Method of modifying a sample surface layer from a microscopic sample

Patent metadata

Field	Value
Publication number	US-2016199878-A1
Application number	US-201614992743-A
Country	US
Kind code	A1
Filing date	Jan 11, 2016
Priority date	Jan 12, 2015
Publication date	Jul 14, 2016
Grant date	—

Abstract

A method of modifying a sample surface layer in the vacuum chamber of a particle-optical apparatus, the method performed in vacuum, the method comprising:
Providing the microscopic sample attached to a manipulator, Providing a first liquid at a first (controlled) temperature, Dipping the sample in the first liquid, thereby causing a sample surface modification, Removing the sample from the first liquid, Providing a second liquid at a second (controlled) temperature, Dipping the sample in the second liquid, and Removing the sample from the second liquid.

This enables the wet processing of a sample in-situ, thereby enhancing speed and/or avoiding subsequent alteration/contamination of the sample, such as oxidation, etc. The method is particularly useful for etching a lamella after machining the lamella with a (gallium) FIB to remove the surface layer where gallium implantation occurred, or where the crystal lattice is disturbed.

First claim

1 . Method of modifying a sample surface layer from a sample in a particle-optical apparatus, the method performed in vacuum, the method comprising the steps of:
providing the sample attached to a manipulator, providing a first liquid at a first temperature, dipping the sample in the first liquid, thereby causing a sample surface modification, removing the sample from the first liquid, providing a second liquid at a second temperature, dipping the sample in the second liquid, and removing the sample from the second liquid.

2 . The method of claim 1 in which the sample surface modification is a modification of the sample surface roughness, the hydrophilicity, surface charge, surface energy, biological compatibility, or reactivity, the addition of functional groups, the addition of biological material, plating the sample surface or the removal of a sample surface layer.

3 . The method of claim 1 in which the sample is attached to the manipulator by forming a weld using beam induced deposition, the beam induced deposition induced by a laser beam, an electron beam or an ion beam.

4 . The method of claim 1 in which the sample has a dimension of less than 10 μm in any direction and the first liquid and the second liquid are deposited as droplets with a volume of less than 1 picoliter, more specifically less than 1 femtoliter.

5 . The method of claim 1 in which the sample is a semiconductor sample.

6 . The method of claim 1 in which the step of providing the sample attached to a manipulator comprises the steps of:
providing a work piece,
attaching the sample to the manipulator, and
excising the sample from the work piece using a focused ion beam.

7 . The method of claim 1 in which the sample surface modification is caused by etching, electro-chemical etching, electroless plating or electroplating, said electroplating using a non-virtual cathode.

8 . The method of claim 7 in which the thickness of the removed or added sample surface layer is less than 10 nm.

9 . The method of claim 1 in which the second liquid is a rinsing liquid, and dipping the sample in the second fluid rinses the sample.

10 . The method of claim 9 in which the sample is rinsed repeatedly.

11 . The method of claim 10 in which each step of rinsing is performed in fresh rinsing liquid.

12 . The method of claim 1 in which the first liquid contains biological material, the sample surface modification comprises providing biological material to the surface of the sample and the second liquid causes bonding of the biological material to the surface of the sample.

13 . The method of claim 1 , the surface modification comprising functionalizing the sample by forming active sites caused by the deposition of enzymes, nanowires or other nanostructures, and the second liquid comprises providing a material to said active sites.

14 . The method of claim 1 in which the two liquids are provided on one surface, the manipulator movable with respect to said surface.

15 . The method of claim 1 in which the sample surface is during and/or after the modification of the sample surface layer inspected using a beam of charged particles.

16 . The method of claim 1 in which the liquids are applied using a first liquid insertion system and a second liquid insertion system.

17 . The method of claim 16 in which the first liquid injection system and the second liquid injection system are integrated in one structural liquid injection system.

18 . An apparatus for modifying a sample surface layer from a sample in a vacuum, comprising:
a vacuum chamber; a manipulator; a source of a first liquid at a first temperature; a source of a second liquid at a second temperature; a controller, the controller programmed to:
apply the first liquid to the sample within the vacuum chamber, thereby causing a sample surface modification; and
apply the second liquid to the sample within the vacuum chamber.

19 . The apparatus of claim 18 , wherein the controller programmed to apply the first liquid to the sample within the vacuum chamber comprises a controller programmed to dip the sample in a first liquid that causes a modification of the sample surface roughness, the hydrophilicity, surface charge, surface energy, biological compatibility, or reactivity, the addition of functional groups, the addition of biological material, plating the sample surface or the removal of a sample surface layer.

20 . The apparatus of claim 18 , wherein the controller programmed to apply the first liquid to the sample within the vacuum chamber comprises a controller programmed to dip the sample in a functionalizing liquid, and wherein the controller programmed to dip the sample in the second liquid comprises a controller programmed to dip the sample in a material liquid, and wherein the functionalizing liquid creates active sites on the sample surface, and material liquid which provides material to the active sites on the sample surface.

Assignees

• Fei Co

Inventors

• Vystavel Tomas
• Botman Aurelien Philippe Jean Maclou

Classifications

• H10P70/00

  Cleaning of wafers, substrates or parts of devices · CPC title

• H10P50/642

  Chemical etching · CPC title

• H10P14/412

  Deposition of metallic or metal-silicide materials · CPC title

• B05D5/02 Primary

  to obtain a matt or rough surface · CPC title

• H01L21/32051

  Electricity · mapped topic