IP Library Granted Patent US 12,286,347
Granted Patent B2
US 12,286,347 · App. 16/647,959 · Granted Apr 29, 2025

Boron nitride nanotube (BNNT)-nanoparticle composites, methods for the preparation thereof and their macroscopic assemblies

Inventors: Keun Su Kim (Ottawa, CA); Benoit Simard (Ottawa, CA); Christopher Thomas Kingston (Ottawa, CA); Homin Shin (Ottawa, CA)
Assignee: National Research Council of Canada
C01B21/0646C01B21/0648B82Y30/00B82Y40/00C01P2002/82C01P2002/84C01P2004/04C01P2004/13
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 12,286,347
App. No.
16/647,959
Granted
Apr 29, 2025
Kind
B2
Abstract

The present application relates to boron nitride nanotube (BNNT)-nanoparticle composites, to methods of preparing such composites and their use, for example, in metal/ceramic matrix composites and/or macroscopic assemblies. For example, the methods comprise subjecting a source of hydrogen, a source of boron, a source of nitrogen and a nanoparticle precursor to a stable induction thermal plasma and cooling the reaction mixture to obtain the composite.

Claims (18)

1. A method for preparing a boron nitride nanotube (BNNT)-nanoparticle composite, the method comprising:

subjecting a source of hydrogen, a source of boron, a source of nitrogen and a nanoparticle precursor that is a non-catalytic metal or a non-catalytic ceramic to a stable induction thermal plasma to form a reaction mixture in the plasma; and

cooling the reaction mixture to obtain the BNNT-nanoparticle composite with nanoparticles attached to on outer surface of BNNTs.

2. The method of claim 1 , wherein the stable induction thermal plasma has a plasma temperature of about 1,000 K to about 10,000 K.

3. The method of claim 1 , wherein the reaction mixture is formed in the plasma at a pressure of less than 2 atm.

4. The method of claim 1 , wherein (a) the source of boron is boron nitride, elemental boron, borane, ammonia borane (borazane), borazine, a boron trihalide, a metal boride or mixtures thereof; (b) the source of nitrogen is boron nitride, N 2 , NH 3 , NH 4 OH, borazane, borazine or mixtures thereof; and/or (c) the source of hydrogen is H 2 , NH 3 , NH 4 OH, borane, borazane, borazine or mixtures thereof.

5. The method of claim 1 , wherein the nanoparticle precursor is a metal ceramic, or a metallic element or alloy.

6. The method of claim 5 , wherein the nanoparticle precursor is aluminum nitride (AIN), gallium nitride (GaN), tantalum nitride (TaN), tungsten nitride (W 2 N, WN, WN 2 ), magnesium nitride (Mg 3 N 2 ) or titanium nitride (TIN).

7. The method of claim 6 , wherein the nanoparticle precursor is AIN.

8. The method of claim 5 , wherein the nanoparticle precursor is copper metal, aluminum metal, silver metal, gold metal, gallium metal or magnesium metal.

9. The method of claim 8 , wherein the nanoparticle precursor is copper metal.

10. The method of claim 1 , wherein the source of boron is hexagonal boron nitride (h-BN); the source of nitrogen is a mixture of hexagonal boron nitride (h-BN) and N 2 ; and the source of hydrogen is H 2 .

11. The method of claim 10 , wherein the N 2 and H 2 are introduced into the stable induction plasma in a sheath gas.

12. The method of claim 11 , wherein the sheath gas further comprises argon.

13. The method of claim 10 , wherein the h-BN and the nanoparticle precursor are introduced into the stable induction plasma as a powder.

14. The method of claim 13 , wherein the ratio by weight of the h-BN to the nanoparticle precursor is from about 99:0.1 to about 50:50.

15. The method of claim 14 , wherein the ratio by weight of the h-BN to the nanoparticle precursor is from about 93.5:6.5 to about 50:50.

16. The method of claim 1 , wherein cooling the reaction mixture comprises cooling in a reaction zone downstream of the stable induction plasma.

Continuity (2)
Provisional Application 62561405 · Sep 21, 2017
Related Publication 20200216317A1 · Jul 9, 2020
References Cited (65)
US 8703023B2 · Sainsbury et al. · 2014 [cited by applicant]
US 20090214799A1 · Simard et al. · 2009 [cited by applicant]
US 20130064750A1 · Zettl · 2013 [cited by applicant]
US 20150033937A1 · Lashmore et al. · 2015 [cited by applicant]
US 20150125374A1 · Smith et al. · 2015 [cited by applicant]
US 20150125380A1 · Biris et al. · 2015 [cited by applicant]
US 20160083253A1 · Kim et al. · 2016 [cited by applicant]
CA 2877060C · 2014 [cited by applicant]
JP 2013538887A · 2013 [cited by applicant]
JP 2016521240A · 2016 [cited by applicant]
JP 2017132662A · 2017 [cited by examiner]
WO WO2014169382A1 · 2014 [cited by examiner]
WO 2015200496A1 · 2015 [cited by applicant]
WO 2017136574A1 · 2017 [cited by applicant]
Kumar et al.; Copper Catalyzed Growth of Hexagonal Boron Nitride Nanotubes on Tungsten Substrate; CrystEngComm; 20, 2713-2719; Apr. 3, 2018. [cited by examiner]
Gao et al.; Noncovalent Functionalization of Boron Nitride Nanotubes in Aqueous Media Opens Application Roads in Nanobiomedicine; Nanobiomedicine, vol. 1; Jan. 2014. [cited by examiner]
Zhi et al.; Boron Nitride Nanotubes: Functionalization and Composites; Journal of Materials Chemistry; 18, 3900-3908; 2008. [cited by examiner]
Zettl et al.; Self-Assembly of Gold Nanoparticles at the Surface of Amine- and Thiol-Functionalized Boron Nitride Nanotubes; J. Phys. Chem. C; 111, 12992-12999; 2007. [cited by examiner]
Dai X.-J., et al. (2011) Controlled Surface Modification of Boron Nitride Nanotubes. Nanotechnology. 22, 245301. 8 pages. [cited by applicant]
Ikuno T., et al. (2007) Amine-Functionalized Boron Nitride Nanotubes. ScienceDirect. Solid State Communications. 142, 643-646. [cited by applicant]
Malik R., et al. (2013) Atmospheric Pressure Plasma Functionalization of Dry-Spun Multi-Walled Carbon Nanotubes Sheets and its Application in CNT-Polyvinyl Alcohol (PVA) Composites. Mater. Res. Soc. Symp. Proc. 1574. DO… [cited by applicant]
Park O.-K., et al. (2015) Effect of Oxygen Plasma Treatment on the Mechanical Properties of Carbon Nanotube Fibers. Materials Letters. 156, 17-20. [cited by applicant]
Chen H., et al. (2007) Eu-Doped Boron Nitride Nanotubes as a Nanometer-Sized Visible-Light Source. Adv. Mater. 19, 1845-1848. [cited by applicant]
Chen Y.-J., et al. (2007) Tunable Electric Conductivities of Au-Doped Boron Nitride Nanotubes. NANO: Brief Reports and Reviews. 2(6), 367-372. [cited by applicant]
Chen H., et al. (2008) Nano Au-Decorated Boron Nitride Nanotubes: Conductance Modification and Field-Emission Enhancement. Applied Physics Letters. 92, 243105. 4 pages. [cited by applicant]
Chen H., et al. (2008) Rare-Earth Doped Boron Nitride Nanotubes. Materials Science and Engineering B. 146, 189-192. [cited by applicant]
Chen Z.-G., et al. (2008) Self-Assembly and Cathodoluminescence of Microbelts from Cu-Doped Boron Nitride Nanotubes. ACS Nano. 2(8), 1523-1532. [cited by applicant]
Cho Y.-J., et al. (2009) Electronic Structure of Si-Doped BN Nanotubes Using X-ray Photoelectron Spectroscopy and First-Principles Calculation. Chem. Mater. 21, 136-143. [cited by applicant]
Fathalizadeh A., et al. (2014) Scaled Synthesis of Boron Nitride Nanotubes, Nanoribbons, and Nanococoons Using Direct Feedstock Injection into an Extended-Pressure, Inductively-Coupled Thermal Plasma. Nano Letters. dx.d… [cited by applicant]
Gao Z., et al. (2011) Nucleotide-Assisted Decoration of Boron Nitride Nanotubes with Semiconductor Quantum Dots Endows Valuable Visible-Light Emission in Aqueous Solution. Soft Matter. 7, 8753-8756. [cited by applicant]
Georgakilas V., et al. (2007) Decorating Carbon Nanotubes with Metal or Semiconductor Nanoparticles. Journal of Materials Chemistry. 17, 2679-2694. [cited by applicant]
Han W.-Q., et al. (2003) Functionalized Boron Nitride Nanotubes with a Stannic Oxide Coating: A Novel Chemical Route to Full Coverage. J. Am. Chem. Soc. 125, 2062-2063. [cited by applicant]
Huang Y., et al. (2010) BN Nanotubes Coated with Uniformly Distributed Fe304 Nanoparticles: Novel Magneto- Operable Nanocomposites. Journal of Materials Chemistry. 20, 1007-1011. [cited by applicant]
Kim K.-S., et al. (2014) Hydrogen-Catalyzed, Pilot-Scale Production of Small-Diameter Boron Nitride Nanotubes and Their Macroscopic Assemblies. ACS Nano. 8(6), 6211-6220. [cited by applicant]
Lahiri D., et al. (2013) Boron Nitride Nanotubes Reinforced Aluminum Composites Prepared by Spark Plasma Sintering: Microstructure, Mechanical Properties and Deformation Behavior. Materials Science and Engineering: A. 5… [cited by applicant]
Lee C.-H., et al. (2013) Room-Temperature Tunneling Behavior of Boron Nitride Nanotubes Functionalized with Gold Quantum Dots. Adv. Mater. 25, 4544-4548. [cited by applicant]
Lee C.-M., et al. (2006) Synthesis of Boron Nitride Nanotubes by Arc-Jet Plasma. Current Applied Physics. 6, 166-170. [cited by applicant]
Li R., et al. (2014) Non-Covalent Surface Modification of Boron Nitride Nanotubes for Enhanced Catalysis. Chem. Commun. 50, 225-227. [cited by applicant]
Oh S.-I., et al. (2012) Fabrication of Carbon Nanofiber Reinforced Aluminum Alloy Nanocomposites by a Liquid Process. Journal of Alloys and Compounds. 542, 111-117. [cited by applicant]
Oku T., et al. Synthesis, Atomic Structures and Electronic States of Boron Nitride Nanocage Clusters and Nanotubes. Institute of Scientific and Industrial Research. Osaka University. Osaka, Japan. Undated manuscript. [cited by applicant]
Pham T., et al. (2015) A Universal Wet-Chemistry Route to Metal Filling of Boron Nitride Nanotubes. Nano Letters. DOI: 10.1021/acs.nanolett.5b03874. [cited by applicant]
Ponraj S.-B., et al. (2014) Fabrication of Boron Nitride Nanotube-Gold Nanoparticle Hybrids Using Pulsed Plasma in Liquid. Langmuir. 30,10712-10720. [cited by applicant]
Tang C., et al. (2003) Boron Nitride Nanotubes Filled with Ni and NiSi2 Nanowires in Situ. J. Phys. Chem. B. 107, 6539-6543. [cited by applicant]
Terrones M., et al. (2007) Pure and Doped Boron Nitride Nanotubes. Materials Today. 10(5), 30-38. [cited by applicant]
Wei X., et al. (2010) Post-Synthesis Carbon Doping of Individual Multiwalled Boron Nitride Nanotubes via Electron-Beam Irradiation. J. Am. Chem. Soc. 132, 13592-13593. [cited by applicant]
Yamaguchi M., et al. (2012) Synthesis, Structural Analysis and in Situ Transmission Electron Microscopy Mechanical Tests on Individual Aluminum Matrix/Boron Nitride Nanotube Nanohybrids. Acta Materialia. 60, 6213-6222. [cited by applicant]
Yu Y., et al. (2015) A Facile Strategy for the Functionalization of Boron Nitride Nanotubes with Pd Nanoparticles. Journal of Nanomaterials. Article ID 310214. http://dx.doi.org/10.1155/2015/310214. 5 pages. [cited by applicant]
Zhi C., et al. (2005) Immobilization of Proteins on Boron Nitride Nanotubes. J. Am. Chem. Soc. 127, 17144-17145. [cited by applicant]
Zhi C., et al. (2006) SnO2 Nanoparticle-Functionalized Boron Nitride Nanotubes. J. Phys. Chem. B. 110, 8548-8550. [cited by applicant]
Office Action on Korean Application No. 10-2020-7007327 dated Jun. 27, 2023. [cited by applicant]
English Translation of Office Action on Korean Application No. 10-2020-7007327 dated Jun. 27, 2023. [cited by applicant]
Office Action on Korean Application No. 10-2020-7007327 dated Jan. 30, 2024. [cited by applicant]
English Translation of Office Action on Korean Application No. 10-2020-7007327 dated Jan. 30, 2024. [cited by applicant]
Notice of Reasons for Rejection dated Apr. 26, 2022. [cited by applicant]
English Translation of Notice of Reasons for Rejection dated Apr. 26, 2022. [cited by applicant]
English Abstract of JP 2013538887. [cited by applicant]
English Abstract of JP 2016521240. [cited by applicant]
English Abstract of JP 2017132662. [cited by applicant]
Partial Supplementary European Search Report dated May 7, 2021. [cited by applicant]
Extended European Search Report dated Jun. 18, 2021. [cited by applicant]
Tiano, A. L. et al. (2014) Boron Nitride Nanotube: Synthesis and Applications. Proceedings of SPIE. 9060. 906006-1-906006-19. 19 pages. [cited by applicant]
Office Action on Korean Application No. 10-2020-7007327 dated Jun. 26, 2024. [cited by applicant]
English Translation of Office Action on Korean Application No. 10-2020-7007327 dated Jun. 26, 2024. [cited by applicant]
Office Action on European Application No. 18858873.5 dated Sep. 27, 2024. [cited by applicant]
Office Action on Canadian Application No. 3,076,087 dated Oct. 29, 2024. [cited by applicant]