CN111268656A - Preparation method of boron nitride nanotube - Google Patents

Preparation method of boron nitride nanotube Download PDF

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CN111268656A
CN111268656A CN202010085418.2A CN202010085418A CN111268656A CN 111268656 A CN111268656 A CN 111268656A CN 202010085418 A CN202010085418 A CN 202010085418A CN 111268656 A CN111268656 A CN 111268656A
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boron nitride
boron
catalyst
mgb
source
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姚亚刚
俄松峰
张凯
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Zhejiang Boju New Material Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C01B21/0641—Preparation by direct nitridation of elemental boron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13—Nanotubes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

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Abstract

The invention discloses a preparation method of a boron nitride nanotube by using a catalyst. The preparation method uses MgB2And as a catalyst, forming boron nitride nanotubes on the growth substrate by a chemical vapor deposition method by using a boron source and a nitrogen source. The process of the invention is suitable for use in B2O3，H3BO3B/CaO, borate compounds and other boron sources can efficiently catalyze the growth of the boron nitride nanotube in a horizontal tube furnace without using a sleeve device, and the prepared boron nitride nanotube has a small diameter of about 30-50 nm.

Description

Preparation method of boron nitride nanotube
Technical Field
The invention belongs to the technical field of inorganic nano material preparation, and particularly relates to a preparation method of a boron nitride nanotube.
Background
The Boron Nitride Nanotubes (BNNTs) have excellent mechanical, thermal, high temperature resistant, oxidation resistant and neutron absorption performances, and have potential application values in the fields of aerospace, thermal interface materials, composite materials, radiation shielding, biomedicine, deep ultraviolet emission and the like. While good synthesis technology is the basis for realizing application, the synthesis of BNNTs is very difficult, and the batch preparation technology is still a great challenge in the academia and the industry. The current synthesis methods mainly include plasma methods, ball milling annealing methods and Chemical Vapor Deposition (CVD).The plasma method can obtain nanotubes with small diameter and thin wall, and can realize the large-scale preparation of BNNTs (Nano Lett.,2014,14, 4881-. Ball milling annealing also achieves a greater number of BNNTs (chem. Phys. Lett.,1999,299,260 and appl. Phys. Lett.,1999,74,2960), but this method generally requires a longer ball milling annealing time, with the ball milling process being at high pressure NH3The operation is inconvenient, and most of the obtained nanotubes are bamboo-shaped, but not ideal cylindrical structures.
CVD is one of the most likely routes to achieve bulk production of BNNTs, with reference to the production history of Carbon Nanotubes (CNTs). Boron Oxide Chemical Vapor Deposition (BOCVD) is one of the most common methods for preparing BNNTs by CVD, using a boron oxide (B) formed by reaction at high temperature using a mixture of boron and a metal oxide as a precursor2O2) And NH3BNNTs (chem.commun.,2002,1290) were grown by action. Through research in recent 20 years, boron/magnesium oxide/ferrous oxide (B/MgO/FeO) has gradually become the most classical precursor (Solid State commun.,2005,135,67) of the method, however, this precursor can only prepare BNNTs efficiently in vertical tube furnace, and has low efficiency in horizontal tube furnace, even can not grow BNNTs.
Based on this, Yap et al (Nanotechnology,2008,19,455605, chem. mater.2010,22,1782), university of michigan, overcome the above problem with a double tube arrangement (placing a quartz tube closed at one end inside another quartz tube), using B/MgO/FeO to successfully prepare BNNTs in a horizontal tube furnace, and considering MgO as a catalyst for the reaction. The method can efficiently prepare the BNNTs in the horizontal tube furnace, but needs a sleeve device, and has a complicated operation process. Another important drawback of this method is that the catalytic activity of MgO has not been experimentally verified and the growth mechanism of BNNTs has not been clearly studied.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides a method for manufacturing a semiconductor deviceMethod for preparing boron nitride nanotubes using a catalyst of MgB2The method can efficiently catalyze the growth of the boron nitride nanotubes in a horizontal tube furnace without using a sleeve device.
Another object of the present invention is to provide a method for using MgB2The boron nitride nanotube prepared by using the catalyst has the diameter of 30-50 nm.
In order to achieve the purpose, the invention adopts the technical scheme that:
with MgB2And as a catalyst, forming boron nitride nanotubes on the growth substrate by a chemical vapor deposition method by using a boron source and a nitrogen source.
An embodiment of the present invention provides a method for preparing a boron nitride nanotube, including:
mixing a boron source and a compound with MgB2The growth substrate of the catalyst is placed in a chemical vapor growth device, and the boron source and the MgB are2The catalysts are distributed in sequence along the advancing direction of the carrier gas;
and raising the temperature in the chemical vapor growth equipment to 1100-1600 ℃ in a protective atmosphere, and then introducing a nitrogen source for heat preservation reaction for 1-5h to form the boron nitride nanotube on the growth substrate.
In a preferred embodiment, the boron source is selected from B2O3、H3BO3B/CaO, borate compounds or a combination thereof.
Further, when the boron source is B/CaO, the molar ratio of B to CaO is 1: 1-6: 1.
In a preferred embodiment, the nitrogen source is selected from the group consisting of NH3Or N2。
In a preferred technical scheme, the boron source is configured with MgB2The distance between the growth substrates of the catalyst is 3-8 cm.
In a preferred technical scheme, the MgB2The catalyst is placed in an open reaction vessel, and the growth substrate is disposed above the open reaction vessel.
Further, the growth substrate is a silicon wafer; the chemical vapor growth equipment is a horizontal tube furnace, and the tube furnace tube is made of corundum; and/or the open reaction vessel is an alumina crucible.
In a preferred technical scheme, the protective atmosphere is argon atmosphere, and the flow rate of the argon gas is 100-500 sccm.
In the preferable technical scheme, the temperature of the heat preservation reaction is 1200-1400 ℃, and the time of the heat preservation reaction is 2-3 h.
Compared with the prior art, the invention has the following technical effects:
(1) with MgB2The catalyst can be used for preparing BNNTs efficiently in a horizontal tube furnace without using a sleeve device, and the prepared nanotubes have small diameters of about 30-50 nm;
(2) MgB discovered by the invention2The catalyst may be the intrinsic catalyst of the B/MgO system;
(3) the invention has good reproducibility and is less influenced by the atmosphere of the tube furnace.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1: the invention discloses a picture of a tubular furnace of chemical vapor deposition equipment of an experimental device;
FIG. 2 a: optical photograph before reaction of catalyst and silicon chip;
FIG. 2 b: an optical photograph after the reaction of the catalyst and the silicon wafer;
FIG. 3: b is2O3BNNTs SEM morphology prepared for boron source;
FIG. 4: b is2O3BNNTs TEM topography prepared for boron source;
FIG. 5: b is2O3BNNTs Raman spectra prepared for boron sources;
FIG. 6: b is2O3BNNTs FTIR spectra prepared for boron source;
FIG. 7: b is2O3BNNTs EDS spectra prepared for boron source;
FIG. 8: b is2O3Contact angle photographs of BNNTs films prepared for boron source;
FIG. 9: b is2O3Cathodoluminescence spectra (CL) of BNNTs films prepared for boron sources;
FIG. 10: h3BO3BNNTs SEM morphology prepared for boron source;
FIG. 11: h3BO3BNNTs TEM topography prepared for boron source;
FIG. 12: BNNTs SEM appearance prepared by B/CaO as boron source;
FIG. 13: the B/CaO is the appearance of BNNTs TEM prepared by a boron source.
Detailed Description
The present invention will be more fully understood from the following detailed description, which should be read in conjunction with the accompanying drawings. Detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which can be embodied in various forms. Therefore, specific functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed embodiment.
Referring to fig. 1 and 2, a method for preparing a boron nitride nanotube according to an embodiment of the present invention is described, which includes: with MgB2And as a catalyst, forming boron nitride nanotubes on the growth substrate by a chemical vapor deposition method by using a boron source and a nitrogen source.
Specifically, a boron source and MgB configured therewith are first introduced2The growth substrate of the catalyst is placed in a chemical vapor growth device, a boron source and MgB2The catalysts are distributed in sequence along the advancing direction of the carrier gas; secondly, raising the temperature in the chemical vapor growth equipment to 1100-1600 ℃ in a protective atmosphere, then introducing a nitrogen source, and carrying out heat preservation reaction for 1-5hAnd forming the boron nitride nanotube on the growth substrate.
In one embodiment, the boron source is selected from B2O3、H3BO3At least one of B/CaO, borate compounds or their combination, boron source and MgB compound2The distance between the growth substrates of the catalyst is 3-8 cm. And, when the boron source is B/CaO, the molar ratio of B to CaO is from 2:1 to 6: 1.
In one embodiment, the nitrogen source is selected from NH3Or N2(ii) a The protective atmosphere is argon atmosphere, and the flow rate of the argon is 100-500 cubic centimeters per minute; the temperature of the heat preservation reaction is 1100-1600 ℃, and the time of the heat preservation reaction is 1-5 h.
In a particular arrangement, as shown in FIG. 1, MgB2The catalyst is placed in an open reaction vessel, and a growth substrate is arranged above the open reaction vessel, wherein the growth substrate can be selected from various materials including silicon wafers. Here, the growth substrate is usually a part of the opening covering the open reaction container, but in other embodiments, the growth substrate may be suspended above the open reaction container, and these simple variations are within the scope of the present invention.
In one embodiment, the open reaction vessel is an alumina crucible.
The chemical vapor deposition equipment used in this embodiment is a horizontal tube furnace made of corundum.
In one embodiment, the diameter of the prepared boron nitride nanotube is 30-50 nm.
MgB in the invention2As a catalyst for preparing boron nitride nanotubes, the high catalytic efficiency of the boron nitride nanotubes is derived from MgB2The high-temperature liquid state characteristic and the satisfaction of the vapor-liquid-solid (VLS) growth mechanism of the one-dimensional nano material. The catalyst can be applied to B2O3,H3BO3B/CaO, borate and the like, and can efficiently catalyze the growth of BNNTs in a horizontal tube furnace without a sleeve device.
In the present invention, B2O3Directly as a source of boron, H3BO3Pyrolysis to produce B2O3High temperature of B/CaOReaction to form B2O2Or B2O3The experimental equations for the latter two are shown below:
2H3BO3(l)→B2O3(g)+3H2O(g) (1)
2B(s)+2CaO(s)→2Ca(l)+B2O2(g) (2)
2B(s)+3CaO(s)→3Ca(l)+B2O3(g) (3)
catalyst MgB of the invention2Theoretically, the method can catalyze other boron sources (such as borate and the like) to grow BNNTs, and provides a theoretical basis for the mass preparation of BNNTs; the BNNTs deposited on the surface of the monocrystalline silicon by the method are expected to be used in the field of super-hydrophobicity.
The technical scheme of the invention is further explained by combining the attached drawings and a plurality of embodiments.
Example 1: weighing 50 mg of MgB2The catalyst was placed in an arc open alumina crucible, 1 silicon wafer 1.5cm x 1.5cm was placed above it, and the crucible was placed in a tube furnace heating thermostat zone. Then, 0.5 g of B was weighed2O3The powder was placed in another alumina crucible and placed 8cm in front of the catalyst. The reaction system is heated to 1300 ℃ in 200sccm Ar, and then Ar is switched to 200sccm NH3And reacting at 1300 ℃ for 2 h. After the reaction was completed, the reaction system was cooled to room temperature in 200sccm Ar, the tube furnace was opened, the crucible was taken out, and it was observed that a layer of white substance, BNNTs, was coated on the surface of the silicon wafer (FIGS. 3-9).
Example 2: weighing 50 mg of MgB2The catalyst was placed in an arc open alumina crucible, 1 silicon wafer 1.5cm x 1.5cm was placed above it, and the crucible was placed in a tube furnace heating thermostat zone. Then, 0.5 g of H was weighed3BO3The powder was placed in another alumina crucible and placed 8cm in front of the catalyst. The reaction system is heated to 1300 ℃ in 200sccm Ar, and then Ar is switched to 200sccm NH3And reacting at 1300 ℃ for 2 h. After the reaction is finished, the reaction system is cooled to room temperature in 200sccm Ar, the tube furnace is opened, the crucible is taken out, and a layer of white substance, namely BNNT, is seen to cover the surface of the silicon wafers (FIGS. 10-11).
Example 3: weighing 50 mg of MgB2The catalyst was placed in an arc open alumina crucible, 1 silicon wafer 1.5cm x 1.5cm was placed above it, and the crucible was placed in a tube furnace heating thermostat zone. Then, an appropriate amount of B/CaO powder mixture with a molar ratio of 2:1 was placed in another alumina crucible and placed 3cm in front of the catalyst. The reaction system is heated to 1300 ℃ in 200sccm Ar, and then Ar is switched to 200sccm NH3And reacting at 1300 ℃ for 2 h. After the reaction was completed, the reaction system was cooled to room temperature in 200sccm Ar, the tube furnace was opened, the crucible was taken out, and it was observed that a layer of white substance, BNNTs, was coated on the surface of the silicon wafer (FIGS. 12-13).
Example 4: weighing 50 mg of MgB2The catalyst was placed in an arc open alumina crucible, 1 silicon wafer 1.5cm x 1.5cm was placed above it, and the crucible was placed in a tube furnace heating thermostat zone. Then, an appropriate amount of B/CaO powder mixture with a molar ratio of 4:1 was placed in another alumina crucible and placed 3cm in front of the catalyst. The reaction system is heated to 1100 ℃ in 100sccm Ar, and then Ar is switched to 200sccm NH3And reacting at 1100 ℃ for 5 hours. After the reaction is finished, the reaction system is cooled to room temperature in 100sccm Ar, the tube furnace is opened, the crucible is taken out, and a layer of white substances, namely BNNTs, is covered on the surface of the silicon wafer.
Example 5: weighing 50 mg of MgB2The catalyst was placed in an arc open alumina crucible, 1 silicon wafer 1.5cm x 1.5cm was placed above it, and the crucible was placed in a tube furnace heating thermostat zone. Then, an appropriate amount of B/CaO powder mixture with a molar ratio of 6:1 was placed in another alumina crucible and placed 3cm in front of the catalyst. The reaction system is heated to 1600 ℃ in 500sccm Ar, and then Ar is switched to 200sccm NH3And reacting at 1600 ℃ for 1 h. After the reaction is finished, the reaction system is cooled to room temperature in 500sccm Ar, the tube furnace is opened, the crucible is taken out, and a layer of white substances, namely BNNTs, is seen to cover the surface of the silicon wafer.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.

Claims (12)

1. The preparation method of the boron nitride nanotube is characterized in that MgB is used2And as a catalyst, forming boron nitride nanotubes on the growth substrate by a chemical vapor deposition method by using a boron source and a nitrogen source.
2. The method for preparing boron nitride nanotubes according to claim 1, specifically comprising:
mixing a boron source and a compound with MgB2The growth substrate of the catalyst is placed in a chemical vapor growth device, and the boron source and the MgB are2The catalysts are distributed in sequence along the advancing direction of the carrier gas;
and raising the temperature in the chemical vapor growth equipment to 1100-1600 ℃ in a protective atmosphere, and then introducing a nitrogen source for heat preservation reaction for 1-5h to form the boron nitride nanotube on the growth substrate.
3. The method for producing boron nitride nanotubes according to claim 1 or 2, wherein the boron source is selected from B2O3、H3BO3B/CaO, borate compounds or a combination thereof.
4. The method for preparing boron nitride nanotubes according to claim 3, wherein when the boron source is B/CaO, the molar ratio of B to CaO is 1:1 to 6: 1.
5. The method for producing boron nitride nanotubes according to claim 1 or 2, wherein the nitrogen source is selected from NH3Or N2。
6. The method of claim 2, wherein the boron source and the MgB are configured2The distance between the growth substrates of the catalyst is 3-8 cm.
7. The method of claim 2, wherein the MgB is present in the form of a powder2The catalyst is placed in an open reaction vessel, and the growth substrate is disposed above the open reaction vessel.
8. The method of claim 7, wherein the growth substrate is a silicon wafer.
9. The method for preparing boron nitride nanotubes according to claim 7, wherein the chemical vapor growth equipment is a horizontal tube furnace, and the tube furnace is made of corundum; and/or the open reaction vessel is an alumina crucible.
10. The method as claimed in claim 2, wherein the protective atmosphere is argon gas, and the flow rate of argon gas is 100-500 standard cubic centimeters per minute (sccm).
11. The method for preparing boron nitride nanotubes of claim 2, wherein the temperature of the incubation reaction is 1200 ℃ and 1400 ℃, and the time of the incubation reaction is 2-3 h.
12. The boron nitride nanotubes produced by the method according to any one of claims 1 to 11, wherein the diameter of the boron nitride nanotubes is 30 to 50 nm.
CN202010085418.2A 2020-02-10 2020-02-10 Preparation method of boron nitride nanotube Pending CN111268656A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113213438A (en) * 2021-06-23 2021-08-06 南京大学 Boron nitride nanotubes and method for producing the same
CN113336202A (en) * 2021-07-05 2021-09-03 南京大学 High-purity boron nitride nanotube and preparation method thereof
CN113353899A (en) * 2021-05-24 2021-09-07 上海硼矩新材料科技有限公司 Preparation method of boron nitride nanotube, boron nitride nanotube and application of boron nitride nanotube

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SONGFENG E等: ""Growth of boron nitride nanotubes from magnesium diboride catalysts"", 《NANOSCALE》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113353899A (en) * 2021-05-24 2021-09-07 上海硼矩新材料科技有限公司 Preparation method of boron nitride nanotube, boron nitride nanotube and application of boron nitride nanotube
CN113353899B (en) * 2021-05-24 2022-09-23 南京大学 A kind of preparation method of boron nitride nanotube, boron nitride nanotube and application thereof
CN113213438A (en) * 2021-06-23 2021-08-06 南京大学 Boron nitride nanotubes and method for producing the same
CN113336202A (en) * 2021-07-05 2021-09-03 南京大学 High-purity boron nitride nanotube and preparation method thereof

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Application publication date: 20200612