Single-step synthesis of nanostructured thin films by a chemical vapor and aerosol deposition process

Patent metadata

Field	Value
Publication number	US-10593928-B2
Application number	US-201514830361-A
Country	US
Kind code	B2
Filing date	Aug 19, 2015
Priority date	Aug 20, 2014
Publication date	Mar 17, 2020
Grant date	Mar 17, 2020

Abstract

The present disclosure is generally directed to a single-step synthesis of nanostructured thin films by a chemical vapor and aerosol deposition (CVAD) process. The present disclosure is also directed to methods for controlling the morphology of the nanostructured thin films. The films can be used, for example, in lithium ion and/or sodium ion battery electrodes, solar cells and gas sensors.

First claim

What is claimed is:

1. A chemical vapor and aerosol deposition process for preparation of a metal species-based nanostructured film comprising niobium doped titanium dioxide nanoparticles, the process comprising:
introducing at least one vaporized metal precursor into a reaction chamber, wherein the reaction chamber includes a temperature controlled metal substrate;
decomposing, at least in part, the at least one vaporized precursor to form metal species-based nanoparticles in the reaction chamber;
depositing the nanoparticles and any remaining vaporized precursor onto the temperature controlled metal substrate in the reaction chamber; and,
sintering the nanoparticles to form the metal species-based nanostructured film in the reaction chamber, wherein the nanostructured film has a morphology selected from the group consisting of a predominantly columnar morphology, a predominantly granular morphology, a predominantly nanorod morphology, a predominantly nanowire morphology, and a predominantly branched morphology.

2. The process of claim 1 , wherein the metal species-based nanoparticles further comprise a metal oxide selected from the group consisting of lithium titanate, aluminum titanate, tin oxide, lithium manganese oxide, lithium cobalt oxide, lithium manganese nickel cobalt oxide, nickel oxide, copper oxide, and combinations thereof.

3. The process of claim 1 , wherein the nanostructure is of a predominantly columnar morphology.

4. The process of claim 3 , wherein the columnar morphology has a crystalline order of from about 1 nanometer to about 5 micrometers.

5. The process of claim 1 , wherein the at least one precursor is selected from the group consisting of titanium tetraisopropoxide (TTIP), niobium ethoxide, aluminum tri-secbutoxide (ATSB), tetramethyl tin (TMT), 2,2,6,6-tetramethyl-3,5-heptanedionato lithium [Li (TMHD)], lithium dipivaloylmethanate [Li(DPM)], lithium acetylacetonate and combinations thereof.

6. The process of claim 1 , wherein the film has a thickness of from about 10 nanometers to about 1 millimeter.

7. The process of claim 1 , wherein the nanoparticles have an average particle size of less than about 100 nanometers.

8. The process of claim 1 , wherein the temperature controlled substrate is controlled to a temperature of from about 20° C. to about 1000° C.

9. The process of claim 1 , wherein the nanostructured film comprises a niobium doping percentage in a range of from about 0.1% to about 10% by weight of the nanostructured film.

10. An anode for an ion battery comprising a metal species-based nanostructured film directly deposited onto a metal substrate, the film comprising nanoparticles and having a single crystal dendritic nanostructure morphology.

11. The anode of claim 10 , wherein the metal species-based nanoparticles comprise a metal oxide selected from the group consisting of lithium titanate, aluminum titanate, titanium dioxide, tin oxide, lithium manganese oxide, lithium cobalt oxide, lithium manganese nickel cobalt oxide, nickel oxide, copper oxide, and combinations thereof.

12. The anode of claim 10 , wherein the nanostructure morphology is a columnar morphology having a crystalline order of from about 1 nanometer to about 5 micrometers.

13. The anode of claim 10 , wherein the nanostructure morphology is a nanorod morphology and comprises tin oxide nanoparticles.

14. The anode of claim 10 , wherein the film comprises niobium doped titanium dioxide nanoparticles.

15. A chemical vapor and aerosol deposition process for production of an ion battery anode, the process comprising:
introducing at least one vaporized metal precursor into a reaction chamber, wherein the reaction chamber includes a temperature controlled metal substrate current collector;
decomposing, at least in part, the at least one vaporized precursor to form metal species-based nanoparticles in the reaction chamber;
directly depositing the nanoparticles and any remaining vaporized precursor onto the temperature controlled metal substrate current collector in the reaction chamber; and,
sintering the nanoparticles to form the metal species-based nanostructured anode in the reaction chamber, wherein the nanostructured anode has a morphology selected from the group consisting of a predominantly columnar morphology, a predominantly granular morphology, a predominantly nanorod morphology, a predominantly nanowire morphology, and a predominantly branched morphology.

16. The process of claim 15 , wherein the at least one precursor is selected from the group consisting of titanium tetraisopropoxide, niobium ethoxide, 2,2,6,6-tetramethyl-3,5-heptanedionato lithium, tetramethyl tin and combinations thereof.

17. The process of claim 15 , wherein the metal species-based nanoparticles comprise a metal oxide selected from the group consisting of lithium titanate, tin oxide, titanium dioxide and combinations thereof.

18. The process of claim 15 , wherein the anode comprises niobium doped titanium dioxide nanoparticles.

19. The process of claim 15 , wherein the anode is selected from the group consisting of a lithium ion battery anode and a sodium ion battery anode.

20. The process of claim 15 , wherein the anode comprises tin oxide nanoparticles.

Assignees

• Univ Washington

Inventors

• Chadha Tandeep Singh
• Biswas Pratim
• An Woo-Jin

Classifications

• C23C16/4551

  Jet streams · CPC title

• H01M4/485

  of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy (H01M4/505, H01M4/525 take precedence) · CPC title

• H01M4/1391

  of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01G1/02

  Oxides · CPC title