# US 10,400,351 B2 · Bulk nanofabrication with single atomic plane precision via atomic-level sculpting of crystalline oxides > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,400,351 B2 - Document ID: US10400351B2 - Status: Granted - Kind: B2 - Application number: 15/697,541 - Filed: 2017-09-07 - Published: 2018-03-08 - Granted: 2019-09-03 - Earliest claimed: 2016-09-07 - Assignees: UT-Battelle, LLC - Applicants: UT-Battelle, LLC - Inventors: Albina Y. Borisevich; Stephen Jesse; Sergei V. Kalinin; Andrew R. Lupini; Raymond R. Unocic; Qian He - Web page: https://patentgrep.com/patent/US10400351B2 ## CPC - C30B 1/00: Single-crystal growth directly from the solid state (unidirectional demixing of eutectoid materials C30B3/00; under a protective fluid C30B27/00) - C30B 19/10: Controlling or regulating (controlling or regulating in general G05) - C30B 29/02: Elements - C30B 29/16: Oxides - C30B 29/32: Titanates; Germanates; Molybdates; Tungstates - C30B 30/00: 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 - H01J 37/3005: {Observing the objects or the point of impact on the object} - H01J 37/317: for changing properties of the objects or for applying thin layers thereon, e.g. for ion implantation (H01J37/36 takes precedence) - H01J 37/3174: {Particle-beam lithography, e.g. electron beam lithography} - H01J 2237/2802: Transmission microscopes - H01J 2237/31735: Direct-write microstructures - H01J 2237/31747: using STM - C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR - H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H) ## 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. ## Claims ### Claim 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. ### Claim 2 (depends on 1) 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. ### Claim 3 (depends on 1) 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. ### Claim 4 (depends on 3) The method according to claim 3 further including slowing a scan rate of the scanning electron beam between scans of the scanning electron beam. ### Claim 5 (depends on 1) 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. ### Claim 6 (depends on 1) The method according to claim 1 wherein the amorphous oxide precursor material and the crystalline substrate are identical oxides. ### Claim 7 (depends on 1) The method according to claim 1 wherein the amorphous oxide precursor material is an alkaline earth metal oxide. ### Claim 8 (depends on 1) The method according to claim 1 wherein the amorphous oxide precursor material is strontium titanate. ### Claim 9 (depends on 1) The method according to claim 1 further including applying a DC bias to scanning coils of the scanning transmission electron microscope. ### Claim 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. ### Claim 11 (depends on 10) 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. ### Claim 12 (depends on 10) 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. ### Claim 13 (depends on 12) The method according to claim 12 further including slowing a scan rate of the electron beam between scans of the electron beam. ### Claim 14 (depends on 10) The method according to claim 10 further including scanning the precursor material with electron energy loss spectroscopy concurrently with each electron beam scan. ### Claim 15 (depends on 10) The method according to claim 10 wherein the amorphous oxide precursor material is an alkaline earth metal oxide.