Method for creating S/TEM sample and sample structure

Patent metadata

Field	Value
Publication number	US-9006651-B2
Application number	US-201314029368-A
Country	US
Kind code	B2
Filing date	Sep 17, 2013
Priority date	Oct 20, 2006
Publication date	Apr 14, 2015
Grant date	Apr 14, 2015

Abstract

An improved method and apparatus for S/TEM sample preparation and analysis. Preferred embodiments of the present invention provide improved methods for TEM sample creation, especially for small geometry (<100 nm thick) TEM lamellae. A novel sample structure and a novel use of a milling pattern allow the creation of S/TEM samples as thin as 50 nm without significant bowing or warping. Preferred embodiments of the present invention provide methods to partially or fully automate TEM sample creation, to make the process of creating and analyzing TEM samples less labor intensive, and to increase throughput and reproducibility of TEM analysis.

First claim

We claim as follows:

1. A method of extracting one or more samples for TEM analysis from a substrate, the method comprising:
loading the substrate with the sample to be extracted into an ion beam system;
locating a first sample site on the substrate surface;
imaging the sample site;
identifying desired fiducial locations for determining the edge positions for said first sample site;
milling a fiducial at each of the desired fiducial locations wherein the milling includes a combination of at least one high precision rectangular fiducial mark around which is milled one low precision circular fiducial mark;
determining the edge positions for the desired sample with respect to said fiducial marks;
automated milling of the substrate surface on either side of the desired sample site leaving a thin layer of material; and
extracting the sample.

2. The method of claim 1 where the substrate comprises a semiconductor wafer.

3. The method of claim 1 wherein the automated milling the substrate surface on either side of the desired sample location leaving a thin layer of material comprises automatically milling the substrate surface on either side of the desired sample location leaving a thin layer of material less than 100 nm thick.

4. The method of claim 1 wherein locating the sample site on the substrate surface comprises locating the sample site on the substrate surface using image recognition software.

5. The method of claim 1 further comprising:
locating a second sample site on the substrate surface;
using pattern recognition to identify second fiducial locations having fiducial marks for said second sample site so that the spatial relationships between the second fiducial locations and the second sample site will be identical to the spatial relationships between said desired fiducial locations and said first sample site.

6. The method of claim 1 in which identifying desired fiducial locations for said first sample site comprises locating said first fiducial location from CAD data and locating the desired fiducial locations on the substrate by using pattern recognition based upon geometric information from the CAD data.

7. The method of claim 1 in which milling a combination of at least one high precision fiducial mark and one low precision fiducial mark comprises milling at least one larger fiducial mark which is recognizable in an image of the sample produced by an ion beam scan at a lower resolution suitable for bulk milling and at least one smaller fiducial mark which is recognizable in an image of the sample produced by an ion beam scan at a higher resolution.

8. The method of claim 1 in which automatically milling the substrate surface on either side of the desired sample location leaving a thin layer of material comprises:
imaging the desired sample location and the at least one low precision fiducial using an ion beam having a first large beam diameter suitable for bulk milling;
positioning the ion beam using the location of the at least one low precision fiducial;
scanning the beam in a rectangular area on a first side of the desired sample location to form a first rectangular hole having a predetermined depth; and
scanning the beam in a rectangular area on a second side, said second side on the opposite side of the desired sample location from the first side, to form a second rectangular hole having a predetermined depth leaving a vertical layer of material between said first and second rectangular holes, said layer including the sample section to be extracted.

9. The method of claim 8 further comprising:
imaging the desired sample location and the at least one high precision fiducial using an ion beam having a second smaller beam diameter suitable for precision milling, said high precision fiducial having at least one axis substantially parallel to the desired final edge of the sample to be extracted;
determining the edge positions for the desired sample with respect to said axis; and
thinning the sample section from both the first and second sides leaving a thinned sample less than 500 nm thick.

10. The method of claim 9 in which thinning the sample section from both the first and second sides comprises:
using image recognition to locate the edges of the vertical layer of material;
thinning the first side of the sample by milling away material within an area beginning at half the desired sample thickness away from the center of the vertical layer of material and extending toward the first side of the sample;
thinning the second side of the sample by milling away material within an area beginning at half the desired sample thickness away from the center of the vertical layer of material and extending toward the second side of the sample.

11. The method of claim 10 in which thinning a side of the sample comprises:
directing a substantially normal ion beam at one side of the sample section in a milling pattern that thins the sample section in a series of passes, each pass comprising moving the beam in a raster pattern from the outside of the sample section inward to the desired sample face and then returning to the outside of the sample section, the series of passes continuing until the sample section has been thinned to a desired depth.

12. The method of claim 10 wherein moving the beam in a raster pattern from the outside of the sample section inward to the desired sample face and then returning to the outside of the sample section comprises moving the beam in a raster pattern having an x-direction parallel to the desired sample face and a y-direction perpendicular to the desired sample face, said raster pattern comprising scanning the beam back and forth in the x-direction and then stepping the beam forward toward the desired sample face, said steps continuing until the desired sample face is reached.

13. The method of claim 10 wherein the beam dwell time increases as the beam approaches the desired sample face.

14. The method of claim 10 in which thinning the sample section comprises thinning a central portion of the sample, leaving thicker material at the bottom and sides of the thinned portion.

Assignees

• Fei Co

Inventors

• Blackwood Jeffrey
• Stone Stacey

Classifications

• G01N1/32

  Polishing; Etching · CPC title

• G01N23/04 Primary

  and forming images of the material · CPC title

• H01J2237/31745

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

• G01N1/28

  Preparing specimens for investigation {including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q}(mounting specimens on microscopic slides G02B21/34; means for supporting the objects or the materials to be analysed in electron microscopes H01J37/20 {; laboratory gas handling apparatus B01L5/00}) · CPC title

• H01J37/3056

  for microworking, e. g. etching of gratings or trimming of electrical components · CPC title