# US 12,417,893 B2 · Diffractometer for charged-particle crystallography

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- Number: US 12,417,893 B2
- Document ID: US12417893B2
- Status: Granted
- Kind: B2
- Application number: 17/611,424
- Filed: 2020-05-19
- Published: 2022-07-28
- Granted: 2025-09-16
- Earliest claimed: 2019-05-20
- Assignees: Eldico Scientific AG
- Applicants: Eldico Scientific AG
- Inventors: Gunther Steinfeld; Gustavo Santiso-Quinones; Eric Hovestreydt
- Web page: https://patentgrep.com/patent/US12417893B2

## CPC

- H01J 37/20: Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
- H01J 37/28: with scanning beams {(H01J37/268, H01J37/292, H01J37/2955 take precedence)}
- G01N 23/2076: {for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS}
- H01J 2237/20207: Tilt
- H01J 2237/20221: Translation
- H01J 2237/20242: Eucentric movement
- H01J 2237/2025: Sensing velocity of translation or rotation
- H01J 2237/2802: Transmission microscopes
- 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

The present invention relates to a diffractometer for charged-particle crystallography of a crystalline sample, in particular for electron crystallography of a crystalline sample. The diffractometer comprises a charged-particle source for generating a charged-particle beam along a charged-particle beam axis, a charged-particle-optical system for manipulating the charged-particle beam such as to irradiate the sample with the charged-particle beam and a charged-particle detection system at least for collecting a diffraction pattern of the sample based on the beam of charged-particles transmitted through the sample. The diffractometer further comprises a sample holder for holding the sample and a manipulator operatively coupled to the sample holder for positioning the sample relative to the beam axis. The manipulator comprises a rotation stage for tilting the sample holder with respect to the incident charged-particle beam around a tilt axis, and a multi-axes translation stage for moving the sample holder at least in a plane perpendicular to the tilt axis. The multi-axes translation stage is operatively coupled between the sample holder and the rotation stage such that the multi-axes translation stage is in a rotational system of the rotation stage and the sample holder is in a moving system of the multi-axes translation stage.

## Claims

### Claim 1

A diffractometer for charged-particle crystallography of a crystalline sample, in particular for electron crystallography of a crystalline sample, the diffractometer comprising:
a charged-particle source for generating a charged-particle beam along a charged-particle beam axis,
a charged-particle-optical system for manipulating the charged-particle beam such as to irradiate the sample with the charged-particle beam;
a sample holder for holding the sample,
a manipulator operatively coupled to the sample holder for positioning the sample relative to the beam axis, wherein the manipulator comprises a rotation stage for tilting the sample holder with respect to the incident charged-particle beam around a tilt axis, and a multi-axes translation stage for moving the sample holder at least in a plane perpendicular to the tilt axis, wherein the multi-axes translation stage is operatively coupled between the sample holder and the rotation stage such that the multi-axes translation stage is in a rotational system of the rotation stage and the sample holder is in a moving system of the multi-axes translation stage, thereby enabling to position the center of mass of the sample substantially on-axis with regard to the tilt axis with a maximum lateral deviation from the tilt axis of at most 1 μm,
a charged-particle detection system at least for collecting a diffraction pattern of the sample based on the beam of charged-particles transmitted through the sample,
wherein the tilt axis is fixed in space and extends in a substantially vertical direction,
wherein the diffractometer further comprises a measurement device including an interferometric measurement device for measuring a position of the sample holder relative to the charged-particle beam, wherein the interferometric measurement device includes a mirror attached to the tilt axis, and
wherein the diffractometer further comprises a feedback controller which is operatively coupled to the measurement device and the manipulator and configured to control the position of the sample relative to the charged-particle beam such that for each tilt angle position of the rotation stage the center of mass of the sample stays substantially on-axis with regard to the tilt axis with a maximum lateral deviation from a predefined reference of the tilt axis of at most 1 μm, and thus that for each tilt angle position of the rotation stage the volume of the sample substantially stays within the charged-particle beam.

### Claim 2 (depends on 1)

The diffractometer according to claim 1, wherein the beam axis is fixed in space, in particular extends in a substantially horizontal direction, or wherein the orientation of the beam axis is adjustable relative to the tilt axis.

### Claim 3 (depends on 1)

The diffractometer according to claim 1, wherein the manipulator further comprises a single-axis translation stage for moving the sample holder along an axis substantially parallel to the tilt axis.

### Claim 4 (depends on 3)

The diffractometer according to claim 3, wherein the single-axis translation stage is operatively coupled between the multi-axes translation stage and the rotation stage such that the single-axis translation stage is in the rotational system of the rotation stage and the multi-axes translation stage is in a moving system of the single-axis translation stage.

### Claim 5 (depends on 3)

The diffractometer according to claim 3, wherein the rotation stage is operatively coupled between the multi-axes translation stage and the single-axis translation stage such that the rotation stage is in a moving system of the single-axis translation stage and the multi-axes translation stage is in the rotational system of the rotation stage.

### Claim 6 (depends on 1)

The diffractometer according to claim 1, wherein the multi-axes translation stage is arranged within a sample chamber of the diffractometer.

### Claim 7 (depends on 6)

The diffractometer according to claim 6, wherein the rotation stage is arranged outside or inside the sample chamber of the diffractometer.

### Claim 8 (depends on 6)

The diffractometer according to claim 6, wherein the manipulator further comprises a single-axis translation stage for moving the sample holder along an axis substantially parallel to the tilt axis, wherein the single-axis translation stage is arranged outside or inside the sample chamber of the diffractometer.

### Claim 9 (depends on 1)

The diffractometer according to claim 1, wherein the diffractometer is a cryogenic diffractometer comprising a cryogenic cooling source which is in thermal contact with the sample holder via the manipulator.

### Claim 10 (depends on 1)

The diffractometer according to claim 1, wherein the rotation stage is configured to tilt the sample holder over an angular range between +70° and −70° with regard to a reference plane which contains the beam axis and is parallel to the tilt axis.

### Claim 11 (depends on 1)

The diffractometer according to claim 1, wherein the rotation stage is configured to tilt the sample holder with a constant angular velocity in a range of 0.1°/s to 100°/s.

### Claim 12 (depends on 1)

The diffractometer according to claim 1, wherein a distance between an intersection of the sample holder and the beam axis and a rotational center of the rotation stage is in a range of 10 cm to 30 cm.

### Claim 13 (depends on 1)

The diffractometer according to claim 1, wherein the charged-particle-optical system is configured to manipulate the charged-particle beam such the charged-particle beam irradiated to the sample is a parallel beam of charged-particles having a beam diameter of at most 1.5 μm.

### Claim 14 (depends on 1)

The diffractometer according to claim 1, wherein the feedback controller is configured to control the position of the sample relative to the charged-particle beam such that for each tilt angle position of the rotation stage the center of mass of the sample stays substantially on-axis with regard to the tilt axis with a maximum lateral deviation from the tilt axis of at most 0.5 μm.

### Claim 15 (depends on 1)

The diffractometer according to claim 1, wherein the feedback controller is configured to control the position of the sample relative to the charged-particle beam such that for each tilt angle position of the rotation stage the center of mass of the sample stays substantially on-axis with regard to the tilt axis with a maximum lateral deviation from the tilt axis of at most 0.3 μm.

### Claim 16 (depends on 1)

The diffractometer according to claim 1, wherein the feedback controller is configured to control the position of the sample relative to the charged-particle beam such that for each tilt angle position of the rotation stage the center of mass of the sample stays substantially on-axis with regard to the tilt axis with a maximum lateral deviation from the tilt axis of at most 0.1 μm.

### Claim 17 (depends on 1)

The diffractometer according to claim 1, wherein the rotation stage is configured to tilt the sample holder over an angular range between +250° and −70° or between −250° and +70° with regard to a reference plane which contains the beam axis and is parallel to the tilt axis.

### Claim 18 (depends on 1)

The diffractometer according to claim 1, wherein the rotation stage is configured to tilt the sample holder over an angular range between +250° and −70° or between −360° and +360° with regard to a reference plane which contains the beam axis and is parallel to the tilt axis.

### Claim 19 (depends on 1)

The diffractometer according to claim 1, wherein the rotation stage is configured to tilt the sample holder with a constant angular velocity in a range of 1°/s to 30°/s.

### Claim 20 (depends on 1)

The diffractometer according to claim 1, wherein a distance between an intersection of the sample holder and the beam axis and a rotational center of the rotation stage is in a range of 15 cm to 20 cm, or in a range of 2 cm to 10 cm.

### Claim 21 (depends on 1)

The diffractometer according to claim 1, wherein the charged-particle-optical system is configured to manipulate the charged-particle beam such the charged-particle beam irradiated to the sample is a parallel beam of charged-particles having a beam diameter of at most 1 μm.

### Claim 22 (depends on 1)

The diffractometer according to claim 1, wherein the charged-particle-optical system is configured to manipulate the charged-particle beam such the charged-particle beam irradiated to the sample is a parallel beam of charged-particles having a beam diameter in a range between 0.5 μm and 0.3 μm.