Automated TEM sample preparation

Patent metadata

Field	Value
Publication number	US-9601313-B2
Application number	US-201514934837-A
Country	US
Kind code	B2
Filing date	Nov 6, 2015
Priority date	Nov 7, 2014
Publication date	Mar 21, 2017
Grant date	Mar 21, 2017

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.

First claim

We claim as follows:

1. A method for automated sample preparation in a charged particle beam system, comprising:
loading a work piece into a vacuum chamber having one or more charged particle beam systems and a sample manipulation probe;
removing material surrounding a thin section of the work piece using a focused ion beam leaving the thin section attached to the bulk work piece by small attachment structures;
shaping the tip of a sample manipulator probe into a machine-recognizable shape by removing material from the tip using the focused ion beam;
using the machine-recognizable shape of the tip to determine the position of the tip relative to the thin section;
using the position of the tip relative to the thin section, automatically moving the sample probe sufficiently close to the thin section to attach the manipulator probe using charged particle beam-induced deposition;
attaching the sample probe to the thin section;
severing said small attachment structures so that the thin section is supported only by the sample probe;
moving the sample probe automatically so that the thin section is sufficiently close to a sample grid for holding thin samples to attach the thin section to the sample grid using charged particle beam-induced deposition;
attaching the thin section to the sample grid; and
removing the tip of the sample probe from the thin section.

2. The method of claim 1 wherein the thin section is a cross section view section.

3. The method of claim 1 further comprising using image analysis to direct the movement of the sample probe.

4. The method of claim 1 further comprising shaping the tip into a chisel shape.

5. The method of claim 1 further comprising locating the probe using image analysis to determine a trajectory to move the probe to the thin section or to the sample grid.

6. The method of claim 5 wherein the image analysis uses image subtraction.

7. The method of claim 1 further comprising calculating an XY vector between said probe and said thin section based on images from one charged particle beam and a Z vector between said probe and said thin section based on images from a second particle beam.

8. The method of claim 1 further comprising reshaping the tip after the thin section has been disconnected from the probe.

9. The method of claim 1 further comprising attaching the probe to the face of the thin section away from a region of interest.

10. The method of claim 1 further comprising thinning the thin section further after it has been attached to the sample grid.

11. An apparatus for automated sample production in a charged particle system comprising:
a vacuum chamber for containing a work piece;
at least two charged particle beam columns for producing charged particle beams for imaging and operating on the work piece within the vacuum chamber;
a moveable sample stage for holding and moving the work piece within the vacuum chamber;
a charged particle detector for forming images from charged particles emitted from the sample upon impact of the charged particle beams;
a sample manipulation probe capable of submicron positioning;
a gas injection system for providing a precursor gas for charged particle beam-induced deposition;
a controller for controlling the operation of the apparatus; and
a computer readable memory for storing computer instruction for execution by the controller for carrying out the method of claim 1 .

12. The apparatus of claim 11 further comprising an apparatus where there are two charged particle beam systems.

13. The apparatus of claim 11 in which the at least two charged particle beam columns for producing charged particle beams for imaging and operating on the work piece include an electron beam column and an ion beam column.

14. The apparatus of claim 11 wherein the computer memory includes computer instructions for the analysis of images formed by the charged particle beams, the image analysis programmed to locate said sample manipulation probe, with or without an attached thin section.

15. The apparatus of claim 14 wherein the image analysis is performed using image subtraction.

16. The apparatus of claim 14 wherein the computer memory includes computer instructions to cause the focused ion beam to form the tip of the sample probe into a chisel shape.

17. The apparatus of claim 11 wherein the at least one of the charged particle beams is a focused ion beam.

18. 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 systems and a sample manipulation probe;
automatically physically re-shaping the manipulation probe to a new shape;
automatically performing charged particle milling operations to form a sample from a portion of a work piece; and
using the re-shaped probe to remove a sample from the work-piece.

19. The method of claim 18 in which using the re-shaped probe to remove the sample from the work piece includes using image recognition software to automatically determine the position of the re-shaped probe.

20. The method of claim 18 in which re-shaping the probe comprises forming a probe tip into rectangular prism.

Assignees

• Fei Co

Inventors

• Brogden Valerie
• Blackwood Jeffrey
• Schmidt Michael
• Trivedi Dhruti
• Young Richard J
• Miller Thomas G
• Routh Jr Brian Roberts
• Stone Stacey
• Templeton Todd

Classifications

• H01J2237/31745

  for preparing specimen to be viewed in microscopes or analyzed in microanalysers · CPC title

• G01N2001/2873

  Cutting or cleaving · CPC title

• H01J37/3045 Primary

  Object or beam position registration · CPC title

• H01J2237/208

  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 · CPC title

• G01N1/286

  involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising (microtomes G01N1/06; pulverising in general B02C; mixing in general B01F) · CPC title