# US 10,319,560 B2 · Method of determining crystallographic properties of a sample and electron beam microscope for performing the method

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- Number: US 10,319,560 B2
- Document ID: US10319560B2
- Status: Granted
- Kind: B2
- Application number: 15/209,988
- Filed: 2016-07-14
- Published: 2017-01-26
- Granted: 2019-06-11
- Earliest claimed: 2015-07-23
- Assignees: Carl Zeiss Microscopy GmbH
- Applicants: Carl Zeiss Microscopy GmbH
- Inventors: Giuseppe Pavia
- Web page: https://patentgrep.com/patent/US10319560B2

## CPC

- H01J 37/244: Detectors; Associated components or circuits therefor
- G01N 23/2251: using incident electron beams, e.g. scanning electron microscopy [SEM]
- H01J 37/06: Electron sources; Electron guns
- G01N 2223/633: thickness, density, surface weight (unit area)
- H01J 2237/24585: Other variables, e.g. energy, mass, velocity, time, temperature
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- 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

A method of determining crystallographic properties of a sample includes: generating first and second electron beams of electrons having first and second mean kinetic energies, respectively; detecting, for each of first locations of a region of the sample, a two-dimensional spatial distribution of electrons incident onto a detection area while directing the first electron beam onto the first locations; generating, for each of the first locations, first data representing the two-dimensional spatial distribution; detecting, for each of second locations of the region of the sample, a two-dimensional spatial distribution of electrons incident onto the detection area while directing the second electron beam onto the second locations; generating, for each of the second locations, second data representing the two-dimensional spatial distribution; and determining the crystallographic properties for target locations of the region based on the first data of the first locations and the second data of the second locations.

## Claims

### Claim 1

A method of determining at least one crystallographic property of a sample, the method comprising:
generating a first electron beam of electrons having a first mean kinetic energy to be irradiated on the sample;
detecting, for each of first locations of a region of the sample, a two-dimensional spatial distribution of electrons transmitting through the sample and being incident onto a detection area while directing the first electron beam onto the first locations;
generating, for each of the first locations, first data representing the two-dimensional spatial distribution;
generating a second electron beam of electrons to be irradiated on the sample, the second electron beam having a second mean kinetic energy different from the first mean kinetic energy;
detecting, for each of second locations of the region of the sample, a two-dimensional spatial distribution of electrons transmitting through the sample and being incident onto the detection area while directing the second electron beam onto the second locations;
generating, for each of the second locations, second data representing the two-dimensional spatial distribution; and
generating an image of the sample,
wherein:
the image comprises: a) first pixels corresponding to first target locations of the sample; and b) second pixels corresponding to second target locations of the sample;
the second target locations are different from the first target locations;
values at the first pixels represent the at least one crystallographic property and are calculated based on the first data; and
values at the second pixels represent the at least one crystallographic property and are calculated based on the second data.

### Claim 2 (depends on 1)

The method according to claim 1, wherein determining the at least one crystallographic property for each current target location of a set of the target locations comprises:
selecting, as selected data, one of the first data of a first location associated with the current target location and the second data of a second location associated with the current target location; and
determining the at least one crystallographic property for the current target location based on the selected data.

### Claim 3 (depends on 2)

The method according to claim 2, wherein selecting comprises:
determining a quality parameter for each of the first data of the first location associated with the current target location and the second data of the second location associated with the current target location; and
selecting, as the selected data, the data having the quality parameter that provides a more accurate determination of crystallographic properties.

### Claim 4 (depends on 3)

The method according to claim 3, wherein the quality comprises a contrast value.

### Claim 5 (depends on 2)

The method according to claim 2, further comprising:
determining the first location associated with the current target location by selecting, among the first locations, the first location having a shortest distance to the current target location; and
determining the second location associated with the current target location by selecting, among the second locations, the second location having a shortest distance to the current target location.

### Claim 6 (depends on 1)

The method according to claim 1, wherein determining the at least one crystallographic property for each current target location of a set of the target locations comprises:
combining the first data of a first location associated with the current target location and the second data of a second location associated with the current target location to provide combined data; and
determining the at least one crystallographic property for the current target location based on the combined data.

### Claim 7 (depends on 6)

The method according to claim 6, wherein combining the first data and the second comprises:
interpolating the first data of the first location associated with the current target location and the second data of the second location associated with the current target location; and/or
averaging the first data of the first location associated with the current target location and the second data of the second location associated with the current target location.

### Claim 8 (depends on 1)

The method according to claim 1, wherein determining the at least one crystallographic property for each current target location of a set of the target locations comprises:
determining the at least one crystallographic property for a first location associated with the current target location based on the first data;
determining the at least one crystallographic property for a second location associated with the current target location based on the second data; and
selecting, as the at least one crystallographic property for the current target location, one of the at least one crystallographic property determined for the first and second locations associated with the current target location.

### Claim 9 (depends on 8)

The method according to claim 8, wherein selecting comprises:
determining a quality parameter for each of the at least one crystallographic property determined for the first and second locations associated with the current target location; and
selecting, as the at least one crystallographic property of the current target location, the at least one crystallographic property having the quality parameter that provides a more accurate determination of crystallographic properties.

### Claim 10 (depends on 9)

The method according to claim 9, wherein the quality parameter comprises a deviation from a predetermined expected value.

### Claim 11 (depends on 1)

The method according to claim 1, further comprising:
generating an image representation of the at least one crystallographic property of the target locations; and/or
determining the first and second locations based on sample information, in particular a thickness profile of the sample.

### Claim 12 (depends on 1)

The method according to claim 1, wherein
determining the at least one crystallographic property comprises identifying and indexing of Kikuchi bands.

### Claim 13 (depends on 1)

The method according to claim 1, wherein at least one of the following holds:
the detected electrons are electrons transmitted through the sample; and
detecting comprises generating detection signals representing a two-dimensional distribution of intensities of electrons incident onto the detection area.

### Claim 14 (depends on 1)

The method according to claim 1, further comprising:
recording a first image of the sample when using the first electron beam, recording a second image of the sample when using the second electron beam; and
aligning the first and second locations based on the first and second images.

### Claim 15 (depends on 1)

The method according to claim 1, wherein the first and second mean kinetic energies differ by at least one of:
1 keV, 2 keV, 5 keV and 10 keV; and
1%, 2%, 5% and 10% of a mean value of the first mean kinetic energy and the second mean kinetic energy.

### Claim 16 (depends on 1)

The method according claim 1, wherein each of the first and second mean kinetic energies is in a range of 10 keV to 30 keV.

### Claim 17 (depends on 1)

The method according to claim 1, according to claim 1 wherein generating the first and second electron beams comprises selecting the first and second mean kinetic energies based on:
sample information, in particular a thickness profile of the sample; or
two-dimensional spatial distributions of electrons emerging from the sample and being incident onto the detection area.

### Claim 18 (depends on 1)

The method according to claim 1, wherein directing the first electron beam onto the first locations and directing the second electron beam onto the second locations comprises: a) deflecting the first and second electron beams; or b) displacing the sample relative to the first and second electron beams.

### Claim 19 (depends on 1)

An electron beam microscope, comprising:
an electron beam column;
a two-dimensional spatially resolving electron detector; and
a controller, comprising:
a processing device; and
a machine-readable hardware storage device comprising instructions that are executable by the processing device to perform operations comprising the method according to claim 1.

### Claim 20

A method of determining at least one crystallographic property of a sample, comprising:
detecting, for each of first locations of a region of the sample, a two-dimensional spatial distribution of electrons transmitting through the sample and being incident onto a detection area while directing a first electron beam onto the first locations;
generating, for each of the first locations, first data representing the two-dimensional spatial distribution;
detecting, for each of second locations of the region of the sample, a two-dimensional spatial distribution of electrons transmitting through the sample and being incident onto the detection area while directing a second electron beam onto the second locations;
generating, for each of the second locations, second data representing the two-dimensional spatial distribution; and
generating an image of the sample,
wherein:
the image comprises: a) first pixels corresponding to first target locations of the sample; and b) second pixels corresponding to second target locations of the sample;
the second target locations are different from the first target locations;
values at the first pixels represent the at least one crystallographic property and are calculated based on the first data; and
values at the second pixels represent the at least one crystallographic property and are calculated based on the second data, and
wherein the first electron beam of electrons has a first mean kinetic energy when irradiated on the sample, and the second electron beam of electrons has a second mean kinetic energy when irradiated on the sample which is different from the first mean kinetic energy.

### Claim 21 (depends on 20)

An electron beam microscope, comprising:
an electron beam column;
a two-dimensional spatially resolving electron detector; and
a controller, comprising:
a processing device; and
a machine-readable hardware storage device comprising instructions that are executable by the processing device to perform operations comprising the method according to claim 20.

### Claim 22 (depends on 1)

The method according to claim 1, wherein the at least one crystallographic property are at least one of an orientation of a lattice structure, a lattice type and lattice parameters.
