect, in which the capture steps employ an electron microscope comprising a surface electron detector and a backscatter electron detector.9. The method of any preceding or following modality / feature / aspect, wherein the electron microscope is a scanning electron microscope (SEM) capable of scanning a substrate with a primary charged particle beam where the substrate emits surface electrons and separately detectable backscattered electrons.10. The method of any previous or next modality / feature / aspect, further comprising: removing a layer of the substrate after a first two-dimensional backscatter electron substrate image and a first two-dimensional electron surface substrate image are captured, and before a second two-dimensional backscatter electron substrate image and a second two-dimensional surface electron substrate image are captured.11. The method of any previous or next modality / feature / aspect, wherein the step of removing a layer is repeated after the second two-dimensional backscatter electron substrate image and the second two-dimensional surface electron substrate image are captured, and repeat the removal step after each subsequent set of surface electron and backscatter electron snaps until at least after the penultimate set of snaps.12. The method of any previous or next modality / feature / aspect, wherein removal comprises dry etching, spraying, or any combinations thereof, by a focused ion beam.13. The method of any previous or following modality / feature / aspect, further comprising: determining a substrate porosity based on a series of surface electron two-dimensional substrate images corrected by comparison with the plurality of surface electron two-dimensional substrate images backscatter.14. The method of any previous or next modality / resource / aspect, where the substrate comprises at least one rock or mineral.15. The method of any previous or next modality / resource / aspect, where the substrate is shale, mudstone, siltstone, claystone, porcelain, dolomite, or a combination thereof.16. The method of any previous or next modality/resource/aspect where the substrate comprises shale.17. The method of any previous or next modality / feature / aspect, further comprising: determining substrate organic base inclusion content from the three-dimensional backscatter electron substrate image.18. The method of any previous or next modality / resource / aspect, in which the inclusion of organic base comprises kerogen.19. The method of any preceding or following modality / feature / aspect, the method further comprising: at least one of displaying the surface electron substrate three-dimensional image and the backscatter electron substrate three-dimensional image on a screen, printing the three-dimensional image of surface electron substrate and backscatter electron substrate three-dimensional image, and store the surface electron substrate three-dimensional image and backscatter electron substrate three-dimensional image in a memory device.20. The method of any previous or next modality / feature / aspect, wherein the volume generated is from voxels having lateral lengths from about 1 nm to about 30 nm.21. The method of any previous or next modality / feature / aspect, wherein the removed layer has a thickness from about 1 nm to about 30 nm.22. A method of creating a three-dimensional volume, comprising: capturing a plurality of two-dimensional surface electron substrate images; capturing a plurality of two-dimensional electron backscatter substrate images; determining an alignment of the plurality of electron backscatter substrate images to generate a three-dimensional volume; generate a three-dimensional substrate volume from the two-dimensional backscatter electron substrate data using the alignment of the plurality of surface electron substrate images.23. A method for generating a three-dimensional digital image of a sample, comprising the steps of: a) scanning a surface of a sample by a primary electron beam generated by an electron source, where the sample comprises kerogen and minerals, and (i) recording first image data based on detecting surface electrons from the sample and storing the first image data as a first two-dimensional image comprising a grayscale value allocated to each of a plurality of pixels in the image, and (ii) ) recording second image data based on detecting backscattered electrons emitted by the sample during scanning and storing the second image data as a second two-dimensional image comprising a grayscale value allocated to each of a plurality of pixels in the image, where the first and second two-dimensional images provide a double set of image data associated with the scanned surface; b) remove a layer from of the sample by an ion beam directed at the sample to provide a different exposed surface on the sample; c) scanning the different exposed surface of the sample by the primary electron beam, and repeating steps a) (i) and a) (ii) , to provide a double set of image data associated with the different exposed surface; d) repeating step b) and step c) a plurality of times; e) stacking a plurality of the double sets of image data obtained from the steps a) and d) by positioning the respective first and second two-dimensional images in the same sequential order as obtained from the sample; f) aligning the first two-dimensional images with reference to the second two-dimensional images; g) analyzing the first and second two-dimensional images of the plurality of double sets of image data comprising allocating the pixels to porous space or kerogen to form first and second analyzed two-dimensional images; h) id identify pixels allocated to kerogen in the first analyzed two-dimensional images that are not allocated to kerogen in the second analyzed two-dimensional images in the double set of image data; and i) relocate the pixels identified in step h) to porous space in the first analyzed two-dimensional images associated with the double set of image data.24. A method for generating a three-dimensional digital image of a sample, comprising the steps of: a) scanning a surface of a sample by a primary electron beam generated by an electron source, where the sample comprises kerogen and minerals, and (i) recording first image data based on detecting surface electrons from the sample and storing the first image data as a first two-dimensional image comprising a grayscale value allocated to each of a plurality of pixels in the image, and (ii) ) recording second image data based on detecting backscattered electrons emitted by the sample during scanning and storing the second image data as a second two-dimensional image comprising a grayscale value allocated to each of a plurality of pixels in the image, where the first and second two-dimensional images provide a double set of image data associated with the scanned surface; b) remove a layer from of the sample by an ion beam directed at the sample to provide a different exposed surface on the sample; c) scanning the different exposed surface of the sample by the primary electron beam, and repeating steps a) (i) and a) (ii) , to provide a double set of image data associated with the different exposed surface; d) repeating step b) and step c) a plurality of times; e) stacking a plurality of double sets of image data obtained from steps a) and d) by positioning the respective first and second two-dimensional images in the same sequential order as obtained from the sample; f) aligning the first two-dimensional images with reference to the second two-dimensional images; g) base analyzing the first two-dimensional images of the plurality of dual sets of image data comprising segmenting the pixels into porous, kerogen, or mineral space to form first base analyzed two-dimensional images; h) first analyzing the second two-dimensional images from the plurality of dual sets of image data comprising selecting only pixels that have grayscale values exceeding a preselected grayscale threshold value for kerogen to define a first mask;i) second analyzing the second two-dimensional images of the plurality of double sets of data image ones comprising selecting only pixels that have grayscale values below a preselected grayscale threshold value for mineral to define a second mask; j) change the first two-dimensional images analyzed from base by the first mask and the second mask, comprising reallocating pixels from kerogen to porous space in the first two-dimensional images analyzed from baseline using the first mask and reallocating pixels from mineral to kerogen in the first two-dimensional images analyzed from baseline using the second mask.25. The method of any previous or next modality / feature / aspect, wherein removing the layer in step b) comprises milling ions through the sample in a direction approximately perpendicular to an exposed anterior surface of the sample to remove a layer of approximately uniform thickness from about 1 nm to about 5 nm.26. The method of any previous or next modality / resource / aspect, where the sample comprises at least one rock or mineral.27. The method of any previous or next modality / feature / aspect, where the sample is shale, clay, siltstone, claystone, porcelain, dolomite, or a combination thereof.28. The method of any previous or next modality/resource/aspect, which further comprises step k), calculate percentage total pore space and percentage total kerogen for reconciled sample images produced through step j).29. A system for generating three-dimensional digital images of a sample, comprising: a) a charged particle microscope comprising: a scanning electron beam column comprising an electron source for generating a primary electron beam, an ion beam column for generate a focused ion beam through a sample to successively remove a thin layer of it in the direction of the sample thickness and expose a different surface of the sample for analysis through a primary electron beam, a first charged particle detector to detect electrons of the sample surface when scanned with the primary electron beam, a second charged particle detector to detect backscattered electrons emitted by the scanned sample b) a first signal processing system for recording first image data based on detected sample surface electrons by the first charged particle detector and store the first ones. image data as a first two-dimensional image comprising a grayscale value allocated to each of a plurality of pixels in the image, and a second signal processing system for recording second image data based on backscattered electrons emitted by the sample during scanning which are detected by the second charged particle detector and storing the second image data as a second two-dimensional image comprising a grayscale value allocated to each of a plurality of pixels in the image, wherein the first and second two-dimensional images provide a double set of image data associated with the different exposed surface; c) a computer comprising at least one processor operable for executing a computer program capable of performing the calculations for creating a three-dimensional digital representation of the sample, in that the calculations comprise: stacking a plurality of double data sets s of images obtained by the first and second processing systems by positioning the respective first and second two-dimensional images in sequential order as obtained from the in-aligned sample, basely analyzing the first two-dimensional images of the plurality of double sets of image data comprising allocating pixels to porous space, kerogen, or mineral to form base analyzed first two-dimensional images, first analyzing second two-dimensional images from the plurality of dual image datasets comprising selecting only pixels that have grayscale values exceeding a threshold value from pre-selected grayscale to kerogen to define a first mask, second analyzing the second two-dimensional images from a plurality of dual image data sets comprising selecting only pixels that have grayscale values below a threshold scale value gray pre-se taught for mineral to define a second mask, change the first two-dimensional images analyzed from base by the first mask and the second mask, comprising relocating pixels from kerogen to porous space in the first two-dimensional images analyzed from base using the first mask and relocating pixels to from mineral to kerogen in the first two-dimensional images analyzed from baseline using the second mask.
[063] The present invention may include any combination of these various features or embodiments above and/or below as set out in sentences and/or paragraphs. Any combination of features described herein is considered part of the present invention and is not intended to be limiting with respect to combinable features.
[064] Applicants specifically incorporate the entire content of all references cited in this disclosure. Furthermore, when an amount, concentration, or other value or parameter is given as a range, preferred range, or a list of higher preferred values and lower preferred values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper end of the range or preferred value and any lower end of the range or preferred value, regardless of whether scales are separately disclosed. When a range of numerical values is described herein, unless otherwise indicated, the range is intended to include the ends of these, and all integers and fractions within the range. The scope of the invention is not intended to be limited to the specific values recited in defining a range.
[065] It is evident to those skilled in the art that various modifications and variations can be made to the embodiments of the present invention without departing from the spirit or scope of the present invention. Thus, it is intended that the present invention encompass other modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.

权利要求:
Claims (24)
[0001]
1. Method for generating a multidimensional image of a sample, characterized in that it comprises: capturing a first two-dimensional substrate image of a surface region of the sample with a first image capture mode, wherein the first two-dimensional substrate image is a two-dimensional surface electron substrate image and where locations of at least one material in the surface region are captured; capturing a second two-dimensional substrate image of the surface region with a second image capture mode that is different from the first mode of image capture, wherein the second image capture modality provides greater accuracy with respect to the locations of at least one material in the surface region than the first image capture modality; spatially aligning the first two-dimensional substrate image based on the second two-dimensional substrate image; generate a first two-dimensional substrate image; dimensional corrected based at least in part on the locations of the at least one material in the second two-dimensional substrate image, the generation comprising determining a substrate porosity based on the two-dimensional surface-corrected electron substrate image by comparison with the second image of two-dimensional substrate.
[0002]
2. Method according to claim 1, characterized in that the first corrected two-dimensional substrate image comprises a first material content determined by the second modality having greater accuracy with regard to the identification of this first material than when measured with the first modality, and a porosity content of the sample is determined by the first modality having greater accuracy with respect to the identification of porosity in the first two-dimensional image than in the second modality.
[0003]
3. Method according to claim 1, characterized in that said generation comprises: identifying locations of at least one material in the first two-dimensional substrate image that correspond with the locations of the at least one material in the second two-dimensional substrate image; and correcting the locations of the at least one material in the first two-dimensional substrate image that correspond to the locations of the at least one material in the second two-dimensional substrate image to generate the corrected first two-dimensional substrate image.
[0004]
4. Method according to claim 3, further comprising: a) removing a layer of the sample in the surface region after capturing the first and second two-dimensional substrate images to expose a different surface region of the sample; b) capturing a first two-dimensional substrate image at the different surface region with the first image capture mode; c) capturing a second two-dimensional substrate image at the different surface region with the second image capture mode; d) repeating the steps a), b), and c) a plurality of times; e) spatially align the first two-dimensional substrate image based on the second two-dimensional substrate image; f) identify, for each different surface region, the locations of the at least one material in the first two-dimensional substrate image that correspond with the locations of the at least one material in the second two-dimensional substrate image; g) correct, to each of the different surface regions, the locations of the at least one material in the first two-dimensional substrate image that correspond to the locations of the at least one material in the second two-dimensional substrate image to generate a corrected second two-dimensional substrate image; h) generating a three-dimensional substrate volume with the corrected two-dimensional substrate images.
[0005]
5. Method according to claim 1, characterized in that the first image capture mode comprises scanning said sample surface region by a charged particle beam and recording first image data by detecting secondary electrons (surface) emitted by said sample and storing said first image data as a first set of image data corresponding to the first two-dimensional substrate image, and wherein the second image capture mode comprises: i) scanning said surface region of the sample by charged particle beam and recording second image data by detecting backscattered electrons emitted by said sample and storing said second image data as a second image data set corresponding to the second two-dimensional substrate image or ii) scanning said region sample surface by charged particle beam and record second image data by detecting x-rays emitted by said sample with an energy dispersive spectrometer and storing said second image data as a second set of image data.
[0006]
6. Method of creating a three-dimensional volume, characterized in that it comprises: capturing a plurality of surface electron two-dimensional substrate images; capturing a plurality of backscatter electron two-dimensional substrate images; removing a substrate layer after a first image two-dimensional surface electron substrate image and a first two-dimensional electron backscatter substrate image are captured, and before a second two-dimensional surface electron substrate image and a second two-dimensional electron backscatter substrate image are captured, in which the one-layer removal step is repeated after the second two-dimensional surface electron substrate image and the second two-dimensional backscatter electron substrate image are captured, and repeating the removal step after each subsequent set of electron image captures surface and and backscattering electron until at least after the penultimate set of image captures; determining an alignment of a plurality of electron backscatter substrate images to generate a three-dimensional volume; generating a three-dimensional substrate volume from the two-dimensional electron substrate images surface using alignment of the plurality of two-dimensional backscatter electron substrate images; determine a substrate porosity based on a series of two-dimensional surface electron substrate images corrected by comparison with the plurality of two-dimensional backscatter electron substrate images .
[0007]
7. Method according to claim 6, characterized in that the capture steps employ an electron microscope comprising a surface electron detector and a backscatter electron detector.
[0008]
8. Method according to claim 7, characterized in that the electron microscope is a scanning electron microscope (SEM) capable of scanning a substrate with a primary charged particle beam in which the substrate emits surface electrons and separately detectable backscattered electrons.
[0009]
9. Method according to claim 6, characterized in that the removal comprises dry etching, spraying, or any combination thereof, by a focused ion beam.
[0010]
10. Method according to claim 6, characterized in that the substrate comprises at least one rock or mineral.
[0011]
11. Method according to claim 6, characterized in that the substrate is shale, mudstone, siltstone, claystone, porcelain, dolomite, or a combination thereof.
[0012]
12. Method according to claim 6, characterized in that the substrate comprises shale.
[0013]
13. Method according to claim 6, characterized in that it further comprises: determining organic base inclusion content of the substrate from the three-dimensional backscatter electron substrate image.
[0014]
14. Method according to claim 13, characterized in that the inclusion of organic base comprises kerogen.
[0015]
15. The method of claim 6, further comprising: at least one of displaying the surface electron substrate three-dimensional image and the backscatter electron substrate three-dimensional image on a screen, printing the three-dimensional image of surface electron substrate and backscatter electron substrate three-dimensional image, and store the surface electron substrate three-dimensional image and backscatter electron substrate three-dimensional image in a memory device.
[0016]
16. Method according to claim 6, characterized in that the volume generated is from voxels having lateral lengths from about 1 nm to about 30 nm.
[0017]
17. Method according to claim 16, characterized in that the removed layer has a thickness from about 1 nm to about 30 nm.
[0018]
18. Method for generating a three-dimensional digital image of a sample, characterized in that it comprises the steps of: a) scanning a surface of a sample by a primary electron beam generated by an electron source, where the sample comprises kerogen and minerals, and (i) recording first image data based on detecting surface electrons of the sample and storing the first image data as a first two-dimensional image comprising a gray scale value allocated to each of a plurality of pixels in the image , and (ii) recording second image data based on detecting backscattered electrons emitted by said sample during said scan and storing the second image data as a second two-dimensional image comprising a gray scale value allocated to each of a plurality of pixels in the image, where the first and second two-dimensional images provide a double set of image data associated with the reference. from the scanned surface; b) removing a layer from the sample by an ion beam directed at said sample to provide a different exposed surface on the sample; c) scanning said different exposed surface from said sample by the primary electron beam, and repeating steps a) (i) and a) (ii) to provide a double set of image data associated with said different exposed surface; d) repeating said step b) and said step c) a plurality of times; ) stacking a plurality of double sets of image data obtained from steps a) and d) by positioning the respective first and second two-dimensional images in the same sequential order as obtained from the sample; f) aligning the first two-dimensional images by referring to said second two-dimensional images; g) analyzing said first and second two-dimensional images of said plurality of dual image data sets comprising and allocate said porous space pixels or kerogen to form first and second analyzed two-dimensional images; h) identify pixels allocated to kerogen in the first analyzed two-dimensional images that are not allocated to kerogen in the second analyzed two-dimensional images in said double set of image data; ei) reallocating the pixels identified in step h) to porous space in the first analyzed two-dimensional images associated with said double set of image data.
[0019]
19. Method for generating a three-dimensional digital image of a sample, characterized in that it comprises the steps of: a) scanning a surface of a sample by a primary electron beam generated by an electron source, in which the sample comprises pores , kerogen and minerals, and (i) recording first image data based on sample surface electron detection and storing the first image data as a first two-dimensional image comprising a grayscale value allocated to each of a plurality of pixels in the image, and (ii) recording second image data based on detecting backscattered electrons emitted by said sample during said scan and storing the second image data as a second two-dimensional image comprising a gray scale value allocated to each of a plurality of pixels in the image, wherein the first and second two-dimensional images provide a double set of image data associated with said surface being scanned; b) removing a layer from the sample by an ion beam directed at said sample to provide a different exposed surface on the sample; c) scanning said exposed surface different from said sample by the primary electron beam, and repeating steps a) (i) and a) (ii) to provide a double set of image data associated with said different exposed surface; d) repeating said step b) and said step c) a plurality of times; e) stacking a plurality of double sets of image data obtained from steps a) and d) by positioning the respective first and second two-dimensional images in the same sequential order as obtained from the sample; f) aligning the first two-dimensional images by referring to said second two-dimensional images; g) analyzing based on said first two-dimensional images of said plurality of dual image data sets comprising segmenting said pixels to porous, kerogen, or mineral space to form base analyzed first two-dimensional images; h) first analyzing said second two-dimensional images from said plurality of dual image data sets comprising selecting only pixels having gray scale values greater than a pre-selected gray scale threshold value for kerogen to define a first mask; i) second analyzing said second two-dimensional images from said plurality of dual image data sets comprising selecting only pixels having gray scale values below a pre-selected grayscale threshold value for mineral to define a second mask; j) altering said first two-dimensional images analyzed from baseline by the first mask and the second mask, comprising reallocating pixels from kerogen to porous space in the first two-dimensional images Baseline analyzed using the first mask and reallocating pixels from mineral to kerogen in the first two-dimensional images analyzed from baseline using the second mask.
[0020]
20. Method according to claim 19, characterized in that removing the layer in step b) comprises grinding ions across said sample in a direction approximately perpendicular to the previous exposed surface of the sample to remove a layer of approximately uniform thickness from about 1 nm to about 5 nm.
[0021]
21. Method according to claim 19, characterized in that the sample comprises at least one rock or mineral.
[0022]
22. Method according to claim 19, characterized in that the sample is shale, mudstone, siltstone, claystone, porcelain, dolomite, or a combination thereof.
[0023]
23. Method according to claim 19, characterized in that it further comprises step k), calculating percentage of total pore space and percentage of total kerogen for reconciled images of the sample produced by step j).
[0024]
24. A system for generating three-dimensional digital images of a sample, characterized in that it comprises: a) a charged particle microscope comprising: a scanning electron beam column comprising an electron source for generating a primary electron beam, a ion beam column to generate a focused ion beam through a sample to successively remove a thin layer of it in the direction of the sample thickness and expose a different surface of the sample for analysis through a primary electron beam, a first detector charged particle detector to detect surface electrons of the sample when scanned with the primary electron beam, a second charged particle detector to detect backscattered electrons emitted by the scanned sampleb) a first signal processing system for recording first image data based on sample surface electrons detected by said first particle detector. loaded cell and storing the first image data as a first two-dimensional image comprising a grayscale value allocated to each of a plurality of pixels in the image, and a second signal processing system for recording second electron-based image data backscatters emitted by said sample during said scan which are detected by said second charged particle detector and store the second image data as a second two-dimensional image comprising a gray scale value allocated to each of a plurality of pixels in the image, wherein the first and second two-dimensional images provide a dual set of image data associated with said different exposed surface; c) a computer comprising at least one processor operable for executing instructions capable of performing the calculations for creating a digital representation three-dimensional sample, in which such calculations c comprise: stacking a plurality of double sets of image data obtained by the first and second processing systems by positioning the respective first and second two-dimensional images in sequential order as obtained from the in-aligned sample, basely analyzing said first two-dimensional images of the said plurality of dual image data sets comprising allocating said pixels to porous, kerogen, or mineral space to form base analyzed first two-dimensional images, first analyzing said second two-dimensional images from said plurality of dual image data sets comprising selecting pixels only having grayscale values greater than a preselected grayscale threshold value for kerogen to define a first mask, according to analyzing said second two-dimensional images of said plurality of dual image data sets comprising having to select only pixels that have grayscale values below a preselected grayscale threshold value for mineral to define a second mask, and altering said first two-dimensional images base analyzed by the first mask and the second mask, comprising relocating pixels from kerogen to porous space in the first two-dimensional images analyzed from baseline using the first mask and reallocate pixels from mineral to kerogen in the first two-dimensional images analyzed from baseline using the second mask.

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BR112014009093A2|2017-04-18|

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CA2850799A1|2013-04-18|

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AU2012322799A1|2014-05-01|

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EP2748793B1|2017-10-11|

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RU2014119260A|2015-11-20|

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NO2730510T3|2018-01-27|

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EP2748793A1|2014-07-02|

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RU2610216C2|2017-02-08|

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WO2013055876A1|2013-04-18|

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法律状态:
2018-12-11| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|

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2019-11-05| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|

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2021-07-06| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2021-08-17| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 11/10/2012, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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US201161547090P| true| 2011-10-14|2011-10-14|

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US61/547,090|2011-10-14|

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PCT/US2012/059689|WO2013055876A1|2011-10-14|2012-10-11|Dual image method and system for generating a multi-dimensional image of a sample|

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