KR20160118835A - Apparatus and method of fabricating boron nitride nanotube - Google Patents

Apparatus and method of fabricating boron nitride nanotube Download PDF

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Publication number
KR20160118835A
KR20160118835A KR1020150047629A KR20150047629A KR20160118835A KR 20160118835 A KR20160118835 A KR 20160118835A KR 1020150047629 A KR1020150047629 A KR 1020150047629A KR 20150047629 A KR20150047629 A KR 20150047629A KR 20160118835 A KR20160118835 A KR 20160118835A
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South Korea
Prior art keywords
boride
boron nitride
process chamber
carbon rod
manufacturing
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KR1020150047629A
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Korean (ko)
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오인섭
김영광
염경태
임병직
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주식회사바텍
(주)바텍이우홀딩스
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Priority to KR1020150047629A priority Critical patent/KR20160118835A/en
Publication of KR20160118835A publication Critical patent/KR20160118835A/en

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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
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • 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

Abstract

The present invention provides an apparatus for producing a boron nitride nanotube comprising: a process chamber; a negative electrode carbon rod positioned within the process chamber; a positive electrode carbon rod which causes arc discharge with the negative electrode carbon rod and where a graphite powder mixture containing a metal catalyst is filled inside; and a gas injection port for injecting boron nitride precursor gas in the process chamber.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to an apparatus and a method for fabricating a boron nitride nanotube,

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for manufacturing boron nitride nanotubes, and more particularly, to an apparatus and a method for manufacturing boron nitride nanotubes capable of producing boron nitride nanotubes by an arc discharge method. will be.

X-ray source performance plays a decisive role in industrial non-destructive imaging and medical radiographic imaging in order to obtain images with good contrast and resolution.

In the prior art, a thermionic emitter that emits electrons at a high temperature using a filament was used as an electron source of an X-ray source, that is, an electron emitter. However, since the thermoelectromotive emitter has to be raised to a temperature higher than 1000 degrees for electron emission, the power consumption is relatively large and the emitter can not be turned on and off instantly.

In order to improve this, a field emitter type emitter which emits electrons by using quantum mechanical tunneling by an electric field is widely used.

In terms of miniaturization of the X-ray source, a nanometer-sized material other than the conventional metal or semiconductor material is used as a field emission emitter. Particularly, researches for using a carbon nano tube (CNT) It is actively proceeding.

In recent years, boron nitride nanotubes (BNNTs), which are structurally similar to CNTs but have a wide band gap (5.5 eV) and are not sensitive to diameters and chirality, ) Are being studied.

Conventionally, a CCVD (combustion chemical vapor deposition) method using a precursor and a floating catalyst has been generally used in manufacturing BNNTs.

However, when the conventional CCVD method is used, the synthesis time of the BNNT is long and the production yield is poor.

The present invention has a problem to provide a method for improving the production efficiency by shortening the synthesis time of BNNT.

In order to achieve the above-mentioned object, the present invention provides a process chamber comprising: a process chamber; A negative electrode carbon rod positioned within the process chamber; A cathode carbon rod having an anode filled with a graphite powder mixture containing a metal catalyst and causing an arc discharge with the anode carbon rod; And a gas injection port for injecting a boron nitride precursor gas into the process chamber.

Here, the graphite powder mixture may include a boride.

The boride may be selected from the group consisting of barium hexaboride (B 6 Ba), tantalum boride (TaB), molybdenum boride (Mo 2 B), hafnium (B 2 Hf), zirconium boride (B 2 Zr), samarium boride (SmB 6 ), calcium boride (CaB 6 ), chromium boride Chromium boride (CrB 2)), cobalt boride (cobalt boride (Co 2 B- Co 3 B)), gadori titanium boride (Gadolinium boride (GdB 6)) , iron boride (Iron boride (FeB)), lanthanum boride (Lanthanum boride (LaB 6)) , neodymium boride (neodymium boride (NdB 6)) , nickel boride (nickel boride (Ni 2 B) ), titanium boride (titanium boride (B 2 Ti) ), niobium (NbB 2 ), tungsten boride (WB + W 2 B), vanadium boride (VB), and magnesium boride (B 2 Mg) Done It may include one or more selected from the group.

The boride may be contained in an amount of 0.01 to 8 parts by weight based on 100 parts by weight of the graphite powder mixture.

The BN precursor may be selected from the group consisting of polyborazylene (B 3 H 6 N 3 ), borane triethylamine (C 2 H 5 ) 3 N BH 3 ), trichloroborazine (H 3 B 3 Cl 3 N 3 )).

And another gas inlet for injecting a buffer gas into the process chamber.

The buffer gas, hydrogen (H 2), nitrogen (N 2), ammonia (NH 3), hydrogen / helium (H 2 / He), hydrogen / nitrogen (H 2 / N 2), a hydrogen / argon (H 2 / Ar), hydrogen / helium / ammonia (H 2 / He / NH 3 ).

And a storage container configured to generate bubbles in the BN precursor solution contained therein to supply the BN precursor gas to the process chamber.

And a heater installed on the outer wall of the process chamber and operated to remove impurities remaining in the process chamber.

In another aspect, the present invention provides a method comprising: injecting a buffer gas and a BN precursor gas into a process chamber; Generating a boron nitride nanotube by generating an arc discharge between a negative electrode carbon rod disposed in the process chamber and a positive carbon rod filled with a graphite powder mixture containing a metal catalyst therein, ≪ / RTI >

Here, after the boron nitride nanotubes are formed, a step of activating the heater to remove the impurities remaining in the process chamber may be performed.

The amount of the BN precursor gas injected may be 10 sccm to 60 sccm.

The passivation step may be performed at a temperature of 500 ° C to 850 ° C for 20 minutes to 70 minutes.

According to the present invention, BNNTs are produced using an arc discharge method. Accordingly, the BNNT can be manufactured in a very short time compared with the conventional method, and the production efficiency is improved to a considerable extent.

Further, impurities can be removed through the passivation process, and the purity of the BNNT can be improved.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view of a BNNT manufacturing apparatus according to an embodiment of the present invention; FIG.
2 is a schematic illustration of a BNNT manufacturing method according to an embodiment of the present invention.
FIG. 3 is a photograph of a BNNT produced by an arc discharge method according to an embodiment of the present invention, using an electron microscope. FIG.
FIG. 4 is a graph showing the results of EELS (electron energy loss spectroscopy) analysis of BNNTs produced by an arc discharge method according to an embodiment of the present invention.

Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

1 is a view schematically showing a BNNT manufacturing apparatus according to an embodiment of the present invention.

Referring to FIG. 1, an arc discharge apparatus is used as the BNNT manufacturing apparatus 10 of the present invention. Such a BNNT manufacturing apparatus 10 may include a process chamber 100, a heater 110, a negative electrode carbon rod and a positive electrode carbon rod 120, and a gas inlet 151 and 152.

The process chamber 100 has an internal space S defined therein. In the inner space S, a process gas is injected for BNNT synthesis by arc discharge, and arc discharge is generated to synthesize BNNT. The synthesized BNNT is formed inside the process chamber 100. After the BNNT synthesis is completed, the BNNT formed therein is collected.

In the process chamber 100, a negative electrode carbon rod and a positive electrode carbon rod 120, 130, in which arc discharge occurs during BNNT synthesis, are disposed.

The negative electrode carbon rods 120 and the positive electrode carbon rods 130 may be arranged such that their longitudinal directions are coincident with each other and the ends thereof face each other.

In other words, the anode carbon rods 120 and the anode carbon rods 130 may be arranged in an on-axis manner in which longitudinal axes coincide with each other.

As another example, the anode carbon rods 120 and the anode carbon rods 130 may be arranged in an off-aixs shape in which the longitudinal directions intersect with each other. As described above, in the case of being disposed in an off-axis manner, arc discharge occurs through the outer peripheral surface of the negative electrode carbon rod 120, so that the arc discharge area can be widened as compared with the on-axis arrangement.

Meanwhile, a filling hole 133 is formed in the positive electrode carbon rod 130 along the longitudinal direction from the end facing the negative electrode carbon rod 120.

The filling hole 133 is filled with the graphite powder mixture 135. The graphite powder mixture 135 may comprise graphite powder and a metal catalyst. In addition, the graphite powder mixture 135 may further comprise a boride.

Examples of the metal catalyst that promotes the synthesis of BNNT include a group consisting of nickel (Ni), copper (Cu), bismuth (Bi), iron (Fe), iron sulfide (FeS), cobalt (Co), and yttrium And < / RTI >

The borides are, for example, barium hexaboride (B 6 Ba), tantalum boride (TaB), molybdenum boride (Mo 2 B), hafnium borate (B 2 Hf), zirconium boride (B 2 Zr), samarium boride (SmB 6 ), calcium boride (CaB 6 ), chromium boride (Chromium boride (CrB 2)) , cobalt boride (cobalt boride (Co 2 B- Co 3 B)), gadori titanium boride (Gadolinium boride (GdB 6)) , iron boride (Iron boride (FeB) ), Lanthanum boride (LaB 6 ), neodymium boride (NdB 6 ), nickel boride (Ni 2 B), titanium boride (B 2 Ti) ), Niobium boride (NbB 2 ), tungsten boride (WB + W 2 B), vanadium boride (VB), magnesium boride (B 2 Mg) )) And may include one or more selected from the group consisting of the < RTI ID = 0.0 >

When the borides are mixed together, the boride is preferably mixed at a ratio of about 0.01 to 8 parts by weight based on 100 parts by weight of the graphite powder mixture 135, but is not limited thereto.

On the other hand, in the BNNT synthesis, it is preferable that power is applied between the anode carbon rods and the anode carbon rods 120 and 130 so as to have a potential difference of 25V in the current range of about 50A to 200A, but the present invention is not limited thereto.

The length of the anode carbon rod 130 is preferably about 300 mm, the outer diameter is about 10 mm, and the diameter of the inner filling hole 133 is preferably about 3 mm, but is not limited thereto.

In addition, the anode carbon rod 130 may be configured to move linearly in the longitudinal direction. To this end, a motor may be connected to the positive electrode rod 130. When the anode carbon rod 130 is moved in the longitudinal direction, the distance to the anode carbon rod 120 can be adjusted, and the intensity of the arc discharge can be controlled.

The heater 110 may be installed on the outer wall of the process chamber 100, but is not limited thereto. The heater 110 may be installed inside the process chamber 100.

The heater 110 maintains the temperature of the internal space S at a predetermined level during the BNNT synthesis process, thereby lengthening the growth time of the BNNT. As a result, generation of impurities such as amorphous carbon and nanoparticles can be suppressed to the utmost, and the yield and purity of BNNT can be improved.

Furthermore, the heater 110 can operate to be heated even in the heat treatment step performed after the BNNT synthesis step. Here, the passivation step is preferably, but not limited to, performed for 20 minutes to 70 minutes at a temperature range of, for example, approximately 500 to 850 degrees.

Thus, by carrying out the heat treatment for the synthesized BNNT, it is possible to improve the purity of BNNT by removing impurities such as amorphous carbon and nanoparticles remaining in the process chamber.

The process chamber 100 is provided with gas injection ports 151 and 152 for injecting gas into the internal space S.

A plurality of gas injection holes 151 and 152 may be provided. For example, a first gas injection hole 151 for injecting a buffer gas G1 and a second gas injection hole 151 for injecting a boron nitride precursor gas G2 A second gas inlet 152 may be provided.

Of course, if desired, the process chamber 100 may be provided with a single gas inlet, and the buffer gas and the BN precursor gas may be injected together through the gas inlet.

Here, the buffer gas (G1) is hydrogen (H 2), nitrogen (N 2), ammonia (NH 3), hydrogen / helium (H 2 / He), hydrogen / nitrogen (H 2 / N 2), hydrogen / argon (H 2 / Ar), and hydrogen / helium / ammonia (H 2 / He / NH 3 ).

The BN precursors include polyborazylene (B 3 H 6 N 3 ), borane triethylamine (C 2 H 5 ) 3 N BH 3 ), trichloroborazine (H 3 B 3 Cl 3 N 3 )).

Here, the flow rate of the BN precursor gas G2 is preferably about 10 sccm to 60 sccm, but the present invention is not limited thereto.

The second injection port 152 may be connected to the storage container 160 for storing the BN precursor solution 165 through the injection pipe 161 when supplying the BN precursor gas G2.

Bubbles are generated in the BN precursor solution 165 when the BN precursor solution 165 is contained in the storage container 160 and gas is injected into the storage container 160. That is, the storage container 160 functions as a gas bubbler.

Thus, a gaseous BN precursor or BN precursor gas G2 can be fed into the process chamber 100 through the injection tube 161.

The BN precursor gas G2 thus supplied is synthesized with the material vaporized in the anode carbon rod 130 by arc discharge, so that the BNNT can be formed.

Here, the BNNT formed through the arc discharge according to the embodiment of the present invention may have a diameter of about 150 nm or less.

Hereinafter, a method of manufacturing a CNT using the CNT manufacturing apparatus 10 having the above-described configuration will be described with reference to FIG.

Referring to FIG. 2, first, the graphite powder mixture 135 is filled in the filling hole 133 in the anode carbon rod 130 (ST1).

Here, the graphite powder mixture 135 may include a catalytic metal, and may further include a boride.

Next, a buffer gas is injected into the process chamber 100, and a BN precursor gas is injected into the process chamber 100 (ST2).

Next, a voltage is applied to the negative electrode carbon rod and the positive electrode carbon rods 120 and 130 to generate arc discharge to generate BNNT (ST3).

Next, the heater 110 is operated to raise the temperature inside the process chamber 100 to perform the heat treatment. Thus, impurities in the process chamber 100 can be removed to improve the purity of the BNNT.

FIG. 3 is a photograph of a BNNT produced by an arc discharge method according to an embodiment of the present invention using an electron microscope. FIG. 4 is a graph showing the electron energy (EELS) of a BNNT produced by an arc discharge method according to an embodiment of the present invention. loss spectroscopy analysis results. In Fig. 4, the abscissa is the energy loss and the unit is <eV>, and the ordinate is the frequency of the relative electron, and the unit is <au>.

Referring to FIGS. 3 and 4, it can be seen that the BNNT was manufactured without any problem through the arc discharge method according to the embodiment of the present invention.

As described above, according to the embodiment of the present invention, the BNNT is manufactured using the arc discharge method. Accordingly, the BNNT can be manufactured in a very short time compared with the conventional method, and the production efficiency is improved to a considerable extent.

Further, impurities can be removed through the passivation process, and the purity of the BNNT can be improved.

The embodiment of the present invention described above is an example of the present invention, and variations are possible within the spirit of the present invention. Accordingly, the invention includes modifications of the invention within the scope of the appended claims and equivalents thereof.

10: CNT manufacturing apparatus 100: Process chamber
110: Heater 120: Negative electrode carbon rod
130: positive electrode carbon rod 133: filling hole
135: Graphite powder mixture 151: First gas inlet
152: second gas inlet 160: storage container
161: Injection tube 165: BN precursor solution
G1: Buffer gas
G2: BN precursor gas

Claims (13)

A process chamber;
A negative electrode carbon rod positioned within the process chamber;
A cathode carbon rod having an anode filled with a graphite powder mixture containing a metal catalyst and causing an arc discharge with the anode carbon rod;
A gas inlet for injecting a boron nitride precursor gas into the process chamber;
Wherein the boron nitride nanotubes are in contact with each other.
The method according to claim 1,
Wherein the graphite powder mixture comprises a boride
A device for manufacturing a boron nitride nanotube.
3. The method of claim 2,
The boride may be selected from the group consisting of barium hexaboride (B 6 Ba), tantalum boride (TaB), molybdenum boride (Mo 2 B), hafnium (B 2 Hf), zirconium boride (B 2 Zr), samarium boride (SmB 6 ), calcium boride (CaB 6 ), chromium boride Chromium boride (CrB 2)), cobalt boride (cobalt boride (Co 2 B- Co 3 B)), gadori titanium boride (Gadolinium boride (GdB 6)) , iron boride (Iron boride (FeB)), lanthanum boride (Lanthanum boride (LaB 6)) , neodymium boride (neodymium boride (NdB 6)) , nickel boride (nickel boride (Ni 2 B) ), titanium boride (titanium boride (B 2 Ti) ), niobium (NbB 2 ), tungsten boride (WB + W 2 B), vanadium boride (VB), and magnesium boride (B 2 Mg) Done Comprising at least one selected from the group
A device for manufacturing a boron nitride nanotube.
3. The method of claim 2,
The boride is contained in a proportion of 0.01 to 8 parts by weight based on 100 parts by weight of the graphite powder mixture
A device for manufacturing a boron nitride nanotube.
The method according to claim 1,
The BN precursor may be selected from the group consisting of polyborazylene (B 3 H 6 N 3 ), borane triethylamine (C 2 H 5 ) 3 N BH 3 ), trichloroborazine (H 3 B 3 Cl 3 N 3 )) and at least one selected from the group consisting of
A device for manufacturing a boron nitride nanotube.
The method according to claim 1,
The other gas inlet for injecting the buffer gas into the process chamber
Wherein the boron nitride nanotubes are in contact with each other.
The method according to claim 6,
The buffer gas, hydrogen (H 2), nitrogen (N 2), ammonia (NH 3), hydrogen / helium (H 2 / He), hydrogen / nitrogen (H 2 / N 2), a hydrogen / argon (H 2 / Ar), hydrogen / helium / ammonia (H 2 / He / NH 3 )
A device for manufacturing a boron nitride nanotube.
The method according to claim 1,
A reservoir container configured to generate bubbles in the BN precursor solution contained therein to supply the BN precursor gas to the process chamber;
Wherein the boron nitride nanotubes are in contact with each other.
The method according to claim 1,
A heater installed on an outer wall of the process chamber and operable to remove impurities remaining in the process chamber,
Wherein the boron nitride nanotubes are in contact with each other.
Injecting a buffer gas and a BN precursor gas into the process chamber;
Generating a boron nitride nanotube by generating an arc discharge between a negative electrode carbon rod disposed in the process chamber and a positive carbon rod filled with a graphite powder mixture including a metal catalyst therein
Wherein the boron nitride carbon nanotubes are prepared by a method comprising the steps of:
11. The method of claim 10,
Performing a heat treatment to remove the impurities remaining in the process chamber by activating the heater after the boron nitride nanotubes are produced,
Wherein the boron nitride nanotubes have a thickness of about 10 nm to about 100 nm.
11. The method of claim 10,
The amount of the BN precursor gas injected is 10 sccm to 60 sccm
A method for manufacturing a boron nitride nanotube.
12. The method of claim 11,
The passivation step is performed at a temperature of 500 to 850 degrees for 20 to 70 minutes
A method for manufacturing a boron nitride nanotube.
KR1020150047629A 2015-04-03 2015-04-03 Apparatus and method of fabricating boron nitride nanotube KR20160118835A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111825463A (en) * 2020-06-29 2020-10-27 井冈山大学 LaB6-CrB2Composite cathode material and preparation method thereof
KR20210015497A (en) * 2019-08-02 2021-02-10 한국과학기술연구원 A device for continuous production of boron nitride and the method for producing the same
KR20230027747A (en) * 2021-08-20 2023-02-28 한국과학기술연구원 Method for manufacturing boron nitride nanotube

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20210015497A (en) * 2019-08-02 2021-02-10 한국과학기술연구원 A device for continuous production of boron nitride and the method for producing the same
CN111825463A (en) * 2020-06-29 2020-10-27 井冈山大学 LaB6-CrB2Composite cathode material and preparation method thereof
KR20230027747A (en) * 2021-08-20 2023-02-28 한국과학기술연구원 Method for manufacturing boron nitride nanotube

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