Methods and systems for acquiring three-dimensional electron diffraction data

Patent metadata

Field	Value
Publication number	US-11815476-B2
Application number	US-202117217103-A
Country	US
Kind code	B2
Filing date	Mar 30, 2021
Priority date	Mar 30, 2021
Publication date	Nov 14, 2023
Grant date	Nov 14, 2023

Abstract

Crystallographic information of crystalline sample can be determined from one or more three-dimensional diffraction pattern datasets generated based on diffraction patterns collected from multiple crystals. The crystals for diffraction pattern acquisition may be selected based on a sample image. At a location of each selected crystal, multiple diffraction patterns of the crystal are acquired at different angles of incidence by tilting the electron beam, wherein the sample is not rotated while the electron beam is directed at the selected crystal.

First claim

What is claimed is:

1. A method, comprising:
acquiring a sample image of a sample;
selecting multiple crystals in the sample image;
determining coordinates of the multiple selected crystals;
directing an electron beam towards each of the multiple selected crystals and acquiring multiple diffraction patterns from the multiple selected crystals without rotating or moving the sample, wherein at a location of each of the multiple selected crystals, adjusting the electron beam to acquire multiple diffraction patterns of the selected crystal at different incident angles; and
extracting crystallographic information from the multiple diffraction patterns.

2. The method of claim 1 , wherein acquiring multiple diffraction patterns of the selected crystal at different incident angles by tilting the electron beam includes acquiring the multiple diffraction patterns while continuously tilting the electron beam.

3. The method of claim 1 , wherein acquiring multiple diffraction patterns of the selected crystal at different incident angles includes acquiring multiple diffraction patterns of the selected crystal with the incident angles from −10 to 10 degrees relative to an optical axis.

4. The method of claim 1 , wherein acquiring multiple diffraction patterns of the selected crystal at different incident angles includes acquiring multiple diffraction patterns of the selected crystal with the incident angles in a range of less than 20 degrees.

5. The method of claim 1 , wherein selecting the multiple crystals in the sample image includes selecting the multiple crystals based on one or more of a size, a morphology, a distribution and a contrast of the crystals in the sample image.

6. The method of claim 1 , further comprising calibrating beam location relative to the sample before directing the electron beam towards one of the selected crystals.

7. The method of claim 6 , wherein calibrating beam location includes acquiring a second sample image with a field of view smaller than the sample image, determining a beam displacement by comparing the second sample image with the sample image, and calibrating the beam location based on the beam displacement.

8. The method of claim 1 , further comprising:
acquiring multiple diffraction patterns at multiple scanning locations within a field of view of the sample image;
generating a diffraction score for each of the multiple diffraction patterns;
generating a diffraction heatmap based on the diffraction scores; and
determining coordinates of the multiple selected crystals based further on the diffraction heatmap.

9. The method of claim 8 , wherein determining coordinates of the multiple selected crystals based further on the diffraction heatmap includes determining coordinates of one or more sub-regions of at least one of the multiple selected crystals based on the diffraction heatmap.

10. The method of claim 1 , wherein acquiring multiple diffraction patterns of the selected crystal at different incident angles by tilting the electron beam includes acquiring the multiple diffractions patterns of the selected crystal by tilting the electron beam in at least a plane orthogonal to a specimen plane.

11. The method of claim 1 , further comprising:
after acquiring the sample image, adjusting a sample position by translating a sample holder; and
calibrating a beam location relative to the sample after adjusting the sample position, and wherein directing the electron beam towards each selected crystal includes directing the electron beam based on the coordinates of the selected crystals and the calibrated beam location.

12. A system, comprising:
an electron source for generating an electron beam along an optical axis;
a sample holder for holding a sample and adjusting a sample position;
a deflector for shifting the electron beam to irradiate different locations of the sample and tilting the electron beam to adjust an incident angle;
a detector for detecting electrons transmitted through the sample; and
a controller including a non-transitory memory for storing computer readable instructions, wherein by executing the computer readable instructions, the controller is configured to:
acquire a sample image of the sample;
select multiple crystals in the sample image;
determine coordinates of the multiple selected crystals;
direct the electron beam towards each of the multiple selected crystals by shifting the electron beam and acquire multiple diffraction patterns from the multiple selected crystals without moving or rotator the sample via the sample holder, wherein at a location of each selected crystal, tilt the electron beam to acquire multiple diffraction patterns of the selected crystal at different incident angles;
merge multiple diffraction patterns of the selected crystals into a diffraction dataset; and
extract crystallographic information from the diffraction dataset.

13. The system of claim 12 , further comprising a second deflector positioned between the sample and the detector for shifting and tilting the electrons transmitted through the sample back to the optical axis with the second deflector.

14. The system of claim 12 , wherein the sample is positioned on a transmission electron microscopy (TEM) grid, and the sample holder holds the sample by attaching to the TEM grid.

15. The system of claim 12 , further comprising a condenser positioned between the sample and the detector, and wherein the controller is further configured to:
adjust the condenser after acquiring the sample image;
acquire a second sample image with the adjusted condenser; and
calibrate beam location by comparing the second sample image with the sample image, and wherein direct the electron beam towards one of the selected crystals includes direct the electron beam towards one of the selected crystals based on the calibrated beam location.

16. The system of claim 12 , wherein the deflector is a bifocal beamformer, the bifocal beamformer splits the electron beam into a diffraction beam for acquiring the multiple diffraction patterns and an imaging beam for acquiring the sample image, wherein the imaging beam and the diffraction beam have different focal properties.

17. The system of claim 16 , wherein the bifocal beamformer shifts the diffraction beam at a specimen plane and tilts the diffraction beam to adjust the incident angle, and wherein direct the electron beam towards one of the selected crystals and acquire multiple diffraction patterns of the selected crystal at different incident angles includes, direct the diffraction beam towards one of the selected crystal within a field of view of the sample image by shifting the diffraction beam and acquire the multiple diffraction patterns of the selected crystal by tilting the diffraction beam.

18. The system of claim 16 , further comprising a third deflector positioned downstream of the bifocal beamformer, and wherein acquire multiple diffraction patterns of the selected crystal at different incident angles includes, acquire the multiple diffraction patterns by tilting the diffraction beam with the third deflector.

19. The system of claim 16 , further comprising an accelerator positioned upstream of the bifocal beamformer, and a multipole element positioned between the bifocal beamformer and the sample.

20. The system of claim 16 , further comprising an accelerator positioned between the bifocal beamformer and the sample, and a multipole element positioned between the bifocal beamformer and the sample.

21. The system of clai

Assignees

• Fei Co

Inventors

• Buijsse Bart
• Belapure Jaydeep Sanjay
• Henstra Alexander
• Janus Michael Patrick
• Vespucci Stefano

Classifications

• G01N23/2055 Primary

  Analysing diffraction patterns · CPC title

• G01N23/20025

  Sample holders or supports therefor · CPC title

• G01N23/20058 Primary

  Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method · CPC title

• H01J37/1472

  Deflecting along given lines · CPC title

• H01J37/222

  Image processing arrangements associated with the tube · CPC title