Method and system to determine crystal structure

Patent metadata

Field	Value
Publication number	US-11988618-B2
Application number	US-202117219627-A
Country	US
Kind code	B2
Filing date	Mar 31, 2021
Priority date	Mar 31, 2021
Publication date	May 21, 2024
Grant date	May 21, 2024

Abstract

Molecular structure of a crystal may be solved based on at least two diffraction tilt series acquired from a sample. The two diffraction tilt series include multiple diffraction patterns of at least one crystal of the sample acquired at different electron doses. In some examples, the two diffraction tilt series are acquired at different magnifications.

First claim

What is claimed is:

1. A method, comprising:
acquiring a first diffraction tilt series of a sample, wherein each diffraction pattern in the first diffraction tilt series has a first electron dose and a first magnification;
acquiring a second diffraction tilt series of the sample, wherein each diffraction pattern in the second diffraction tilt series has a second electron dose and a second magnification; and
solving a molecular structure of a crystal based on the first diffraction tilt series and the second diffraction tilt series.

2. The method of claim 1 , wherein the first electron dose is higher than the second electron dose, and the first magnification is lower than the second magnification.

3. The method of claim 2 , wherein a beam stopper is used while acquiring the first diffraction tilt series and the second diffraction tilt series, and the method further comprising adjusting the first magnification to the second magnification based on a size of the beam stopper.

4. The method of claim 2 , further comprising adjusting the first magnification to the second magnification based on unit cell size.

5. The method of claim 1 , wherein solving a molecular structure of a crystal based on the first diffraction tilt series and the second diffraction tilt series includes: obtaining a high-resolution dataset based on the first diffraction tilt series; obtaining a lower-resolution dataset based on the second diffraction tilt series; obtaining a merged dataset by combining the higher-resolution dataset with the lower-resolution dataset in a reciprocal space; and solving the molecular structure based on the merged dataset.

6. The method of claim 1 , wherein acquiring the first diffraction tilt series includes acquiring multiple diffraction patterns of a first crystal of the sample at the first electron dose by adjusting an angle between the first crystal and an electron beam, wherein acquiring the second diffraction tilt series includes acquiring multiple diffraction patterns of the first crystal at the second electron dose by adjusting the angle between the first crystal and the electron beam.

7. The method of claim 6 , wherein the second diffraction tilt series is acquired after acquiring the first diffraction tilt series.

8. The method of claim 6 , wherein the angle between the first crystal and the electron beam are adjusted by tilting the electron beam and/or rotating a sample stage for holding the sample.

9. The method of claim 6 , wherein acquiring the first diffraction tilt series further includes acquiring multiple diffraction patterns of a second crystal of the sample at the first electron dose by adjusting an angle between the second crystal and the electron beam, and acquiring the second diffraction tilt series further includes acquiring multiple diffraction patterns of the second crystal at the second electron dose by adjusting the angle between the second crystal and the electron beam.

10. The method of claim 1 , wherein the sample includes multiple crystals, and wherein acquiring the first diffraction tilt series includes directing an electron beam towards one or more of the multiple crystals and acquire one or more diffraction patterns for each of the multiple crystals, and acquiring the second diffraction tilt series include directing the electron beam towards one or more of the multiple crystals and acquire one or more diffraction patterns for each of the multiple crystals.

11. The method of claim 1 , wherein a data acquisition time for the first diffraction tilt series is the same as a data acquisition time for the second diffraction tilt series.

12. A method, comprising:
acquiring one or more first diffraction patterns of a crystal at a first electron dose;
acquiring one or more second diffraction patterns of the crystal at a second electron dose;
obtaining a high-resolution dataset based on the first diffraction patterns;
obtaining a low-resolution dataset based on the second diffraction patterns;
generating a merged dataset by combining the high-resolution dataset and the low-resolution dataset in a reciprocal space;
and
solving a molecular structure of the crystal based on the merged dataset.

13. The method of claim 12 , wherein the second diffraction patterns are acquired after the first diffraction patterns, and the first electron dose is higher than the second electron dose.

14. The method of claim 12 , wherein the first diffraction patterns are acquired at a magnification lower than a magnification of the second diffraction patterns.

15. A system, comprising:
an electron source for generating an electron beam along an optical axis;
a sample stage for holding a sample and adjusting a sample position;
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 first diffraction tilt series of the sample, wherein each diffraction pattern in the first diffraction tilt series has a first electron dose and a first magnification;
acquire a second diffraction tilt series of the sample, wherein each diffraction pattern in the second diffraction tilt series has a second electron dose and a second magnification; and
solve a molecular structure of a crystal of the sample based on the first diffraction tilt series and the second diffraction tilt series.

16. The system of claim 15 , wherein the first electron dose is higher than the second electron dose, and the first magnification is lower than the second magnification.

17. The system of claim 15 , wherein the first diffraction tilt series and the second diffraction tilt series are acquired by rotating the sample stage relative to the electron beam at a same rotation speed.

18. The system of claim 15 , wherein solve a molecular structure of a crystal based on the first diffraction tilt series and the second diffraction tilt series includes: obtain a high-resolution dataset based on the first diffraction tilt series; obtain a lower-resolution dataset based on the second diffraction tilt series; obtain a merged dataset by combining the higher-resolution dataset with the lower-resolution dataset in a reciprocal space; and solve the molecular structure based on the merged dataset.

19. The system of claim 15 , further including a beam stopper for acquiring the first diffraction tilt series and the second diffraction tilt series, and wherein a magnification is adjusted based on a size of the beam stopper.

20. The system of claim 15 , wherein a magnification is adjusted based on a unit cell size of the crystal.

Assignees

• Fei Co

Inventors

• Buijsse Bart
• Raaijmakers Hans
• Tiemeijer Peter Christiaan

Classifications

• G01N23/2055 Primary

  Analysing diffraction patterns · CPC title

• G01N23/20025

  Sample holders or supports therefor · CPC title

• G01N23/207

  Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions · CPC title

• G01N2223/0565

  diffraction of electrons, e.g. LEED · CPC title

• G01N2223/102

  beta or electrons · CPC title