CN107673318A - Boron nitride nano-tube and its batch preparation - Google Patents
Boron nitride nano-tube and its batch preparation Download PDFInfo
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- CN107673318A CN107673318A CN201610619062.XA CN201610619062A CN107673318A CN 107673318 A CN107673318 A CN 107673318A CN 201610619062 A CN201610619062 A CN 201610619062A CN 107673318 A CN107673318 A CN 107673318A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- 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
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of boron nitride nano-tube and its batch preparation.The preparation method includes：Predecessor is formed by boron source supported catalyst of borate, the catalyst includes transistion metal compound；The predecessor is heated to 1200~1400 DEG C, and the insulation reaction in ammonia atmosphere in nitrogen containing atmosphere, is down to room temperature in protective atmosphere afterwards, obtains crude product；And the crude product is post-processed, the boron nitride nano-tube is made.Boron nitride nanometer tube preparation method provided by the invention has the characteristics that low cost, technique is simple, yield is high, and it is easy to amplify, realize a large amount of productions, it is 10~150nm to obtain boron nitride nano-tube caliber simultaneously, pipe range has broad prospect of application up to 20~100 microns, in fields such as composite, Heat Conduction Materials.
Description
Technical field
Present invention relates particularly to a kind of batch preparation of boron nitride nano-tube, belongs to inorganic nano material technology neck
Domain.
Background technology
For boron nitride nano-tube (BNNT) as a kind of new nano material, it not only has class with CNT (CNT)
As crystal structure, but also have the mechanical property to be compared favourably with CNT and heat-conductive characteristic.In addition, boron nitride nanometer
Pipe also has excellent inoxidizability, chemical stability and good insulating properties.These unique performances make BNNT partly be led in nanometer
The fields such as body device, hydrogen storage material, insulating materials and anti-oxidant clad have a wide range of applications.
Currently used boron nitride nano-tube synthetic method has arc discharge method, laser ablation method, mechanical attrition method, CVD
Method thermal decomposition method etc..In recent years, with the further investigation of boron nitride nano-tube, very big success is obtained in preparation method and is entered
Exhibition.But these existing preparation technology generally existings prepare cost height or apparatus and process is complicated, and the raw material used has certain
Toxicity and the shortcomings of not high boron nitride nano-tube yield.
The content of the invention
It is a primary object of the present invention to provide a kind of boron nitride nano-tube and its batch preparation, to overcome existing skill
Deficiency in art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
A kind of batch preparation of boron nitride nano-tube is provided in the embodiment of the present invention, it includes：
Predecessor is formed by boron source supported catalyst of borate, the catalyst includes transistion metal compound；
The predecessor is heated to 1200~1400 DEG C, and the insulation reaction in ammonia atmosphere in nitrogen containing atmosphere, it
Room temperature is down in protective atmosphere afterwards, obtains crude product,
The crude product is post-processed, the boron nitride nano-tube is made.
Further, the caliber of the boron nitride nano-tube is 10~150nm, and pipe range is 20~100 microns.
Compared with prior art, boron nitride nanometer tube preparation method provided by the invention is using borate cheap and easy to get as boron
Source, by the design of catalyst, boron nitride nano-tube is directly obtained on presoma (i.e. boron source) surface, it is not necessary to which other substrates are made
For the collection carrier of boron nitride nano-tube, technique is simple, and condition is easily-controllable, and cost is cheap, can be mass, boron nitride nano-tube production
Rate is high, and obtained boron nitride nano-tube has broad prospect of application in fields such as composite, Heat Conduction Materials.
Brief description of the drawings
Fig. 1 a-1b are the SEM figures of obtained boron nitride nano-tube in the embodiment of the present invention 1；
Fig. 2 is the TEM figures of obtained boron nitride nano-tube in the embodiment of the present invention 1；
Fig. 3 is SEAD (SAED) figure of single boron nitride nano-tube in Fig. 2；
Fig. 4 is the Raman spectrograms of obtained boron nitride nano-tube in the embodiment of the present invention 1.
Embodiment
In view of deficiency of the prior art, inventor is able to propose the present invention's through studying for a long period of time and largely putting into practice
Technical scheme, it mainly uses borate as boron source, by a variety of mode of loadings, by transition metal salt or its oxide or hydrogen
The catalyst such as oxide are carried on borate surface, then insert in chemical vapor depsotition equipment, are heated simultaneously in nitrogen containing atmosphere
Insulation reaction, then post-treated obtain boron nitride nano-tube.The technical scheme, its implementation process and principle etc. will be made as follows into
The explanation of one step.
The one side of the embodiment of the present invention provides a kind of batch preparation of boron nitride nano-tube, and it includes：
Predecessor is formed by boron source supported catalyst of borate, the catalyst includes transistion metal compound；
The predecessor is heated to 1200~1400 DEG C, and the insulation reaction in ammonia atmosphere in nitrogen containing atmosphere, it
Room temperature is down in protective atmosphere afterwards, obtains crude product,
The crude product is post-processed, the boron nitride nano-tube is made.
In some embodiments, the preparation method includes：At least from any one side in ball-milling method, infusion process
Formula makes the boron source supported catalyst.
In some more preferred embodiment, the preparation method includes：The catalyst and boron source are mixed simultaneously
Ball milling is carried out, ball milling speed is 200~300r/min, and the time is 100~150h, obtains the predecessor.
Further, borate powder can be mixed with transistion metal compound and is placed in ball milling 100 in planetary ball mill
~150h, 200~300r/min of rotating speed.
In some more preferred embodiment, the preparation method includes：By the catalyst and boron source in solvent
Middle ultrasonic mixing, processing is dried afterwards, obtains the predecessor, the solvent includes ethanol.
Further, can be by borate powder and ethanol solution 5~10h of ultrasonic mixing of transistion metal compound, so
After dry.
Further, the borate includes MgB4O7、Mg2B2O5、Mg3B2O6、CaB4O7And Li2B4O7In any one
Or two or more combinations, preferably MgB4O7, but not limited to this.
Further, the transistion metal compound includes transition metal salt or transition metal oxide.
For example, the transition metal salt includes Fe (NO3)3、Co(NO3)2With Ni (NO3)3In any one or two kinds with
On combination.For example, the transition metal oxide includes Fe2O3It is but unlimited with any one in CoO or two kinds of combination
In this.
Further, the transistion metal compound is preferably Fe (NO3)3。
It is more preferable, the mol ratio of boron element and the transition metal contained by the catalyst contained by the boron source
For 1:0.01~0.1.
Further, the nitrogen containing atmosphere includes ammonia atmosphere or nitrogen/hydrogen mixed gas atmosphere.
Further, the protective atmosphere includes hydrogen, nitrogen or inert atmosphere (such as Ar atmosphere), naturally it is also possible to is
Wherein two or the mixed atmosphere of three.
In some more preferred embodiment, the preparation method includes：By the predecessor in nitrogen containing atmosphere
1200~1400 DEG C are heated to 5~15 DEG C/min heating rate, afterwards the insulation reaction in ammonia atmosphere.
In some embodiments, the preparation method includes：The post processing includes：Obtained crude product is carried out successively
Pickling, drying process, the boron nitride nano-tube is made.
In some more specific embodiment, the preparation method includes：Urged by boron source carried metal of borate
Mixture, is then put into chemical vapor depsotition equipment by agent or transistion metal compound, and in ammonia or nitrogen and hydrogen
5~15 DEG C/min heating rate is heated to 1200~1400 DEG C in gas mixed atmosphere, afterwards the insulation reaction in ammonia atmosphere
0.5~5h, insulation are cooled to room temperature in nitrogen or argon gas atmosphere after terminating, white crude are obtained, by crude product through peracid
Wash, dry the acquisition boron nitride nano-tube.
In one more specifically case study on implementation, the preparation method comprises the following steps：
(1) by MgB4O7The upper catalyst of powder load (such as Fe (NO3)3) after, it is (such as high to be placed in high-temperature region reaction crucible
Warm area aluminium oxide boat) in, then insert chemical vapor depsotition equipment (such as tube furnace)；
(2) in ammonia or nitrogen and hydrogen mixed gas atmosphere, then temperature programming is incubated 0.5 to 1100~1400 DEG C
~5h, obtain the boron nitride nano-tube.
Wherein, MgB4O7With Fe (NO3)3Mol ratio be preferably 1：0.01~1：0.1.
The embodiment of the present invention another aspect provides the boron nitride nano-tube prepared by methods described, its caliber is 10
~150nm, pipe range are 20~100 microns.
The growth mechanism of boron nitride nano-tube may be in the present invention：Boron source comes from the antifungin of solid-state.In ammonia gas
In atmosphere, boron element separates out from antifungin lattice, is dissolved in the catalyst granules for being attached to surface, is decomposed simultaneously from ammonia
Nitrogen also is soluble in catalyst granules.When two kinds of elements reach supersaturation, boron nitrogen separates out and forms nitridation in certain proportion
Boron nanotube, and it is grown on antifungin particle surface (see shown in Fig. 2) by site of catalyst.
Boron nitride nanometer tube preparation method provided by the invention has low cost, technique is simple, yield is high, product crystallinity
The features such as good, and be easy to amplify, a large amount of productions are realized, while obtained boron nitride nano-tube is led in composite, Heat Conduction Material etc.
Domain has broad prospect of application.
Below in conjunction with accompanying drawing and some embodiments the technical solution of the present invention is further explained explanation.
Embodiment 1：Weigh 0.0404gFe (NO3)3.9H2O and 1.8gMgB4O7Powder is dissolved in ultrasonic 2h in 5ml absolute ethyl alcohols
Dried afterwards under the conditions of 60 DEG C, obtain faint yellow antifungin powder, antifungin powder is put into aluminium oxide boat be placed in afterwards
In CVD stoves, the air in furnace chamber is excluded with Ar, then be passed through 200sccm NH3, temperature programming is to 1300 DEG C and is incubated 180min,
Reaction closes ammonia after terminating, and room temperature is cooled in argon gas atmosphere, and white crude is made.It is obtained to refer to Fig. 1 a-1b
Crude product in boron nitride nano-tube SEM figures, show to have substantial amounts of boron nitride nano-tube to generate, and boron nitride nano-tube is given birth to
It is longer than boric acid magnesium surface.Foregoing crude product is by the chlorohydric acid pickling that concentration is 1mol/L~5mol/L, ultrasound 10~12, after filtering
Cleaned for several times with deionized water again, then 60 DEG C of dry 12h, you can to obtain pure boron nitride.Refer to Fig. 2 and Fig. 3 points
Not Wei obtained boron nitride nano-tube TEM figures and SEAD (SAED) figure, show that boron nitride nano-tube has good knot
Crystalline substance.
Embodiment 2：Weigh MgB4O7Powder, Fe (NO3)3With mol ratio 1:0.1 mixing, is placed in planetary ball mill afterwards
200~300r/min of setting speed and ball milling 150h, further take out mixture 1g and are put into aluminium oxide boat and be placed in CVD stoves, use Ar
The air in furnace chamber is excluded, is passed through 100 standard milliliters/minute (sccm) N2With 100sccm H2, temperature programming is to 1300 DEG C.
It is then shut off N2And H2, nitrogen 200sccm is passed through, is incubated 180min, reaction terminates to close ammonia, cooled in argon gas atmosphere
Room temperature.Sample is taken out, obtains white crude, it is boron nitride nano-tube to characterize it.
Embodiment 3：Weigh 0.0404gFe (NO3)3.9H2O and 1.8gMgB4O7Powder is dissolved in ultrasonic 2h in 5ml absolute ethyl alcohols
Dried afterwards under the conditions of 60 DEG C, obtain faint yellow antifungin powder, antifungin powder is put into aluminium oxide boat be placed in afterwards
In CVD stoves, the air in furnace chamber is excluded with Ar, then be passed through 100 standard milliliters/minute (sccm) N2With 100sccm's
H2, temperature programming is to 1300 DEG C and is incubated 180min, and reaction closes N after terminating2And H2, room temperature is cooled in argon gas atmosphere, is made
Obtain white crude boron nitride nano-tube.
Embodiment 4：Weigh 0.0404gFe (NO3)3.9H2O and 1.8gMgB4O7Powder is dissolved in ultrasonic 2h in 5ml absolute ethyl alcohols
Dried afterwards under the conditions of 60 DEG C, obtain faint yellow antifungin powder, antifungin powder is put into aluminium oxide boat be placed in afterwards
In CVD stoves, the air in furnace chamber is excluded with Ar, then be passed through 200sccm NH3, temperature programming is to 1200 DEG C and is incubated 180min,
Reaction closes ammonia after terminating, and room temperature is cooled in argon gas atmosphere, and white crude boron nitride nano-tube is made.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this
The personage of item technology can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all
The equivalent change or modification made according to spirit of the invention, it should all be included within the scope of the present invention.
Claims (12)
- A kind of 1. batch preparation of boron nitride nano-tube, it is characterised in that including：Predecessor is formed by boron source supported catalyst of borate, the catalyst includes transistion metal compound；The predecessor is heated to 1200~1400 DEG C, and the insulation reaction in ammonia atmosphere, Zhi Hou in nitrogen containing atmosphere Room temperature is down in protective atmosphere, obtains crude product,The crude product is post-processed, the boron nitride nano-tube is made.
- 2. the batch preparation of boron nitride nano-tube according to claim 1, it is characterised in that including：At least select ball Any one mode in mill method, infusion process makes the boron source supported catalyst.
- 3. the batch preparation of boron nitride nano-tube according to claim 2, it is characterised in that including：By the catalysis Agent and boron source mix and carry out ball milling, and ball milling speed is 200~300r/min, and the time is 100~150h, obtains the forerunner Thing.
- 4. the batch preparation of boron nitride nano-tube according to claim 2, it is characterised in that including：By the catalysis Agent and the boron source ultrasonic mixing in solvent, are dried processing afterwards, obtain the predecessor, and the solvent includes ethanol.
- 5. the batch preparation of the boron nitride nano-tube according to any one of claim 1-4, it is characterised in that：It is described The mol ratio of boron element contained by boron source and the transition metal contained by the catalyst is 1:0.01~0.1.
- 6. the batch preparation of boron nitride nano-tube according to claim 1, it is characterised in that：The borate includes MgB4O7、Mg2B2O5、Mg3B2O6、CaB4O7And Li2B4O7In any one or two or more combinations.
- 7. the batch preparation of boron nitride nano-tube according to claim 1, it is characterised in that：The transition metal Compound includes transition metal salt or transition metal oxide.
- 8. the batch preparation of boron nitride nano-tube according to claim 7, it is characterised in that：The transition metal salt Including Fe (NO3)3、Co(NO3)2With Ni (NO3)3In any one or two or more combinations；And/or the transition metal Oxide includes Fe2O3With any one in CoO or two kinds of combination.
- 9. the batch preparation of boron nitride nano-tube according to claim 1, it is characterised in that：The nitrogen containing atmosphere bag Include ammonia atmosphere or nitrogen/hydrogen mixed gas atmosphere；And/or the protective atmosphere is included in hydrogen, nitrogen, inert atmosphere Combination more than either or both.
- 10. the batch preparation of boron nitride nano-tube according to claim 1, it is characterised in that including：Before described Drive thing and be heated to 1200~1400 DEG C in nitrogen containing atmosphere with 5~15 DEG C/min heating rate, protected afterwards in ammonia atmosphere Temperature reaction.
- 11. the batch preparation of boron nitride nano-tube according to claim 1, it is characterised in that the post processing bag Include：Pickling, drying process are carried out successively to obtained crude product, the boron nitride nano-tube is made.
- 12. boron nitride nano-tube prepared by the method as any one of claim 1-11, its caliber is 10~150nm, pipe A length of 20~100 microns.
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Cited By (5)
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| CN111204720A (en) * | 2020-02-10 | 2020-05-29 | 浙江硼矩新材料科技有限公司 | Batch preparation method of boron nitride nanotubes |
| CN112320770A (en) * | 2020-08-19 | 2021-02-05 | 耐尔泰科株式会社 | Preparation method and device of nano material |
| 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 |
| CN114852976A (en) * | 2022-06-09 | 2022-08-05 | 桂林理工大学 | Hollow boron nitride short rod 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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| 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 |
| 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 |
| CN114852976A (en) * | 2022-06-09 | 2022-08-05 | 桂林理工大学 | Hollow boron nitride short rod and preparation method thereof |
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Effective date of registration: 20201204 Address after: No. 6-2, No. 2 and No. 3, Huayuan Ginza, hi tech Zone, Ningbo City, Zhejiang Province, 315000 Patentee after: Ningbo haiwozi Environmental Protection Technology Co.,Ltd. Address before: 215123, Suzhou, Jiangsu province Suzhou Industrial Park alone villa lake high Parish, if the waterway 398 Patentee before: SUZHOU INSTITUTE OF NANO-TECH AND NANO-BIONICS (SINANO), CHINESE ACADEMY OF SCIENCES |
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