CN102120568B - Method for preparing boron nitride nanorod by using precursor conversion method - Google Patents
Method for preparing boron nitride nanorod by using precursor conversion method Download PDFInfo
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- CN102120568B CN102120568B CN201110110490A CN201110110490A CN102120568B CN 102120568 B CN102120568 B CN 102120568B CN 201110110490 A CN201110110490 A CN 201110110490A CN 201110110490 A CN201110110490 A CN 201110110490A CN 102120568 B CN102120568 B CN 102120568B
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Abstract
The invention relates to a method for preparing a boron nitride nanorod by using a precursor conversion method. The method for preparing the boron nitride nanorod comprises the following steps of: soaking a carbon nanotube in concentrated nitric acid at 60 DEG C for 10-24h, washing and drying; dissolving poly(alkylamino) borazine in an organic solvent, and soaking the dried carbon nanotube in a mixed solution; and filtering at a reduced pressure, then carrying out solid-liquid separation, placing solid in a high temperature finance and preserving the temperature for 0.5-5h at 60-200 DEG C in ammonia gas, then heating to 800-1500 DEG C in a heating speed of 60-450DEG C/min, preserving the temperature for 0.5-5h, and removing carbon element while pyrolyzing to obtain the boron nitride nanorod. The prepared boron nitride nanorod has the diameter of 50nm, has the advantages of simple process, no need of catalyst, high purity, low production cost and high efficiency and is easy to realize large-scale production. The prepared boron nitride nanorod can be applied to materials with the functions of hydrogen storage, catalysis, structure reinforcement and high-temperature resistance and has wide application prospect.
Description
Technical field
The present invention relates to a kind of method of Stainless Steel via Precursor Pyrolysis boron nitride nanometer rod.
Background technology
Existing boron nitride nanometer preparation methods mainly contains arc discharge method, mechanical ball milling method, inorganics reaction method, template and method of electrostatic spinning etc.The output of arc process is very low, and the product form is various.Mechanical ball milling method required time is long, needs usually more than the 100h, in mechanical milling process, can introduce a large amount of impurity, and product structure is unordered simultaneously, and the diameter of product is also wayward.The boron nitride nanometer material of inorganicization reaction method preparation often will use a large amount of catalyzer, and output and purity are all very low and contain a lot of impurity, are unfavorable for the application of product in matrix material.Template and method of electrostatic spinning prepare boron nitride nanometer material (nanofiber, nanotube, nanometer rod), have product purity height, the uniform characteristics of diameter, employing such as Beachelany template (referring to
J. Phys. Chem. C, 111,13378 (2007)) and prepared the about 200nm of diameter, the BN nanotube that is evenly distributed.Employing such as Miele polymeric preceramic body combination method of electrostatic spinning (referring to
Nano scale, 2,215 (2010)) and prepared BN nanofiber, diameter 200-500nm.Qiu etc. are immersed in B with carbon nano fiber respectively
2O
3In the ethanolic soln (referring to
Nanotechnology, 20,345603 (2009)) and the about 50-250nm of boron nitride nanometer Fibre diameter that makes, adopt static to spin B
2O
3And polyvinyl butyral acetal (PVB) (referring to
J. Phys. Chem. C, 113,11228 (2009)) preparation the about 80-350nm of BN nanofiber diameter.Static such as Hwang spin nanometer BN/ Z 150PH, the about 200-500nm of boron nitride nanometer Fibre diameter that makes (referring to Macromol Res, 18,551 (2010)).But the research of the boron nitride nanometer rod of diameter (< 50nm) at present is report not also both at home and abroad.
Summary of the invention
The object of the present invention is to provide a kind of method of Stainless Steel via Precursor Pyrolysis boron nitride nanometer rod.With the boron nitride nanometer rod diameter of realizing preparation (< 50nm); Another order of the present invention is to realize that the operation steps of preparation boron nitride nanometer rod is simpler, need not to use catalyzer, high, good, the easy realization of large-scale production of controllability of product purity.
The present invention includes following steps:
(1) carbon nanotube is soaked 10-24h in 60 ℃ concentrated nitric acid, the washing after drying;
(2) will gather the alkylamino radical borazine and be dissolved in the organic solvent, what be made into mass percentage concentration and be 20-60% gathers alkylamino radical borazine solution, with dried carbon nanotube vacuum impregnation 4-16h in this mixing solutions, decompress filter, solid-liquid separation;
(3) solid is put into vacuum drying oven in 50-100 ℃ of dry 0.5-5h; Organic solvent after the solid-liquid separation is recycled;
(4) cooled solid is put into High Temperature Furnaces Heating Apparatus, in dry ammonia, handle 0.5-5h in 60-150 ℃ of insulation;
(5) temperature rise rate by 60-450 ℃/h rises to 800-1500 ℃, and insulation 0.5-5h makes the cracking of alkylamino radical borazine remove carbon simultaneously, promptly makes the boron nitride nanometer rod of diameter 30-50nm.
In said (1) step, carbon nanotube soaks 12-20h in 60 ℃ concentrated nitric acid.
The softening temperature that gathers the alkylamino radical borazine in said (2) step is 80-130 ℃.
The organic solvent in said (2) step is YLENE, toluene or N.
In said (4) step, the insulation treatment temp is 80-130 ℃, and the time is 1-4h.
The temperature rise rate in said (5) step is 80-400 ℃/h, and the insulation treatment temp is 1000-1400 ℃, and the time is 1-4h.
The present invention adopts the boron nitride nanometer rod of Stainless Steel via Precursor Pyrolysis, prepares nanofiber (rod) relatively with existing method, the boron nitride nanometer of preparation rod diameter < 50nm; And technology is simple, does not need catalyzer, and degree of purity of production is high, and production cost is lower, and efficient is high; Easy realization of large-scale production.The BN nanometer rod of preparation can be used as Chu Qing, catalysis, structure enhancing and high temperature resistant functional materials, has broad application prospects.
Description of drawings
The full spectrogram of x-ray photoelectron power spectrum of the BN nanometer rod that Fig. 1 makes for embodiment 1;
The match spectrogram of the x-ray photoelectron power spectrum B of the BN nanometer rod that Fig. 2 makes for embodiment 1;
The match spectrogram of the x-ray photoelectron power spectrum N of the BN nanometer rod that Fig. 3 makes for embodiment 1;
The transmission electron microscope photo of the BN nanometer rod that Fig. 4 makes for embodiment 1.
Description of drawings
The field emission scanning electron microscope photo of the BN nano wire that Fig. 1 obtains for embodiment 1;
The infrared spectrogram of the BN nano wire that Fig. 2 obtains for embodiment 1.
Embodiment
Below in conjunction with embodiment the present invention is described further.But must not be the restriction to protection domain of the present invention with said instance interpretation, the method for equivalence be all within protection scope of the present invention therewith.
Embodiment 1:
(1) carbon nanotube is soaked 10h in 60 ℃ concentrated nitric acid, the washing after drying;
(2) will gather the alkylamino radical borazine and be dissolved in the YLENE, the preparation mass percent concentration is 30% solution.With vacuum impregnation technology with dried carbon nanotube 15h in immersing this mixing solutions, decompress filter solid-liquid separation;
(4) solid that step (2) is obtained is put into vacuum drying oven in 100 ℃ of dry 3h;
(5) cooled solid is put into High Temperature Furnaces Heating Apparatus and handle 1h in 80 ℃ of insulations at dry ammonia;
(6) temperature rise rate by 300 ℃/h rises to 1000 ℃, and insulation 3h makes the cracking of alkylamino radical borazine remove carbon simultaneously, promptly makes the BN nanometer rod, diameter 30-50 nm.
Embodiment 2:
(1) carbon nanotube is soaked 15h in 60 ℃ concentrated nitric acid, the washing after drying;
(2) will gather the alkylamino radical borazine and be dissolved in the organic solvent toluene, the preparation mass percent concentration does
Material, electromagnetic wave transparent material etc. have broad application prospects.
Embodiment
Below in conjunction with embodiment the present invention is described further.But must not be the restriction to protection domain of the present invention with said instance interpretation, the method for equivalence be all within protection scope of the present invention therewith.
Embodiment 1:
(1) according to prior art synthetic have a following structural formula gather alkylamino radical borazine precursor: (synthetic referring to
Chinese Chem. Lett., 21,1079 (2010), its softening temperature is about 75 ℃,
(2) will gather in the glove box of alkylamino radical borazine precursor under the Ar gas shiled and grind, 1000 orders sieve; Precursor powder after sieving is put in the graphite boat, and in tube furnace, the temperature rise rate according to 4 ℃/min under the high pure nitrogen atmosphere is warming up to 150 ℃, and nitrogen flow is 60ml/min, insulation 1h; Temperature rise rate according to 5 ℃/min is heated to 600 ℃ again, insulation 2h; According to the temperature rise rate of 5 ℃/min, control nitrogen flow 50ml/min is heated to 1300 ℃ again, and insulation 2h obtains the BN nano wire.
The SEM photo of its BN nano wire is as depicted in figs. 1 and 2.Its diameter is more even, about 12 ~ 18nm.
Embodiment 2:
(1) the synthetic alkylamino radical borazine precursor of gathering, (synthetic referring to
Chinese Chem. Lett., 21,1079 (2010)), its softening temperature is about 83 ℃;
(2) will gather in the glove box of alkylamino radical borazine precursor under the Ar gas shiled and grind, 1000 orders sieve; Precursor powder after sieving is put in the graphite boat, and in tube furnace, the temperature rise rate according to 4 ℃/min under the high pure nitrogen atmosphere is warming up to 150 ℃, and nitrogen flow is 60ml/min, insulation 1h; Temperature rise rate according to 5 ℃/min is heated to 700 ℃ again, insulation 1h; According to the temperature rise rate of 10 ℃/min, control nitrogen flow 70ml/min is heated to 1600 ℃ again, and insulation 2h obtains the BN nano wire, diameter 12 ~ 18nm.
40% solution.With dried carbon nanotube vacuum impregnation 20h in this mixing solutions, decompress filter solid-liquid separation;
(4) solid that step (2) is obtained is put into vacuum drying oven in 100 ℃ of dry 5h;
(5) cooled solid is put into High Temperature Furnaces Heating Apparatus and handle 1h in 90 ℃ of insulations at dry ammonia;
(6) temperature rise rate by 200 ℃/h rises to 1000 ℃, and insulation 3h makes the cracking of alkylamino radical borazine remove carbon simultaneously, promptly makes the BN nanometer rod, diameter 30-50nm.
Embodiment 3:
(1) carbon nanotube is soaked 15h in 60 ℃ concentrated nitric acid, the washing after drying;
(2) will gather the alkylamino radical borazine and be dissolved in the organic solvent N, the preparation mass percent concentration is 40% solution.With dried carbon nanotube vacuum impregnation 24h in this mixing solutions, decompress filter solid-liquid separation;
(4) solid that step (2) is obtained is put into vacuum drying oven in 120 ℃ of dry 2h;
(5) cooled solid is put into High Temperature Furnaces Heating Apparatus and handle 2h in 100 ℃ of insulations at dry ammonia;
(6) temperature rise rate by 400 ℃/h rises to 1200 ℃, and insulation 4h makes the cracking of alkylamino radical borazine remove carbon simultaneously, promptly makes the BN nanometer rod, diameter 30-50nm.
Claims (6)
1. the method for a Stainless Steel via Precursor Pyrolysis boron nitride nanometer rod is characterized in that, may further comprise the steps:
(1) carbon nanotube is soaked 10-24h in 60 ℃ concentrated nitric acid, the washing after drying;
(2) will gather the alkylamino radical borazine and be dissolved in the organic solvent, what be made into mass percentage concentration and be 20-60% gathers alkylamino radical borazine solution, with dried carbon nanotube vacuum impregnation 4-16h in this mixing solutions, decompress filter, solid-liquid separation;
(3) solid is put into vacuum drying oven in 50-100 ℃ of dry 0.5-5h; Organic solvent after the solid-liquid separation is recycled;
(4) cooled solid is put into High Temperature Furnaces Heating Apparatus, in dry ammonia, handle 0.5-5h in 60-150 ℃ of insulation;
(5) temperature rise rate by 60-450 ℃/h rises to 800-1500 ℃, and insulation 0.5-5h makes and gathers the cracking of alkylamino radical borazine and remove carbon simultaneously, promptly makes the boron nitride nanometer rod of diameter 30-50nm.
2. the preparation method of boron nitride nanometer rod according to claim 1 is characterized in that, in said (1) step, carbon nanotube soaks 12-20h in 60 ℃ concentrated nitric acid.
3. the preparation method of boron nitride nanometer rod according to claim 1 and 2 is characterized in that the softening temperature that gathers the alkylamino radical borazine in said (2) step is 80-130 ℃.
4. the preparation method of boron nitride nanometer rod according to claim 1 and 2 is characterized in that the organic solvent in said (2) step is YLENE, toluene or N.
5. the preparation method of boron nitride nanometer rod according to claim 1 and 2 is characterized in that, in said (4) step, the insulation treatment temp is 80-130 ℃, and the time is 1-4h.
6. the preparation method of boron nitride nanometer rod according to claim 1 and 2 is characterized in that the temperature rise rate in said (5) step is 80-400 ℃/h, and the insulation treatment temp is 1000-1400 ℃, and the time is 1-4h.
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| CN103451852B (en) * | 2013-08-31 | 2015-09-23 | 中国人民解放军国防科学技术大学 | A kind of TiO 2the preparation method of nanometer rods/SiC composite fibrofelt |
| CN109706550B (en) * | 2019-01-14 | 2021-03-23 | 中原工学院 | Method for preparing hexagonal boron nitride by using carbon nanofibers as template |
| CN110773109A (en) * | 2019-11-01 | 2020-02-11 | 成都理工大学 | Preparation method of boron nitride nanoflower |
| CN114558602B (en) * | 2022-01-26 | 2023-08-01 | 天津大学 | Copper-loaded porous boron nitride nanorod catalyst and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1227531A (en) * | 1996-08-06 | 1999-09-01 | 大塚化学株式会社 | Boron nitride and process for preparing the same |
| CN1238304A (en) * | 1998-05-14 | 1999-12-15 | 中国科学院金属研究所 | Process for preparing nm-class boron nitride tube |
| US6709471B2 (en) * | 2000-07-11 | 2004-03-23 | Nec Corporation | Single layer carbon nanotube electrode battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1227531A (en) * | 1996-08-06 | 1999-09-01 | 大塚化学株式会社 | Boron nitride and process for preparing the same |
| CN1238304A (en) * | 1998-05-14 | 1999-12-15 | 中国科学院金属研究所 | Process for preparing nm-class boron nitride tube |
| US6709471B2 (en) * | 2000-07-11 | 2004-03-23 | Nec Corporation | Single layer carbon nanotube electrode battery |
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