Bulk nanofabrication with single atomic plane precision via atomic-level sculpting of crystalline oxides

Patent metadata

Field	Value
Publication number	US-10400351-B2
Application number	US-201715697541-A
Country	US
Kind code	B2
Filing date	Sep 7, 2017
Priority date	Sep 7, 2016
Publication date	Sep 3, 2019
Grant date	Sep 3, 2019

Abstract

A method for sculpting crystalline oxide structures for bulk nanofabrication is provided. The method includes the controlled electron beam induced irradiation of amorphous and liquid phase precursor solutions using a scanning transmission electron microscope. The atomically focused electron beam includes operating parameters (e.g., location, dwell time, raster speed) that are selected to provide a higher electron dose in patterned areas and a lower electron dose in non-patterned areas. Concurrently with the epitaxial growth of crystalline features, the present method includes scanning the substrate to provide information on the size of the crystalline features with atomic resolution. This approach provides for atomic level sculpting of crystalline oxide materials from a metastable amorphous precursor and the liquid phase patterning of nanocrystals.

First claim

The invention claimed is:

1. A method of fabricating a crystalline oxide nanostructure comprising:
providing a scanning transmission electron microscope for generating a scanning electron beam;
positioning a sample including an amorphous oxide precursor material on a crystalline substrate within a sample area of the scanning transmission electron microscope; and
activating the scanning transmission electron microscope such that the scanning electron beam impinges the sample in a region of the precursor material and physically and chemically transforms the precursor material into an epitaxially grown crystalline oxide nanostructure.

2. The method according to claim 1 further including varying an intensity of the scanning electron beam such that the sample includes a patterned area and a non-patterned area, the patterned area receiving a higher electron dose than the non-patterned area.

3. The method according to claim 1 wherein activating the scanning transmission electron microscope includes repeated scans of the scanning electron beam to achieve progressive epitaxial growth of the crystalline oxide nanostructure with each scan of the scanning electron beam.

4. The method according to claim 3 further including slowing a scan rate of the scanning electron beam between scans of the scanning electron beam.

5. The method according to claim 1 further including scanning the sample with electron energy loss spectroscopy concurrently with the activation of the scanning transmission electron microscope.

6. The method according to claim 1 wherein the amorphous oxide precursor material and the crystalline substrate are identical oxides.

7. The method according to claim 1 wherein the amorphous oxide precursor material is an alkaline earth metal oxide.

8. The method according to claim 1 wherein the amorphous oxide precursor material is strontium titanate.

9. The method according to claim 1 further including applying a DC bias to scanning coils of the scanning transmission electron microscope.

10. A method of forming a nanostructure comprising:
selecting an amorphous oxide precursor material;
applying the oxide precursor material to a crystalline substrate to form a precursor layer;
positioning a scanning transmission electron microscope probe over the precursor layer; and
irradiating the precursor material with an electron beam from the scanning transmission electron microscope probe such that the electron beam impinges the precursor material and physically and chemically transforms the precursor material into an epitaxially grown crystalline oxide nanostructure.

11. The method according to claim 10 further including applying a DC bias to scanning coils of the scanning transmission electron microscope probe to control a location, a dwell time, and a raster speed of the electron beam.

12. The method according to claim 10 wherein said irradiating the precursor material with an electron beam includes repeated scans of the electron beam to achieve progressive epitaxial growth of the crystalline oxide nanostructure with each scan of the electron beam.

13. The method according to claim 12 further including slowing a scan rate of the electron beam between scans of the electron beam.

14. The method according to claim 10 further including scanning the precursor material with electron energy loss spectroscopy concurrently with each electron beam scan.

15. The method according to claim 10 wherein the amorphous oxide precursor material is an alkaline earth metal oxide.

Assignees

• Ut Battelle Llc

Inventors

• Borisevich Albina Y
• Jesse Stephen
• Kalinin Sergei V
• Lupini Andrew R
• Unocic Raymond R
• He Qian

Classifications

• H01J2237/31735

  Direct-write microstructures · CPC title

• C30B30/00

  Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions · CPC title

• H01J37/317

  for changing properties of the objects or for applying thin layers thereon, e.g. for ion implantation (H01J37/36 takes precedence) · CPC title

• H01J2237/2802

  Transmission microscopes · CPC title

• C30B29/16

  Oxides · CPC title