This application claims benefit of priority under 35 U.S.C. § 119 to European
Patent Application number EP22186329.3, filed Jul. 21, 2022, the entire contents of this application being incorporated herein by reference.
The invention relates to a method of examining a sample using a charged particle microscope, comprising the steps of detecting using a first detector emissions of a first type from the sample in response to a charged particle beam scanned over the area of the sample, and using spectral information of detected emissions of the first type for examining said sample.
Charged particle microscopy is a well-known and increasingly important technique for imaging microscopic objects, particularly in the form of electron microscopy. Historically, the basic genus of electron microscope has undergone evolution into a number of well-known apparatus species, such as the Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM), and Scanning Transmission Electron Microscope (STEM), and also into various sub-species, such as so-called “dual-beam” apparatus (e.g. a FIB-SEM), which additionally employ a “machining” Focused Ion Beam (FIB), allowing supportive activities such as ion-beam milling or Ion-Beam-Induced Deposition (IBID), for example. The skilled person will be familiar with the different species of charged particle microscopy.
Irradiation of a sample by a scanning electron beam precipitates emanation of “auxiliary” radiation from the sample, in the form of secondary electrons, backscattered electrons, X-rays and cathodoluminescence (infrared, visible and/or ultraviolet photons). One or more components of this emanating radiation may be detected and used for sample analysis.
Typically, in a SEM backscattered electrons are detected by a solid state detector in which each backscattered electron is amplified as it creates many electron-hole pairs in a semiconductor detector. The backscattered electron detector signal is used to form an image as the beam is scanned, with the brightness of each image point determined by the number of backscattered electrons detected at the corresponding point on the sample as the primary beam moves across the sample. The image merely provides information on the topology of the sample to be examined.
In a process called “energy dispersive x-ray spectroscopy” or “EDS”, the energies of x-rays coming from the sample in response to the electron beam are measured and plotted in a histogram to form a material specific spectrum. The measured spectrum can be compared to known spectra of various elements to determine which elements and minerals are present in said sample.
During EDS mapping individual x-ray counts are detected and registered to the pixel they have originated from. As an EDS spectrum can be processed to get chemical composition (or chemical characterization of a sample, in general), it is (in principle) possible to calculate the concentration of a single element for each pixel and display this in an element map. Typically, a grid with discrete analysis points is used. The electron beam dwells on each analysis point while the EDS detectors record x-rays. Once sufficient x-ray counts are recorded the beam moves to the next analysis point. The signal from the EDS detectors is fed to a signal processing unit that builds an x-ray spectrum curve for each analysis point, which can be matched to an extensive library of known mineral phases to select the best match for that analysis point. Quantification requires spectra with enough counts to get accurate results and acquiring dense spectra is time-consuming and not always possible. Because of that the counts from several close pixels are often binned together, sacrificing spatial resolution for chemical accuracy. The optimal size of this binning depends on total amount of data and use-case. Larger bins produce images with lower spatial resolution but also lower noise.
It is an object of the present invention to provide an improved method of examining a sample using a charged particle microscope, wherein spectral information of detected emissions is used for examining said sample. In particular, it is an object of the present invention to provide a method and apparatus for more rapidly and more accurately acquiring information about a sample.
To this end, the invention provides a method of examining a sample using a charged particle microscope as defined in claim 1.
The method as defined herein comprises the steps of providing a charged particle beam and scanning said beam over an area of the sample, detecting spectral emissions from the sample in response to the charged particle beam being scanned over the area of the sample, and identifying a first plurality of substantially similar spectral emissions, at different points of the scan, and determining a first chemical element associated with said first plurality of substantially similar spectral emissions.
The method as defined herein is characterized by the step of providing a first base spectral number value associated with said first determined chemical element. This first base spectral number value is related to the number of similar spectral emissions that are required for confidently determining said first chemical element.
The method as defined herein is further characterized by the step of dividing at least a part of the scanned area of the sample into a first number of segments associated with said first chemical element, wherein said first base spectral number value is used for defining a size of each of said first number of segments.
The method further provides a graphical representation of the sample, wherein said graphical representation includes said first chemical element and corresponding segments.
In this method, the first base spectral number value thus acts as a binning parameter that determines the substantially optimal size of binning for the first determined chemical element. Inventors realized that this binning parameter may be different for different chemical elements. The inventors found that the error in quantification is proportional to the (square root of the) absolute number of counts in an element's peak (net counts). Thus, net counts can be used as a criterion for segment activation. This way, elements with a variable concentration are rendered in with high resolution in high concentration areas, and with lower resolution in lower concentration areas. Additionally, the method allows trace elements to be correctly displayed.
Advantageous embodiments are described below.
A method according to claim 1, further comprising:
The method may comprise the step of identifying a second plurality of substantially similar spectral emissions and determining a second chemical element associated with said second plurality of substantially similar spectral emissions. Then, a second base spectral number value associated with said second determined chemical element may be provided, wherein said second base spectral number value is related to the number of similar spectral emissions that are required for confidently determining said second chemical element. With this, at least a part of the scanned area of the sample may be divided into a second number of segments associated with said second chemical element, wherein said second base spectral number value is used for defining a size of each of said second number of segments.
The second base spectral number value may differ from said first base spectral number value, and said size of each of said second number of segments may differ from said size of each of said first number of segments. This means that segments can vary in size, not only within the first number of segments, but only between the first number and the second number of segments.
When at least a plurality of chemical elements are to be identified, the method may comprise the step of identifying at least one further plurality of substantially similar spectral emissions and determining a further chemical element associated with said further plurality of substantially similar spectral emissions. The method may then comprise the step of providing, for each of the at least one further chemical elements, a respective further base spectral number value associated with said respective further determined chemical element, wherein said respective further base spectral number value is related to the number of similar spectral emissions that are required for confidently determining said respective further chemical element. Finally, at least a part of the scanned area of the sample may be divided into a corresponding set of further number of segments, each set associated with a respective further chemical element, wherein said further base spectral number value is used for defining a size of each of said corresponding further number of segments.
In effect, the use of a first, second, and/or further base spectral number value, which may be different for the first, second, and/or further chemical elements, leads to the selection of different spatial resolution separately for each element based on its presence.
It is noted that the method may comprise the step of updating and/or modifying at least one segment in response to the beam being scanned over the sample. Thus, as more data is coming in, the size and shape of segments can be changed and/or updated to improve the accuracy of the graphical representation.
According to an aspect of the invention, a charged particle microscope for examining a sample using the method as described above is provided. The apparatus as defined herein comprises:
According to the invention, said charged particle microscope is arranged for executing the method according to the invention. Thus, an apparatus is obtained with which information about the sample can be acquired in a more rapid and/or more accurate way. Thus, the object of the invention is achieved.
The invention will now be elucidated in more detail on the basis of exemplary embodiments and the accompanying schematic drawings, in which:
The sample S is held on a sample holder H that can be positioned in multiple degrees of freedom by a positioning device/stage A, which moves a cradle A′ into which holder H is (removably) affixed; for example, the sample holder H may comprise a finger that can be moved (inter alia) in the XY plane (see the depicted Cartesian coordinate system; typically, motion parallel to Z and tilt about X/Y will also be possible). Such movement allows different parts of the sample S to be illuminated/imaged/inspected by the electron beam B traveling along axis B′ (in the Z direction) (and/or allows scanning motion to be performed, as an alternative to beam scanning). If desired, an optional cooling device (not depicted) can be brought into intimate thermal contact with the sample holder H, so as to maintain it (and the sample S thereupon) at cryogenic temperatures, for example.
The electron beam B will interact with the sample S in such a manner as to cause various types of “stimulated” radiation to emanate from the sample S, including (for example) secondary electrons, backscattered electrons, X-rays and optical radiation (cathodoluminescence). If desired, one or more of these radiation types can be detected with the aid of analysis device 22, which might be a combined scintillator/photomultiplier or EDX (Energy-Dispersive X-Ray Spectroscopy) module, for instance; in such a case, an image could be constructed using basically the same principle as in a SEM. However, alternatively or supplementally, one can study electrons that traverse (pass through) the sample S, exit/emanate from it and continue to propagate (substantially, though generally with some deflection/scattering) along axis B′. Such a transmitted electron flux enters an imaging system (projection lens) 24, which will generally comprise a variety of electrostatic/magnetic lenses, deflectors, correctors (such as stigmators), etc. In normal (non-scanning) TEM mode, this imaging system 24 can focus the transmitted electron flux onto a fluorescent screen 26, which, if desired, can be retracted/withdrawn (as schematically indicated by arrows 26′) so as to get it out of the way of axis B′. An image (or diffractogram) of (part of) the sample S will be formed by imaging system 24 on screen 26, and this may be viewed through viewing port 28 located in a suitable part of a wall of enclosure 2. The retraction mechanism for screen 26 may, for example, be mechanical and/or electrical in nature, and is not depicted here.
As an alternative to viewing an image on screen 26, one can instead make use of the fact that the depth of focus of the electron flux leaving imaging system 24 is generally quite large (e.g. of the order of 1 meter). Consequently, various other types of analysis apparatus can be used downstream of screen 26, such as:
It should be noted that the order/location of items 30, 32 and 34 is not strict, and many possible variations are conceivable. For example, spectroscopic apparatus 34 can also be integrated into the imaging system 24.
In the embodiment shown, the microscope M further comprises a retractable X-ray Computed Tomography (CT) module, generally indicated by reference 40. In Computed Tomography (also referred to as tomographic imaging) the source and (diametrically opposed) detector are used to look through the sample along different lines of sight, so as to acquire penetrative observations of the sample from a variety of perspectives.
Note that the controller (computer processor) 20 is connected to various illustrated components via control lines (buses) 20′. This controller 20 can provide a variety of functions, such as synchronizing actions, providing setpoints, processing signals, performing calculations, and displaying messages/information on a display device (not depicted). Needless to say, the (schematically depicted) controller 20 may be (partially) inside or outside the enclosure 2, and may have a unitary or composite structure, as desired.
The skilled artisan will understand that the interior of the enclosure 2 does not have to be kept at a strict vacuum; for example, in a so-called “Environmental TEM/STEM”, a background atmosphere of a given gas is deliberately introduced/maintained within the enclosure 2. The skilled artisan will also understand that, in practice, it may be advantageous to confine the volume of enclosure 2 so that, where possible, it essentially hugs the axis B′, taking the form of a small tube (e.g. of the order of 1 cm in diameter) through which the employed electron beam passes, but widening out to accommodate structures such as the source 4, sample holder H, screen 26, camera 30, camera 32, spectroscopic apparatus 34, etc.
The charged particle microscope M according to the invention, and of which an embodiment is shown in
Now first referring to
Thus the charged particle microscope M as shown in
The apparatus shown in
Now referring to
The area 50 of the sample is scanned with a beam of charged particles. The first detector, for example an EDS detector as described with reference to
In the embodiment shown, a subsequent step is to provide a first base spectral number value associated with said first determined chemical element, wherein said first base spectral number value is related to the number of similar spectral emissions that are required for confidently determining said first chemical element. In this embodiment, a further step of providing a second base spectral number value associated with said second determined chemical element as well. The first and second base spectral number value may be provided by means of a look-up table. For example, and using controller/processor 20 of the charged particle microscope M. The first and second base spectral number value may, and in practice will, be non-identical to each other. The first and second base spectral number value indicate how many events are needed to confidently indicate the presence of a first and second chemical element, respectively. When the first base spectral number value is lower than the second base spectral number value, it means that less events are needed for confidently identifying the first chemical element compared to the second chemical element. According to the method as defined herein, the scanned area of the sample is divided into a first number of segments associated with said first chemical element, wherein said first base spectral number value is used for defining a size of each of said first number of segments. In the embodiment shown, the scanned area of the sample is also divided into a second number of segments associated with said second chemical element, wherein said second base spectral number value is used for defining a size of each of said second number of segments.
This aspect of the method as defined herein is shown in the right-hand side of
This means that as data is coming in (as indicated from top to bottom, left-hand side of
One skilled in the art will understand that the acquired data 54a, 54b can, in principle have many values (not only black or white), and that the representation values can be arbitrarily selected in dependence of the desired application. This means that further chemical elements may be present, each of which has it's own respective further base spectral number value that can be used to create segments. The example shown is merely an illustration of a single possibility and is not intended to be limited.
Now, as the number of data points 54a, 54b increases (in the sequence of
Note that, even though the base spectral number value for the white dots is equal to “2”, and the same number is used to create segments 154a, 155a, the actual size of the different segments 154a, 155a can vary.
Thus, it can be seen that the granularity and accuracy of the represented data (right hand side) increases as more data points are acquired: the image becomes more detailed and contains more information. Note also that segments previously indicated as being “white” can be changed (partly) into “black”. Notice that cluster 56b (a group of four black dots, being equal to the base spectral number value) is used to generate a further segment 156b in the graphical representation. Similarly, the two white dots 56a are equal to the base spectral number value for white and can be grouped, thus leading to segment 156a. Thus, the size and number of the segments may vary. In the particular example a single, irregular black segment is formed, due to the fact that most black dots are seemingly connected to each other. This may vary, in practice, of course, and this will be understood by those skilled in the art.
It is conceivable that the area 50 to be scanned is scanned multiple times to obtain the desired data quantity. Scanning multiple times may include scanning only a part of the area 50 of the sample. For example it is conceivable that, based on a first scan (or first set of scans), regions of interest and regions of non-interest are defined, and that only regions of interest are scanned in a second scan (or second set of scans). This increases the efficiency of the method. In particular, the regions of interest may be defined using the data obtained from the emissions of the second type, i.e. the EM data may be used to define regions of interest that are in particular scanned for obtaining EDS data.
The invention has been explained above by means of several embodiments. The desired protection is defined by the attached claims.
Number | Date | Country | Kind |
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22186329.3 | Jul 2022 | EP | regional |