CN1424254A - Preparation of boron nitride nano tube - Google Patents
Preparation of boron nitride nano tube Download PDFInfo
- Publication number
- CN1424254A CN1424254A CN 03114737 CN03114737A CN1424254A CN 1424254 A CN1424254 A CN 1424254A CN 03114737 CN03114737 CN 03114737 CN 03114737 A CN03114737 A CN 03114737A CN 1424254 A CN1424254 A CN 1424254A
- Authority
- CN
- China
- Prior art keywords
- nts
- powder
- boron nitride
- temperature
- nitride nano
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- Granted
Links
- 239000002071 nanotube Substances 0.000 title claims abstract description 9
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 238000002360 preparation method Methods 0.000 title description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010453 quartz Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 229910000608 Fe(NO3)3.9H2O Inorganic materials 0.000 abstract 1
- 235000013877 carbamide Nutrition 0.000 abstract 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
A process for preparing nanotubes of boron nitride (BN-NTs) includes such steps as dissolving H3BO3, CO(NH2)2 and Fe(NO3)3.9H2O or Co(NO3)2.6H2O, or Ni(NO3)2.6H2O) in deionized water, vacuum drying to obtain mixture powder, loading in open quartz tube, heating to 1000-1300 deg.C, holding the temp for 60-90 min, cooling, and immersing the powder in diluted nitric acid for removing catalyst. Its advantages are simple process and low cost.
Description
Technical field
The present invention relates to a kind of method for preparing boron nitride nano-tube (BN-NTs).
Background technology
Since having found carbon nanotube (C-NTs) afterwards, with the BN that has hexagonal structure equally, BC
3And BC
2The whole bag of tricks that N prepares nanotube also occurs successively.Theoretical Calculation shows that the number of plies of diameter, spirality and tube wall of the energy gap of BN-NTs and nanotube is irrelevant, this than electrical properties along with the C-NTs that the textural factors such as the number of plies of diameter, spirality and the tube wall of nanotube change has more advantage, and BN-NTs is a stable structure, thereby unique application prospect is arranged on nano-device.BN-NTs has better high-temperature oxidation resistance than C-NTs in addition, is good heat conductor and isolator.
The method of using plasma arc-over has been synthesized BN-NTs at first.Laser ablation method also success synthesized BN-NTs.But the output of these two kinds of methods, purity are not high, and cost height, and complex process are unfavorable for industrial production.Develop the synthetic method that the carbon nanotube substitution reaction recently again, wherein the carbon nanotube role provides the skeleton of BN-NTs growth, BN-NTs that obtains and the similar of C-NTs, but the BN-NTs of this method preparation inevitably is mixed with C-NTs, and this has influenced the popularization of this method.Use the chemical Vapor deposition process (CVD) of metal catalyst can synthesize BN-NTs, but former CVD method all will feed reactant gases in addition, and some the catalyzer price that adopts is very high, this has also limited its application to a certain extent.
Summary of the invention
The method that the purpose of this invention is to provide a kind of BN-NTs of preparation, its selects urea and boric acid respectively as N source and B source, introduces Fe, or Co, or Ni need not other reactant gases as catalyzer, can prepare a large amount of high-quality BN-NTs.
It comprises following step the technical solution used in the present invention: 1) with chemical pure H
3BO
3, CO (NH
2)
2And Fe (NO
3)
39H
2O or Co (NO
3)
26H
2O or Ni (NO
3)
26H
2O, its mol ratio 1: 2-5: 0.05-0.1 is dissolved in the deionized water together; 2) under 60-80 ℃ of constant temperature, in vacuum drying oven, evaporated 6-10 hour then, remove the water in the solution, obtain the blended powder; 3) mixed powder is put into quartz boat, place the silica tube central thermal zone that adopts the horizontal chamber oven heating then, the silica tube two ends communicate with atmosphere, when temperature rises to 1000-1300 ℃, and constant temperature 60-90 minute; 4) wait until that then temperature reduces to room temperature, take out quartz boat, obtain linen powder.5) again powder was soaked 8-12 hour with rare nitric acid (20-30wt%), remove catalyzer, obtain the pure BN-NTs of white.
Characteristics of the present invention: 1. by thorough mixing H in solution
3BO
3, CO (NH
2)
2And Fe (NO
3)
39H
2O or Co (NO
3)
26H
2O or Ni (NO
3)
26H
2O, remove the water in the solution after, can obtain at the mixed powder of molecular level.Contact well thus between catalyzer and the reactant, help the BN-NTs of growing high-quality.2. be reflected in the silica tube of opening and carry out, need not to feed in addition other reactant gasess.3. this method technology is simple, and cost of material is cheap, and cost is low, and reaction is easy to control.
Description of drawings
Fig. 1 is the transmission electron microscope photo (amplifying 40,000 times) of embodiment gained BN-NTs;
Fig. 2 is the high-resolution electron microscope photo (amplifying 410,000 times) of embodiment gained BN-NTs.
Embodiment
Embodiment:
Take by weighing 0.602gCO (NH respectively
2)
2, 0.618gH
3BO
3, 0.404gFe (NO
3)
39H
2O (mol ratio is 1: 3: 0.1) is dissolved in the 300ml deionized water together, and heating 6h obtains filemot mixed powder except that anhydrating in 60 ℃ of homothermic vacuum drying ovens then.Again this powder is put into quartz boat, place by horizontal chamber oven heating the silica tube central thermal zone.The silica tube both ends open communicates with atmosphere.Be warming up to 1000 ℃, be incubated 60 minutes.Concrete process is as follows: urea begins fusing and decomposites NH after temperature surpasses 133 ℃
3, at about NH more than 700 ℃
3Just can with H
3BO
3Reaction generates BN.While Fe (NO
3)
3At pyrolytic decomposition is Fe
2O
3And oxynitride.NH
3Have reductibility, Fe can be restored.Under the katalysis of Fe nanoparticle, grow BN-NTs.
Product is a pale powder, measures with X-ray diffraction to show that wherein main component is hexagonal BN, and Fe
2O
3, Fe
2O
3Be catalyzer oxidized product in reaction, can remove with rare nitric acid (30%) very easily.Product disperses the back to observe under transmission electron microscope with dehydrated alcohol.Find a large amount of BN-NTs, the diameter range of nanotube is at 30-50nm, several microns long (seeing accompanying drawing 1).The BN-NTs structure of growing as can be seen by the observation of high-resolution electron microscope is very complete, and internal diameter and external diameter are respectively 15nm and 40nm (seeing accompanying drawing 2).
Claims (1)
1. a method for preparing boron nitride nano-tube is characterized in that it comprises the steps:
1) chemical pure H
3BO
3, CO (NH
2)
2And Fe (NO
3)
39H
2O or Co (NO
3)
26H
2O, or Ni (NO
3)
26H
2O, its mol ratio 1: 2-5: 0.05-0.1 is dissolved in the deionized water together;
2) under 60-80 ℃ of constant temperature, in vacuum drying oven, evaporated 6-10 hour then, remove the water in the solution, obtain the blended powder;
3) mixed powder is put into quartz boat, place the silica tube central thermal zone that adopts the horizontal chamber oven heating then, the silica tube two ends communicate with atmosphere, when temperature rises to 1000-1300 ℃, and constant temperature 60-90 minute;
4) wait until that then temperature reduces to room temperature, take out quartz boat, obtain linen powder;
5) again with rare nitric acid dousing 8-12 hour of powder usefulness 20-30wt%, remove catalyzer, obtain the pure BN-NTs of white.
Priority Applications (1)
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---|---|---|---|
CN 03114737 CN1208245C (en) | 2003-01-03 | 2003-01-03 | Preparation of boron nitride nano tube |
Applications Claiming Priority (1)
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---|---|---|---|
CN 03114737 CN1208245C (en) | 2003-01-03 | 2003-01-03 | Preparation of boron nitride nano tube |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1424254A true CN1424254A (en) | 2003-06-18 |
CN1208245C CN1208245C (en) | 2005-06-29 |
Family
ID=4790463
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---|---|---|---|
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1302850C (en) * | 2004-12-02 | 2007-03-07 | 黄德欢 | Method for preparing supported nano gold powder by thermal decomposition and apparatus therefor |
CN100347079C (en) * | 2005-04-20 | 2007-11-07 | 中国科学院金属研究所 | Production of boron nitride nanometer tube with water as growth improver |
WO2011032231A1 (en) * | 2009-09-21 | 2011-03-24 | Deakin University | Method of manufacture |
CN101550599B (en) * | 2009-04-16 | 2011-05-11 | 山东大学 | Preparation method of boron nitride crystal whisker |
CN103058697A (en) * | 2012-12-14 | 2013-04-24 | 西北工业大学 | Method for modifying boron nitride interface phase of ceramic matrix composite material |
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 |
CN105950141A (en) * | 2016-05-13 | 2016-09-21 | 湖州师范学院 | Preparation method of nitride-boride fluorescent powder material |
CN107673318A (en) * | 2016-08-01 | 2018-02-09 | 中国科学院苏州纳米技术与纳米仿生研究所 | Boron nitride nano-tube and its batch preparation |
CN113788464A (en) * | 2021-08-20 | 2021-12-14 | 武汉工程大学 | Method for preparing boron nitride nanotube by using double transition metal oxide as catalyst |
-
2003
- 2003-01-03 CN CN 03114737 patent/CN1208245C/en not_active Expired - Fee Related
Cited By (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1302850C (en) * | 2004-12-02 | 2007-03-07 | 黄德欢 | Method for preparing supported nano gold powder by thermal decomposition and apparatus therefor |
CN100347079C (en) * | 2005-04-20 | 2007-11-07 | 中国科学院金属研究所 | Production of boron nitride nanometer tube with water as growth improver |
CN101550599B (en) * | 2009-04-16 | 2011-05-11 | 山东大学 | Preparation method of boron nitride crystal whisker |
CN102753475B (en) * | 2009-09-21 | 2016-07-13 | 迪肯大学 | Manufacture method |
WO2011032231A1 (en) * | 2009-09-21 | 2011-03-24 | Deakin University | Method of manufacture |
CN102753475A (en) * | 2009-09-21 | 2012-10-24 | 迪肯大学 | Method of manufacture |
AU2010295253B2 (en) * | 2009-09-21 | 2015-09-24 | Deakin University | Method of manufacture |
US9199854B2 (en) | 2009-09-21 | 2015-12-01 | Deakin University | Method of manufacture |
CN103058697A (en) * | 2012-12-14 | 2013-04-24 | 西北工业大学 | Method for modifying boron nitride interface phase of ceramic matrix composite material |
CN103058697B (en) * | 2012-12-14 | 2015-03-04 | 西北工业大学 | Method for modifying boron nitride interface phase of ceramic matrix composite material |
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 |
CN105036096B (en) * | 2015-07-22 | 2017-07-21 | 哈尔滨工业大学 | A kind of method that utilization reacting gas vortex prepares high-purity boron nitride nano-tube |
CN105950141A (en) * | 2016-05-13 | 2016-09-21 | 湖州师范学院 | Preparation method of nitride-boride fluorescent powder material |
CN105950141B (en) * | 2016-05-13 | 2019-01-25 | 湖州师范学院 | A kind of preparation method of nitrogen boride phosphor material powder |
CN107673318A (en) * | 2016-08-01 | 2018-02-09 | 中国科学院苏州纳米技术与纳米仿生研究所 | Boron nitride nano-tube and its batch preparation |
CN107673318B (en) * | 2016-08-01 | 2020-11-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Boron nitride nanotubes and batch preparation method thereof |
CN113788464A (en) * | 2021-08-20 | 2021-12-14 | 武汉工程大学 | Method for preparing boron nitride nanotube by using double transition metal oxide as catalyst |
CN113788464B (en) * | 2021-08-20 | 2022-12-27 | 武汉工程大学 | Method for preparing boron nitride nanotube by using double transition metal oxide as catalyst |
Also Published As
Publication number | Publication date |
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