# US 2017/0256380 A1 · Automated tem sample preparation

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- Number: US 2017/0256380 A1
- Document ID: US20170256380A1
- Status: Published application
- Kind: A1
- Application number: 15/464,307
- Filed: 2017-03-20
- Published: 2017-09-07
- Earliest claimed: 2014-11-07
- Assignees: FEI Company
- Applicants: FEI Company
- Inventors: Valerie Brogden; Jeffrey Blackwood; Michael Schmidt; Dhruti Trivedi; Richard J. Young; Thomas G. Miller; Brian Roberts Routh, JR.; Stacey Stone; Todd Templeton
- Web page: https://patentgrep.com/patent/US20170256380A1

## CPC

- H01J 37/3023: {Program control}
- G01N 1/286: {involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising (microtomes G01N1/06; pulverising in general B02C; mixing in general B01F)}
- H01J 37/28: with scanning beams {(H01J37/268, H01J37/292, H01J37/2955 take precedence)}
- H01J 37/285: Emission microscopes, e.g. field-emission microscopes
- H01J 37/3045: {Object or beam position registration}
- H01J 37/31: for cutting or drilling
- G01N 2001/2873: {Cutting or cleaving}
- H01J 2237/208: Elements or methods for movement independent of sample stage for influencing or moving or contacting or transferring the sample or parts thereof, e.g. prober needles or transfer needles in FIB/SEM systems
- H01J 2237/31745: for preparing specimen to be viewed in microscopes or analyzed in microanalysers
- 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

Techniques are described that facilitate automated extraction of lamellae and attaching the lamellae to sample grids for viewing on transmission electron microscopes. Some embodiments of the invention involve the use of machine vision to determine the positions of the lamella, the probe, and/or the TEM grid to guide the attachment of the probe to the lamella and the attachment of the lamella to the TEM grid. Techniques that facilitate the use of machine vision include shaping a probe tip so that its position can be readily recognized by image recognition software. Image subtraction techniques can be used to determine the position of the lamellae attached to the probe for moving the lamella to the TEM grid for attachment. In some embodiments, reference structures are milled on the probe or on the lamella to facilitate image recognition.

## Claims

### Claim at position 1

1-25. (canceled)

### Claim 26

A method for automated sample preparation in a charged particle beam system, comprising:
loading a work piece into a vacuum chamber including one or more charged particle beam columns and a sample manipulation probe;
performing charged particle beam milling operations to form from a portion of a work piece a sample for observation on a transmission electron microscope;
forming one or more fiducials on the sample;
attaching the sample manipulation probe to the sample;
removing the sample from the work piece; and
using the one or more fiducials on the sample to determine a position and/or a rotational alignment of the sample.

### Claim 27 (depends on 26)

The method of claim 26 in which forming a fiducial on the sample includes directing a charged particle beam toward the sample to form the fiducial.

### Claim 28 (depends on 26)

The method of claim 26 in which the sample is a lamella having a thickness of less than 200 nm and in which forming a fiducial on the sample includes directing a charged particle beam toward the lamella to form the fiducial.

### Claim 29 (depends on 26)

The method of claim 26 in which using the one or more fiducials on the sample to determine the position and/or a rotational alignment of the sample includes automatically moving the sample to a TEM grid and attaching the sample to the TEM grid using beam-induced deposition.

### Claim at position 6

30-43. (canceled)

### Claim 44

A method for automated preparation in a charged particle beam system of a sample for viewing a region of interest in a transmission electron microscope, comprising:
loading a work piece into a vacuum chamber of the charged particle beam system having one or more charged particle beam columns and a sample manipulation probe;
identifying a region of interest in the work piece;
directing an ion beam toward the work piece to remove material from either side of the region of interest to leave a lamella having a thickness of less than 100 nm containing the region of interest;
directing the ion beam to form one or more fiducials on the lamella;
attaching the sample manipulation probe to the lamella;
freeing the lamella from the work piece;
moving the sample manipulation probe with the lamella to the vicinity of a TEM grid;
using image recognition software to recognize the one or more fiducials in the lamella;
using a position of the one or more fiducials in the lamella to determine a trajectory to move the lamella to an attachment point at the TEM grid; and
attaching the lamella to the TEM grid.

### Claim 45 (depends on 44)

The method of claim 44 in which directing the ion beam to form a fiducial on the lamella includes milling a shaped hole in the lamella.

### Claim 46 (depends on 44)

The method of claim 44 in which directing the ion beam to form a fiducial on the lamella includes milling a shape in a surface of the lamella.

### Claim at position 10

47-49. (canceled)

### Claim 50 (depends on 26)

The method of claim 26 further comprising using the position and/or rotational alignment determined using the fiducials in a subsequent processing or imaging step.

### Claim 51 (depends on 26)

The method of claim 26 further comprising automatically moving the sample to the sample holder using the position of the sample determined by the automated image recognition.

### Claim 52 (depends on 26)

The method of claim 26 further comprising positioning and/or rotationally aligning the sample using the position and/or rotational alignment determined using the fiducials.

### Claim 53 (depends on 44)

The method of claim 44 further comprising rotationally aligning the lamella with the TEM grid using the one or more fiducials.

### Claim 54 (depends on 26)

The method of claim 26 in which the one or more fiducials comprises multiple fiducials.

### Claim 55 (depends on 26)

The method of claim 26 in which the one or more fiducials comprises a single fiducial.

### Claim 56 (depends on 26)

The method of claim 26 in which positioning and/or rotationally aligning the sample for further processing comprises positioning and/or aligning the sample with a TEM grid further comprising attaching the sample to the TEM grid.

### Claim 57 (depends on 26)

The method of claim 26 in which:
using the one or more fiducials on the sample to determine the position and/or the rotational alignment of the sample includes using the one or more fiducials on the sample to determine the rotational alignment of the sample; and
positioning or rotationally aligning the sample using the one or more fiducials comprises rotationally aligning the sample using the one or more fiducials.

### Claim 58 (depends on 26)

The method of claim 26 in which using the one or more fiducials on the sample to determine the position or rotational alignment of the sample comprises using image recognition software to recognize the one or more fiducials.

### Claim 59 (depends on 26)

The method of claim 26 in which positioning or rotationally aligning the sample using the one or more fiducials comprises moving the sample to a sample holder using the one or more fiducials.

### Claim 60 (depends on 26)

The method of claim 26 in which forming one or more fiducials on the sample comprises etching the sample using charged particle beam etching to form the one or more fiducials.

### Claim 61 (depends on 26)

The method of claim 26 in which forming one or more fiducials on the sample comprises depositing material using charged particle beam-induced deposition to form the one or more fiducials.

### Claim 62 (depends on 26)

The method of claim 26 in which forming one or more fiducials on the sample comprises forming one or more fiducials adjacent to a region of interest.

### Claim 63 (depends on 26)

The method of claim 26 in which using the one or more fiducials on the sample to determine a position and/or a rotational alignment of the sample comprises using the one or more fiducials during thinning of the sample to determine how features evolve as the sample is thinned.

### Claim 64 (depends on 26)

The method of claim 26 in which forming one or more fiducials on the sample comprises forming one or more circular fiducials on the probe tip.

### Claim 65 (depends on 26)

The method of claim 26 in which forming one or more fiducials on the sample comprises forming one or more shapes on, or holes in, the sample.

### Claim 66 (depends on 26)

The method of claim 26 in which positioning or rotationally aligning the sample using the one or more fiducials comprises using the one or more fiducials on the sample to guide the sample to a TEM grid for attachment.

### Claim 67

A sample for examination under a transmission electron microscope, comprising:
a lamella having a thin section containing a region of interest, the thin section having a thickness of less than 200 nm; and
one or more fiducials formed on the lamella, the fiducials facilitating positioning and orienting the lamella.

### Claim 68 (depends on 67)

The sample of claim 67 in which the one or more fiducials comprises multiple fiducials.
