Production method for the boron nitride nanotubes

Patent metadata

Field	Value
Publication number	US-9487402-B2
Application number	US-201314898474-A
Country	US
Kind code	B2
Filing date	Jun 14, 2013
Priority date	Jun 14, 2013
Publication date	Nov 8, 2016
Grant date	Nov 8, 2016

Abstract

The present invention relates to a method, which essentially comprises the steps of performing crude boron nitride nanotube (BNNT) synthesis ( 110 ) and purifying BNNTs obtained in the crude form ( 120 ), and wherein direct BNNT production is provided with the use of colemanite that is a borate mineral.

First claim

The invention claimed is:

1. A method for producing boron nitride nanotubes (BNNTs), comprising the steps of:
synthesizing crude BNNTs, wherein the step of synthesizing the crude BNNTs further comprises sub-steps of:
mixing colemanite, catalyst and pure water to obtain a first mixture;
pre-heating the first mixture after taking the first mixture into a container;
heating the pre-heated first mixture in a furnace under NH 3 atmosphere;
cooling the furnace;
collecting crude BNNTs by removing the container from the furnace to obtain the crude BNNTs; and

purifying the crude BNNTs, wherein the step of purifying the crude BNNTs comprising the sub-steps of;
mixing, the crude BNNTs with a hydrochloric acid (HCl) solution after adding the crude BNNTs into the hydrochloric acid (HCl) solution to obtain a second mixture;
centrifuging the second mixture;
stirring the centrifuged second mixture after adding the centrifuged second mixture into a nitric acid (HNO 3 ) solution to obtain a third mixture;
centrifuging the third mixture;
obtaining pure BNNTs as a result of washing and drying after the precipitated solid is separated.

2. The method for producing the boron nitride nanotubes according to claim 1 , wherein the catalyst comprises at least one of metal oxides.

3. The method for producing the boron nitride nanotubes according to claim 2 , wherein 0.15-0.17 g metal oxide and 2 mL of pure water are used per 2 g of colemanite in the step of mixing the colemanite, catalyst and the pure water.

4. The method for producing the boron nitride nanotubes according to claim 2 , wherein the metal oxides are Fe 2 O 3 or MgO or the combination thereof.

5. The method for producing the boron nitride nanotubes according to claim 1 , wherein the step of pre-heating the first mixture in a container further comprises a sub-step of vaporizing the pure water by heating at 150-180° C. for 10-20 minutes in an alumina boat.

6. The method for producing the boron nitride nanotubes according to claim 1 , wherein the container which holds the first mixture, is placed in the center of a tubular furnace and the pre-heating step is applied to remove water from the first mixture, wherein the pre-heating step is performed under the NH 3 atmosphere in a high temperature furnace.

7. The method for producing the boron nitride nanotubes according to claim 6 , wherein the first mixture is heated in a furnace with a heating rate of 8° C./minute for 3 hours until the temperature reaches 1250-1300° C. in step of heating the first mixture in the high temperature furnace.

8. The method for producing the boron nitride nanotubes according to claim 7 , wherein the temperature of the furnace is decreased to 500-550° C. in step of cooling the furnace.

9. The method for producing the boron nitride nanotubes according to claim 1 , wherein the container in which the BNNTs are present is removed from the cooled furnace and the BNNTs therein are collected and preserved in dry room conditions in step of collecting the crude BNNTs by removing the container from the furnace.

10. The method for producing the boron nitride nanotubes ( 100 ) according to claim 1 , the crude BNNTs are stirred in 50 mL of 4 M HCl solution for 4 hours at 90° C. in the step of mixing the crude BNNTs by adding into the hydrochloric acid (HCl) solution.

11. The method for producing the boron nitride nanotubes according to claim 1 , wherein the second mixture stirred in HCl acid solution is subjected to centrifuging for 30 minutes at 14000 rpm in the step of centrifuging the mixture.

12. The method for producing the boron nitride nanotubes according to claim 1 , wherein the centrifuged second mixture is taken to 30 ml, of 1 M HNO 3 solution and stirred for 6 hours at 30° C. in the step of stirring the centrifuged second mixture by adding into the nitric acid (HNO 3 ) solution.

13. The method for producing the boron nitride nanotubes according to claim 1 , wherein the third mixture stirred in HNO 3 solution is subjected to centrifuging for 30 minutes at 14000 rpm in the step of centrifuging the third mixture.

14. The method for producing the boron nitride nanotubes according to claim 1 , wherein the BNNTs precipitated are dried at 50-60° C. in step of obtaining pure BNNTs as a result of washing and drying the precipitated solid by separating.

Assignees

• Univ Yeditepe

Inventors

• Culha Mustafa

Classifications

• C01P2002/84

  by UV- or VIS- data · CPC title

• C01P2002/72

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

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01B21/0646 Primary

  Preparation by pyrolysis of boron and nitrogen containing compounds · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title