BORON NITRIDE MATERIAL AND METHOD OF PREPARATION THEREOF

• US 20190016600A1
• Filed: 01/09/2017
• Published: 01/17/2019
• Est. Priority Date: 01/08/2016
• Status: Active Grant

• Current Assignee: Nanyang Technology University
• Original Assignee: Nanyang Technology University
• Inventors: TAY, Yingjie Roland, LI, Hongling, TSANG, Siu Hon, TEO, Hang Tong Edwin
• Granted Patent: US 10,457,553 B2
• Time in Patent Office: Days
• CPC Class Codes: C01B 21/064 with boron
• CPC Class Codes: C01P 2002/60 Compounds characterised by their crystallite size
• CPC Class Codes: C04B 2235/5284 Hollow fibers, e.g. nanotubes
• CPC Class Codes: C04B 2235/5288 Carbon nanotubes
• CPC Class Codes: C04B 2235/6028 Shaping around a core which is removed later
• CPC Class Codes: C04B 35/583 based on boron nitride
• CPC Class Codes: C04B 35/62218 obtaining ceramic films, e.g. by using temporary supports
• CPC Class Codes: C04B 35/6229 based on boron nitride
• CPC Class Codes: C04B 35/62868 Boron nitride
• CPC Class Codes: C04B 38/0022 obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
• CPC Class Codes: C04B 38/0029 Porous deposits from the gas phase, e.g. on a temporary support
• CPC Class Codes: C04B 38/04 by dissolving-out added substances
• CPC Class Codes: C04B 38/0615 the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles C04B38/0022 takes precedence
• CPC Class Codes: C23C 16/01 on temporary substrates, e.g. substrates subsequently removed by etching
• CPC Class Codes: C23C 16/0227 by cleaning or etching
• CPC Class Codes: C23C 16/342 Boron nitride
• CPC Class Codes: C23C 16/36 Carbonitrides
• CPC Class Codes: C23C 16/56 After-treatment
• CPC Class Codes: C30B 25/02 Epitaxial-layer growth
• CPC Class Codes: C30B 25/18 characterised by the substrate
• CPC Class Codes: C30B 29/403 : AIII-nitrides
• CPC Class Codes: C30B 29/602 : Nanotubes

Abstract

A method of preparing a boron nitride material, such as boron nitride (BN) or boron carbonitride (BCN), is provided. The method may include providing a substrate, and sublimating an amine borane complex onto the substrate to obtain the boron nitride material. The amine borane complex may include, but is not limited to, borazine, amino borane, trimethylamine borane and triethylamine borane. In addition, the temperature at which the sublimating is carried out may be varied to control composition of the boron nitride material formed. In addition, various morphologies can be obtained by using the present method, namely films, nanotubes and porous foam.

Claims

1. A method of preparing a boron nitride material, the method comprising

providing a substrate, and

sublimating an amine borane complex onto the substrate to obtain the boron nitride material, wherein temperature at which the sublimating is carried out is varied to control composition of the boron nitride material formed.

2. The method according to claim 1, wherein the boron nitride material is a boron nitride nanotube.

3. The method according to claim 2, wherein providing the substrate comprises providing a substrate having a layer of a metal in discrete particulate form arranged on a support.

4. The method according to claim 2, wherein providing the substrate comprises providing a substrate having one or more carbon nanotubes.

5. The method according to claim 4, further comprising removing the one or more carbon nanotubes by annealing the substrate following sublimating of the amine borane complex onto the substrate in an environment containing oxygen at a temperature in the range of about 400°

C. to about 700°

C.

7. The method according to claim 1, wherein providing the substrate comprises providing a layer of a metal arranged on a porous support to form the boron nitride material as a porous boron nitride material.

8. The method according to claim 7, further comprising removing the substrate by subjecting the substrate to an etching process following sublimating of the amine borane complex onto the substrate.

10. The method according to claim 1, wherein providing the substrate comprises providing a layer of a metal in continuous form arranged on a support to form the boron nitride material as a boron nitride film.

11. The method according to claim 10, further comprising removing the substrate by subjecting the substrate to an electrochemical delamination process following sublimating of the amine borane complex onto the substrate.

12. The method according to claim 1, wherein providing the substrate comprises annealing the substrate in an inert environment at a temperature of about 700°

C. or more.

13. The method according to claim 1, further comprising carrying out the sublimating of the amine borane complex onto the substrate for a time period in the range from about 5 minutes to about 20 minutes to form the boron nitride material as a monolayer on the substrate.

15. The method according to claim 1, wherein the amine borane complex has general formula

R₃N.BX₃,

wherein

X at each occurrence is independently selected from the group consisting of hydrogen and a halogen, and

R at each occurrence is independently selected from the group consisting of hydrogen, a substituted or unsubstituted C₁-C₂₀ alkyl, a substituted or unsubstituted C₁-C₂₀ alkoxy, a substituted or unsubstituted C₂-C₂₀ alkenyl, a substituted or unsubstituted C₂-C₂₀ alkynyl, a substituted or unsubstituted C₃-C₂₀ alicyclic group, a substituted or unsubstituted C₅-C₁₅ aryl, a substituted or unsubstituted C₆-C₃₀ alkyl-aryl, a substituted or unsubstituted C₃-C₂₀ heterocycle, a substituted or unsubstituted C₄-C₃₀ alkyl-heterocycle, a substituted or unsubstituted C₅-C₁₅ heteroaryl, —

NR″

R′

, —

NR″

, —

OR, —

SR″

, —

CN, —

NO₂, —

C(O)—

R″

, —

COOR″

, —

C(O)—

NR″

R′

, —

C(NR″

)—

R′

, —

SO₂—

R″

, —

(SO₂)—

OR″

, —

C(S)—

R″

, and —

C(S)—

NR″

R′

; and

R″ and

R′

are independently selected from the group consisting of H, a halogen, a substituted or unsubstituted C₁-C₂₀ alkyl, a substituted or unsubstituted C₁-C₂₀ alkoxy, a substituted or unsubstituted C₂-C₂₀ alkenyl, a substituted or unsubstituted C₂-C₂₀ alkynyl, and a substituted or unsubstituted C₅-C₁₅ aryl.

17. The method according to claim 15, wherein R is independently a linear or branched, unsubstituted alkyl with 1 to 20 carbon atoms.

20. The method according to claim 1, further comprising carrying out the sublimating of the amine borane complex at a temperature of less than about 100°

C. to form the boron nitride material as a boron nitride material doped with about 0 wt % to about 5 wt % carbon.

22. The method according to claim 20, wherein the boron nitride material comprises one or more single-crystal domains, wherein each of the one or more single-crystal domains has a maximal dimension of 100 μ

m or more.

24. The method according to claim 1, further comprising carrying out the sublimating of the amine borane complex at a temperature of about 50°

C. or less.

25. The method according to claim 24, wherein the boron nitride material consists essentially of boron nitride.

26. The method according to claim 1, further comprising carrying out the sublimating of the amine borane complex at a temperature greater than about 50°

C. and less than about 100°

C.

27. The method according to claim 26, wherein the boron nitride material is formed as a boron nitride material doped with about 2 wt % to about 5 wt % carbon.

28. The method according to claim 1, further comprising carrying out the sublimating of the amine borane complex at a temperature of about 100°

C. or more to form the boron nitride material as a boron nitride composite comprising one or more domains of boron nitride and carbon.

6. (canceled)

9. (canceled)

14. (canceled)

16. (canceled)

18-19. -19. (canceled)

21. (canceled)

23. (canceled)

29-30. -30. (canceled)