CN107522180A - A kind of preparation method of boron nitride nano-tube - Google Patents
A kind of preparation method of boron nitride nano-tube Download PDFInfo
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- CN107522180A CN107522180A CN201610452958.3A CN201610452958A CN107522180A CN 107522180 A CN107522180 A CN 107522180A CN 201610452958 A CN201610452958 A CN 201610452958A CN 107522180 A CN107522180 A CN 107522180A
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- boron nitride
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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
- C01B21/0648—After-treatment, e.g. grinding, purification
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- 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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
This application discloses a kind of preparation method of boron nitride nano-tube, and using amorphous boron powder as boron source, iron oxide is adjuvant, NH3For nitrogen source, at 1250~1350 DEG C, boron nitride nano-tube is synthesized by chemical vapour deposition technique.The boron nitride nano-tube yield height of the inventive method acquisition, pattern is good, purity is high.
Description
Technical field
The application belongs to field of material technology, more particularly to a kind of preparation method of boron nitride nano-tube.
Background technology
Boron nitride nano-tube has similar structure to CNT, and 1994, Rubio etc. was pre- in theory
Survey the presence of boron nitride nano-tube, nineteen ninety-five Chopra etc. and successfully synthesize boron nitride nano-tube, so as to
The research prelude of boron nitride nano-tube is pulled open.Boron nitride nano-tube has fabulous chemical stability and resistance to
Hot, theoretical and experimental study shows it as wide energy gap semiconductor, and electric property is not straight by its nanotube
Footpath and chiral influence.Boron nitride nano-tube also has the high tenacity and high intensity suitable with CNT,
Available for the enhancing of material, toughness reinforcing and modification.The unique performance of boron nitride nano-tube make its new material,
The numerous areas such as Nanosemiconductor Device, energy and material and biological medicine have important application value.
In the prior art, the preparation of boron nitride nanometer material has that synthesis condition is harsh, yield is small, purity
Low, the problems such as cost is high, seriously limit the performance study and practical application of boron nitride nanometer material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of boron nitride nano-tube, to overcome prior art
In deficiency.
To achieve the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of preparation method of boron nitride nano-tube, using amorphous boron powder as boron source,
Iron oxide is adjuvant, NH3For nitrogen source, at 1250~1350 DEG C, synthesized by chemical vapour deposition technique
Boron nitride nano-tube.
Preferably, in the preparation method of above-mentioned boron nitride nano-tube, the method comprising the steps of：
(1), amorphous boron nitride and croci are mixed；
(2) ball milling, is carried out to compound；
(3) 1250~1350 DEG C, are warming up to 5~10 DEG C/min heating rates, 3~4 hours reaction time,
In NH3Under gas, boron nitride nano-tube is formed by chemical gaseous phase depositing process；
(4), product cleaning and dry.
Preferably, in the preparation method of above-mentioned boron nitride nano-tube, in step (1), amorphous nitrogen
It is (40~45) to change boron and croci mol ratio:1.
Preferably, in the preparation method of above-mentioned boron nitride nano-tube, in step (2), ball radius
4~6mm, ratio of grinding media to material are (7~10)：1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 are small
When.
Preferably, in the preparation method of above-mentioned boron nitride nano-tube, the purity of amorphous boron nitride exists
More than 97%.
Preferably, in the preparation method of above-mentioned boron nitride nano-tube, the NH3Throughput is 50sccm
Preferably, in the preparation method of above-mentioned boron nitride nano-tube, in step (4), with watery hydrochloric acid,
Distilled water and ethanol are carried out after cleaning for several times to sample, and are dried in vacuum drying chamber.
Compared with prior art, the advantage of the invention is that：The boron nitride nano-tube that the inventive method obtains
Yield is high, pattern is good, purity is high.
Embodiment
The present invention is described further by the following example：, can be more preferably geographical according to following embodiments
The solution present invention.However, as it will be easily appreciated by one skilled in the art that specific material described by embodiment
The present invention is merely to illustrate than, process conditions and its result, without should be also without limitation on claims
In the described in detail present invention.
Embodiment 1
The preparation method of boron nitride nano-tube
(1), by amorphous boron nitride and croci mol ratio according to 40:1 ratio mixes, to mixing
Material carries out ball milling, ball radius 4mm, ratio of grinding media to material 10：1,500 turns/min of rotational speed of ball-mill, during ball milling
Between 5 hours；
(2) 1250 DEG C, are warming up to 10 DEG C/min heating rates, in NH3Under gas, pass through chemical gas
Mutually it is deposited on metal substrate surface and forms boron nitride nano-tube, 3 hours reaction time, NH3Throughput is
50sccm。
(3) after, carrying out cleaning for several times to sample with watery hydrochloric acid, distilled water and ethanol, and it is being dried in vacuo
Dried in case.
Product is analyzed by XRD, SEM, TEM and FTIR, it was demonstrated that product is boron nitride nano-tube.
Yield is 94%, purity 96%.
For the diameter of prepared nanotube between 40~100nm, length obtains nitrogen more than 200 μm
It is high to change boron nanotube purity.
The boron nitride nano-tube yield height of the inventive method acquisition, pattern is good, purity is high.
Embodiment 2
The preparation method of boron nitride nano-tube
(1), by amorphous boron nitride and croci mol ratio according to 45:1 ratio mixes, to mixing
Material carries out ball milling, ball radius 6mm, ratio of grinding media to material 7：1,600 turns/min of rotational speed of ball-mill, during ball milling
Between 5 hours；
(2) 1300 DEG C, are warming up to 8 DEG C/min heating rates, in NH3Under gas, pass through chemical gas
Mutually it is deposited on metal substrate surface and forms boron nitride nano-tube, 3 hours reaction time, NH3Throughput is
50sccm。
(3) after, carrying out cleaning for several times to sample with watery hydrochloric acid, distilled water and ethanol, and it is being dried in vacuo
Dried in case.
Product is analyzed by XRD, SEM, TEM and FTIR, it was demonstrated that product is boron nitride nano-tube.
Yield is 91%, purity 95%.
Embodiment 3
The preparation method of boron nitride nano-tube
(1), by amorphous boron nitride and croci mol ratio according to 40:1 ratio mixes, to mixing
Material carries out ball milling, ball radius 6mm, ratio of grinding media to material 7：1,600 turns/min of rotational speed of ball-mill, during ball milling
Between 5 hours；
(2) 1350 DEG C, are warming up to 10 DEG C/min heating rates, in NH3Under gas, pass through chemical gas
Mutually it is deposited on metal substrate surface and forms boron nitride nano-tube, 4 hours reaction time, NH3Throughput is
50sccm。
(3) after, carrying out cleaning for several times to sample with watery hydrochloric acid, distilled water and ethanol, and it is being dried in vacuo
Dried in case.
Product is analyzed by XRD, SEM, TEM and FTIR, it was demonstrated that product is boron nitride nano-tube.
Yield is 93%, purity 95%.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant meaning
Covering including for nonexcludability so that process, method, article including a series of elements or
Equipment not only includes those key elements, but also the other element including being not expressly set out, or also wraps
Include as this process, method, article or the intrinsic key element of equipment.
Claims (7)
- A kind of 1. preparation method of boron nitride nano-tube, it is characterised in that：Using amorphous boron powder as boron source, iron oxide is adjuvant, NH3For nitrogen source, at 1250~1350 DEG C, boron nitride nano-tube is synthesized by chemical vapour deposition technique.
- 2. the preparation method of boron nitride nano-tube according to claim 1, it is characterised in that the method comprising the steps of：(1), amorphous boron nitride and croci are mixed；(2) ball milling, is carried out to compound；(3) 1250~1350 DEG C, are warming up to 5~10 DEG C/min heating rates, 3~4 hours reaction time, in NH3Under gas, boron nitride nano-tube is formed by chemical gaseous phase depositing process；(4), product cleaning and dry.
- 3. the preparation method of boron nitride nano-tube according to claim 2, it is characterised in that：In step (1), amorphous boron nitride and croci mol ratio is (40~45):1.
- 4. the preparation method of boron nitride nano-tube according to claim 2, it is characterised in that：In step (2), 4~6mm of ball radius, ratio of grinding media to material is (7~10)：1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 hours.
- 5. the preparation method of boron nitride nano-tube according to claim 2, it is characterised in that：The purity of amorphous boron nitride is more than 97%.
- 6. the preparation method of boron nitride nano-tube according to claim 2, it is characterised in that：The NH3Throughput is 50sccm.
- 7. the preparation method of boron nitride nano-tube according to claim 2, it is characterised in that：In step (4), after carrying out cleaning for several times to sample with watery hydrochloric acid, distilled water and ethanol, and dried in vacuum drying chamber.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610452958.3A CN107522180A (en) | 2016-06-21 | 2016-06-21 | A kind of preparation method of boron nitride nano-tube |
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| CN201610452958.3A CN107522180A (en) | 2016-06-21 | 2016-06-21 | A kind of preparation method of boron nitride nano-tube |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113336202A (en) * | 2021-07-05 | 2021-09-03 | 南京大学 | High-purity boron nitride nanotube and preparation method thereof |
| WO2023019664A1 (en) * | 2021-08-20 | 2023-02-23 | 武汉工程大学 | Method for preparing boron nitride nanotube by means of double-transition metal oxide catalysis |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899956A (en) * | 2006-06-27 | 2007-01-24 | 华南理工大学 | Method for synthesizing single shape boron nitride nano tube |
| CN101633498A (en) * | 2009-09-01 | 2010-01-27 | 北京工业大学 | Preparation method of boron nitride nano tube with controllable dimension |
| CN103922295A (en) * | 2014-04-17 | 2014-07-16 | 河北工业大学 | Preparation method of boron nitride nano tube |
| CN105036096A (en) * | 2015-07-22 | 2015-11-11 | 哈尔滨工业大学 | Method for preparing high-purity boron nitride nanotubes through reaction gas vortexes |
-
2016
- 2016-06-21 CN CN201610452958.3A patent/CN107522180A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899956A (en) * | 2006-06-27 | 2007-01-24 | 华南理工大学 | Method for synthesizing single shape boron nitride nano tube |
| CN101633498A (en) * | 2009-09-01 | 2010-01-27 | 北京工业大学 | Preparation method of boron nitride nano tube with controllable dimension |
| CN103922295A (en) * | 2014-04-17 | 2014-07-16 | 河北工业大学 | Preparation method of boron nitride nano tube |
| CN105036096A (en) * | 2015-07-22 | 2015-11-11 | 哈尔滨工业大学 | Method for preparing high-purity boron nitride nanotubes through reaction gas vortexes |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113336202A (en) * | 2021-07-05 | 2021-09-03 | 南京大学 | High-purity boron nitride nanotube and preparation method thereof |
| WO2023019664A1 (en) * | 2021-08-20 | 2023-02-23 | 武汉工程大学 | Method for preparing boron nitride nanotube by means of double-transition metal oxide catalysis |
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Application publication date: 20171229 |