# US 11,310,438 B2 · System, apparatus, and method for determining elemental composition using 4D STEM

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- Number: US 11,310,438 B2
- Document ID: US11310438B2
- Status: Granted
- Kind: B2
- Application number: 16/851,835
- Filed: 2020-04-17
- Published: 2020-10-22
- Granted: 2022-04-19
- Earliest claimed: 2019-04-19
- Assignees: Direct Electron, LP
- Applicants: Direct Electron, LP
- Inventors: Benjamin Bammes; Robert Bilhorn
- Web page: https://patentgrep.com/patent/US11310438B2

## CPC

- H01J 37/244: Detectors; Associated components or circuits therefor
- H04N 23/741: by increasing the dynamic range of the image compared to the dynamic range of the electronic image sensors
- G01N 23/2251: using incident electron beams, e.g. scanning electron microscopy [SEM]
- H01J 37/28: with scanning beams {(H01J37/268, H01J37/292, H01J37/2955 take precedence)}
- H04N 5/00: Details of television systems (scanning details or combination thereof with generation of supply voltages H04N3/00)
- H04N 23/667: Camera operation mode switching, e.g. between still and video, sport and normal or high- and low-resolution modes
- H04N 23/81: for suppressing or minimising disturbance in the image signal generation
- H04N 25/445: by skipping some contiguous pixels within the read portion of the array
- H04N 25/531: by controlling rolling shutters in CMOS SSIS
- H04N 25/673: by using reference sources
- G01N 2223/6126: tissue
- H01J 2237/2441: Semiconductor detectors, e.g. diodes
- H01J 2237/2446: Position sensitive detectors
- H01J 2237/24592: Inspection and quality control of devices
- H01J 2237/2802: Transmission microscopes
- H01J 2237/2806: Secondary charged particle
- H01J 2237/2817: Pattern inspection
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- H04N: PICTORIAL COMMUNICATION, e.g. TELEVISION
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

The present disclosure relates to transmission electron microscopy for evaluation of biological matter. According to an embodiment, the present disclosure further relates to an apparatus for determining the structure and/or elemental composition of a sample using 4D STEM, comprising a direct bombardment detector operating with global shutter readout, processing circuitry configured to acquire images of bright-field disks using either a contiguous array or non-contiguous array of detector pixel elements, correct distortions in the images, align each image of the images based on a centroid of the bright-field disk, calculate a radial profile of the images, normalize the radial profiles by a scaling factor, calculate the rotationally-averaged edge profile of the bright-field disk, and determine elemental composition within the specimen based on the characteristics of the edge profile of the bright-field disk corresponding to each specimen location.

## Claims

### Claim 1

A method for determining material properties of a sample using 4D STEM, comprising:
directing an electron beam from an electron source toward the sample;
detecting electrons of the electron beam interacting with the sample via an electron detector including an array of detector elements;
acquiring, from the electron detector, images of bright-field disks and surrounding dark-field diffraction based on the detected electrons; and
determining an elemental composition of the sample based on the acquired images of the bright-field disks and the surrounding dark-field diffractions,
wherein the detecting detects the electrons using the electron detector in a global shutter readout mode, and synchronizes each acquired image from the electron detector with a movement of a probe directing the electron beam.

### Claim 2 (depends on 1)

The method according to claim 1, further comprising:
correcting distortions in the acquired images.

### Claim 3 (depends on 2)

The method according to claim 2, wherein the determining of the elemental composition of the sample based on the acquired images of the bright-field disks and the surrounding dark-field diffractions further comprises:
calculating a radial profile of the distortion-corrected acquired images;
normalizing the radial profile by a scaling factor;
determining a shape of the radial profile at an edge of the bright-field disks; and
determining the elemental composition based on the shape of the radial profile at the edge of the bright-field disks.

### Claim 4 (depends on 2)

The method according to claim 2, wherein the distortions in the acquired images are geometric and the correcting of the geometric distortions includes fitting an ellipse to the bright-field disks.

### Claim 5 (depends on 3)

The method according to claim 3, wherein the radial profile is normalized based on an average intensity of the bright-field disks.

### Claim 6 (depends on 1)

The method according to claim 1, further comprising:
aligning each image of the images of the bright-field disks with one another based on a center of each of the bright-field disks.

### Claim 7 (depends on 3)

The method according to claim 3, where the shape of the radial profile corresponds to a slope of the radial profile for a transition between areas of the bright-field disks and the surrounding dark-field diffractions.
