Method for preparing thin samples for TEM imaging

Patent metadata

Field	Value
Publication number	US-9279752-B2
Application number	US-201414514199-A
Country	US
Kind code	B2
Filing date	Oct 14, 2014
Priority date	Jun 3, 2011
Publication date	Mar 8, 2016
Grant date	Mar 8, 2016

Abstract

A method and apparatus for preparing thin TEM samples in a manner that reduces or prevents bending and curtaining is realized. Embodiments of the present invention deposit material onto the face of a TEM sample during the process of preparing the sample. In some embodiments, the material can be deposited on a sample face that has already been thinned before the opposite face is thinned, which can serve to reinforce the structural integrity of the sample and refill areas that have been over-thinned due to a curtaining phenomena. In other embodiments, material can also be deposited onto the face being milled, which can serve to reduce or eliminate curtaining on the sample face.

First claim

We claim as follows:

1. A method of preparing a sample for TEM analysis, the method comprising:
at least partially separating a sample section containing a feature of interest from a bulk substrate;
thinning a first side of the sample to expose a first sample face;
depositing a layer of a material onto the exposed first sample face using a beam-activated precursor deposition from a precursor gas;
thinning a second side of the sample;
removing at least a portion of the deposited material; and
in which removing at least a portion of the deposited material comprises removing at least a portion of the deposited material by a method other than ion beam milling.

2. The method of claim 1 further comprising depositing a layer of a material onto the exposed second sample face.

3. The method of claim 1 further comprising repeating the steps of thinning a first side of the sample and depositing a layer of a material onto the exposed first sample face until a desired final sample face is exposed.

4. The method of claim 1 in which the sample is prepared using a particle beam system.

5. The method of claim 1 in which the sample is prepared using a focused ion beam system.

6. The method of claim 1 in which removing at least a portion of the deposited material comprises removing at least a portion of the deposited material by gas-assisted etching.

7. The method of claim 6 in which removing at least a portion of the deposited material comprises removing at least a portion of the deposited material after the sample is removed from the vacuum chamber.

8. A method of preparing a sample for TEM analysis, the method comprising:
loading a sample into the vacuum chamber of a particle beam system;
at least partially separating a sample section containing a feature of interest from a bulk substrate by particle beam milling;
thinning a first side of the sample using the particle beam to expose a first sample face;
depositing a layer of a material onto the exposed first sample face using beam induced deposition;
thinning a second side of the sample using the particle beam to expose a second sample face:
depositing a layer of a material onto the exposed second sample face using beam induced deposition; and
in which the steps of thinning a side of the sample to expose a sample face and depositing a layer of a material onto that exposed sample face are performed simultaneously.

9. The method of claim 8 further comprising removing at least a portion of the deposited material.

10. A charged particle beam apparatus, comprising:
a charged particle source;
a focusing column with charged particle lenses for focusing and directing a charged particle beam;
a vacuum chamber for containing a sample;
a gas source for providing a gas at the sample; and
a system controller, the controller programmed for carrying out the method of claim 8 .

11. A non-transitory computer-readable storage medium configured with a computer program, where the storage medium so configured causes a computer to control a charged particle beam system to carry out the steps of the method of claim 8 .

12. The method of claim 8 in which the final TEM sample is 30 nm or less in thickness.

13. The method of claim 8 in which the deposited material will not significantly interfere with imaging the TEM sample.

14. The method of claim 1 in which removing at least a portion of the deposited material includes removing substantially all of the deposited material.

15. The method of claim 8 further comprising removing at least some material from both sides of the sample.

Assignees

• Fei Co

Inventors

• Moriarty Michael
• Stone Stacey
• Blackwood Jeffrey

Classifications

• H10P14/6516

  of treatments performed after formation of the materials · CPC title

• G01N2001/2886

  Laser cutting, e.g. tissue catapult · CPC title

• H01J37/3056

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

• G01N1/32 Primary

  Polishing; Etching · CPC title

• G01N1/286 Primary

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