# US 10,370,255 B2 · Method and apparatus for preparing boron nitride nanotubes by heat treating boron precursor prepared by using air-jet

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- Number: US 10,370,255 B2
- Document ID: US10370255B2
- Status: Granted
- Kind: B2
- Application number: 15/581,713
- Filed: 2017-04-28
- Published: 2018-08-02
- Granted: 2019-08-06
- Earliest claimed: 2017-02-02
- Assignees: Naieel Technology
- Applicants: NAiEEL Technology
- Inventors: Min Kyung Zo; Jaewoo Kim; Duck Bong Seo; Hee Jin Kim
- Web page: https://patentgrep.com/patent/US10370255B2

## CPC

- C01B 35/146: {Compounds containing boron and nitrogen, e.g. borazoles (ammonium tetrafluoborates C01B35/063; ammonium borates C01B35/12)}
- B01J 8/008: {Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction (B01J8/0285, B01J8/067, B01J8/087, B01J8/1836 take precedence)}
- B01J 8/009: {Membranes, e.g. feeding or removing reactants or products to or from the catalyst bed through a membrane}
- C01B 21/064: with boron
- C01B 21/0641: {Preparation by direct nitridation of elemental boron}
- C23C 16/342: {Boron nitride}
- C23C 16/4418: {Methods for making free-standing articles (C23C16/01 takes precedence)}
- B01J 2208/00008: Controlling the process
- B01J 2208/00017: Controlling the temperature
- C01P 2004/03: obtained by SEM
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/13: Nanotubes
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A method and apparatus for preparing boron nitride nanotubes (BNNTs) according to an embodiment may ensure mass-production, may increase yield by reducing a production time, and may prepare BNNTs with high purity. The method includes steps of providing a first powder including boron, forming a second powder including a boron precursor by nano-sizing the first powder, forming a precursor disk by mixing the second powder with a binder; and growing BNNTs on the precursor disk.

## Claims

### Claim 1

A method of preparing boron nitride nanotubes (BNNTs), the method comprising steps of:
providing a first powder by mixing boron and a catalyst powder;
forming a second powder comprising a boron precursor by nano-sizing the first powder;
forming a precursor disk having a thickness of 100 μm to 1000 μm by mixing 100 wt % of a precursor powder with 5 to 50 wt % of a binder including at least one of sugar, syrup, grain syrup, polypropylene carbonate, polyvinyl alcohol, polyvinyl butyral, and ethylcellulose; and
growing BNNTs on the precursor disk;
wherein the growing of the BNNTs on the precursor disk comprises steps of:
locating the precursor disk in a heating zone of a reaction chamber;
heating the heating zone; and
applying a reactive gas to the heating zone to thereby grow the BNNTs by forming pores on the precursor disk as the binder is sublimated and removed; and
wherein the nano-sizing of the first powder comprises steps of:
applying first air in a direction inclined to a perpendicular direction of a round nano-sizing area;
applying the first powder to the nano-sizing area to form an acute angle towards a flow direction of the first air; and
forming the second powder by using the first air in the nano-sizing area.

### Claim 2 (depends on 1)

The method of claim 1, further comprising a step of:
collecting the second powder in a second air in the nano-sizing area.

### Claim 3 (depends on 2)

The method of claim 2, wherein the step of collecting the second powder comprises steps of:
causing the second air to pass through a first membrane connected to the nano-sizing area;
causing the second air to be collected to a first collecting container for accommodating the first membrane;
causing the second air from the first collecting container to pass through a second membrane; and
accommodating the second powder in a receiver connected to the second membrane.

### Claim 4 (depends on 1)

The method of claim 1, further comprising steps of:
causing a rod to pass through a plurality of the precursor disks; and
locating the rod in the heating zone.

### Claim 5 (depends on 4)

The method of claim 4, further comprising steps of:
causing a cassette having a plurality of the rods to be positioned within a reaction chamber, wherein a reaction gas is supplied from a lower part of the cassette.