CN107055491A - A kind of method that utilization urea assisting ultrasonic prepares hexagonal boron nitride nanosheet - Google Patents
A kind of method that utilization urea assisting ultrasonic prepares hexagonal boron nitride nanosheet Download PDFInfo
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- CN107055491A CN107055491A CN201710295863.XA CN201710295863A CN107055491A CN 107055491 A CN107055491 A CN 107055491A CN 201710295863 A CN201710295863 A CN 201710295863A CN 107055491 A CN107055491 A CN 107055491A
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- boron nitride
- urea
- hexagonal boron
- nitride nanosheet
- assisting ultrasonic
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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
- 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
- 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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
The invention discloses a kind of method that utilization urea assisting ultrasonic prepares hexagonal boron nitride nanosheet, Step 1: pressing hexagonal boron nitride powder and water according to 1g:50 200ml ratio is mixed and stirred for, then by the mass ratio 20 100 of urea and hexagonal boron nitride powder:1 ratio adds urea, continues to stir, mixture is made;Step 2: mixture made from step one is placed in ice bath, ultrasonically treated 2 10 hours, dispersion liquid is obtained;Step 3: dispersion liquid made from step 2 is centrifuged, then take supernatant liquor to be filtered, the product being filtrated to get is cleaned with deionized water, product obtains boron nitride nanosheet after drying.The present invention uses water as solvent and instead of organic solvent, and additive is urea, easy to operate, and cost is relatively low, environmentally safe, and yield is higher, is advantageously implemented large-scale production.
Description
Technical field
The present invention relates to a kind of method for preparing boron nitride nanosheet, and in particular to one kind is prepared using urea assisting ultrasonic
The method of hexagonal boron nitride nanosheet.
Background technology
It is the focus studied now because the nano material of layer structure has novel performance.As a kind of important
Two-dimension nano materials, hexagonal boron nitride nanosheet (BNNS, also known as white graphite alkene), a kind of graphene analog, with a variety of excellent
Different in nature energy, such as high intrinsic thermal conductivity, excellent chemical stability and heat endurance, electrical insulation properties.After being found, it one
It is directly one of two-dimentional non-carbon nanomaterial for most being furtherd investigate, and in many fields such as nano composite material, medium
Substrate, sensor, catalyst, hyperpyrexia inoxidzable coating are widely used.Up to the present, preparing BNNS method has
The ultrasonic stripping method of mechanical stripping method, liquid phase, chemical synthesis, chemical vapour deposition technique etc..But, there are many offices in the above method
It is sex-limited so that BNNS extensive preparation and application is restricted.Such as mechanical stripping method can introduce defect, liquid to nanometer sheet
Mutually ultrasonic stripping method often uses organic solvent, and the difficult environmental pollution of post processing is larger, and chemical vapour deposition technique is generally required
Costly and complicated equipment, and toxic gas such as ammonia can be used.Therefore need badly it is a kind of without using organic solvent, cost compared with
It is low, easy to operate, environmentally safe, the high method for preparing boron nitride nanosheet of yield.
The content of the invention
Based on above the deficiencies in the prior art, technical problem solved by the invention is to provide one kind using urea auxiliary
The method that ultrasound prepares hexagonal boron nitride nanosheet, this method is without using organic solvent, and cost is relatively low, easy to operate, to environment
Pollution-free, yield is higher.
In order to solve the above-mentioned technical problem, the present invention provides one kind and prepares hexagonal nanometer boron nitride using urea assisting ultrasonic
The method of piece, is comprised the following steps:
Step 1: pressing hexagonal boron nitride powder and water according to 1g:50-200ml ratio is mixed and stirred for, then by urine
The mass ratio 20-100 of element and hexagonal boron nitride powder:1 ratio adds urea, continues to stir, mixture is made;
Step 2: mixture made from step one is placed in ice bath, it is ultrasonically treated 2-10 hours, obtain dispersion liquid;
Step 3: dispersion liquid made from step 2 is centrifuged, then supernatant liquor is taken to be filtered, the production to being filtrated to get
Product are cleaned with deionized water, and product obtains boron nitride nanosheet after drying.
As the preferred embodiment of above-mentioned technical proposal, prepared by utilization urea assisting ultrasonic provided in an embodiment of the present invention
The method of hexagonal boron nitride nanosheet further comprises the part or all of of following technical characteristic:
As the improvement of above-mentioned technical proposal, in one embodiment of the invention, in the step one, hexagonal boron nitride
Powder is with water according to 1g:100ml ratio mixing.
As the improvement of above-mentioned technical proposal, in one embodiment of the invention, in the step 2, at ice-bath ultrasonic
The power of reason is 200w.
As the improvement of above-mentioned technical proposal, in one embodiment of the invention, in the step 3, centrifugal condition is
Rotating speed is that 3000rpm centrifuges 30min.
As the improvement of above-mentioned technical proposal, in one embodiment of the invention, in the step 3, deionized water is clear
Wash 2-3 times.
As the improvement of above-mentioned technical proposal, in one embodiment of the invention, in the step 3, drying condition is
8h is handled at a temperature of 60 DEG C.
The mechanism that the present invention peels off boron nitride is as follows:The energy that liquid phase ultrasonic method is distributed by ultrasonic wave, utilizes fluid force
Learn, Surface Physical Chemistry property is destroyed the Van der Waals force of boron nitride, so as to be stripped between layers.At the same time, surpass
The energy that sound wave is produced can promote the urea being dissolved in water to hydrolyze, and the amino and few layer boron nitride for hydrolyzing generation pass through
Chemical bond produces bonding.As a result amino can be exactly made to be connected to defect and the edge of hexagonal boron nitride, and amino can also hinder
The only reunion of boron nitride nanosheet, so as to make boron nitride stable dispersion in aqueous, so as to improve charge stripping efficiency.
Compared with prior art, technical scheme has the advantages that:
(1) present invention is using urea, water as raw material, and cheap, simple to operate, stripping means is not directed to use with to ring
There are the toxic organic solvents or corrosive chemical of harm, such as 1-METHYLPYRROLIDONE and tetrahydrofuran in border and human body
Deng environmentally safe.
(2) present invention operation processing is simple, and production efficiency is high.The yield of boron nitride nanosheet has certain compared with organic solvent
Improve, 8% can at most be reached by disposably preparing the yield of boron nitride nanosheet, be suitable for producing boron nitride nanometer in enormous quantities
Piece.The present invention largely shortens the ultrasonically treated time, and do not rely on highly when obtaining final products in addition
Separation process, thus operation is more convenient, reduces labour.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the above and other objects, features and advantages of the present invention can
Become apparent, below in conjunction with preferred embodiment, describe in detail as follows.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will simply be situated between to the accompanying drawing of embodiment below
Continue.
Fig. 1 is the profile scanning electron microscope of boron nitride nanosheet prepared by the embodiment of the present invention 1;
Fig. 2 is the low power transmission electron microscope picture of boron nitride nanosheet prepared by the embodiment of the present invention 1;
Fig. 3 is the high power transmission electron microscope picture of boron nitride nanosheet prepared by the embodiment of the present invention 1;
Fig. 4 is the atomic force microscopy diagram and its thickness size of boron nitride nanosheet prepared by the embodiment of the present invention 1.
Embodiment
The following detailed description of the present invention embodiment, its as part of this specification, by embodiment come
Illustrate the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Embodiment 1
(1) in the ratio of 1g hexagonal boron nitride powders and 100ml water, hexagonal boron nitride and water are mixed, Ran Houzai
Add the urea 60g (mass ratioes 60 with hexagonal boron nitride powder:1), continue to stir, mixture is made.
(2) mixture is placed in ice bath under the conditions of power is 200w (500w × 40%), ultrasonically treated 8 hours.
(3) finally, it is that 3000rpm centrifuges 30min with rotating speed by obtained dispersion liquid, removes unstripped boron nitride powder
End.Take supernatant liquor to be filtered, the product being filtrated to get is cleaned 2-3 times with deionized water, product is in 60 DEG C of drying process
After 8h, that is, obtain boron nitride nanosheet.
Fig. 1 is the profile scanning electron microscope of boron nitride nanosheet prepared by the embodiment of the present invention 1, and nitrogen is observed under Electronic Speculum
Change boron nanometer sheet to accumulate in irregular sheet form, and it is nearly transparent.Compared with original boron nitride powder, lamella size and thickness
Degree has reduced.Fig. 2 is the low power transmission electron microscope picture of boron nitride nanosheet prepared by the embodiment of the present invention 1, can be with from figure
Find out that the lamella of boron nitride is very thin, in order to keep stable, the edge of lamella there occurs fold and curling, this form with graphene
It is consistent.Fig. 3 is the high power transmission electron microscope picture of boron nitride nanosheet prepared by the embodiment of the present invention 1, it can be seen that
Obvious lattice fringe is presented in the region, and the about 2nm of the thickness containing 4 layers of BNNS can be observed in addition, and this in document with reporting
The thickness 0.333nm for the individual layer nanometer sheet that road is crossed is consistent.Fig. 4 is boron nitride nanosheet prepared by the embodiment of the present invention 1
Atomic force microscopy diagram and its thickness size, it is observed that the BNNS numbers of plies after most of stripping are thinned, horizontal chi
Very little reduce is about 400nm.From height map it is also seen that, boron nitride thickness is shown as 0.69nm and 1.08nm or so, there is document
Report, is influenceed, the thickness and 0.333nm of monoatomic layer boron nitride nanosheet under an atomic force microscope by solvent and substrate
Difference, so prepared BNNS is respectively 2 and 3 atomic layer level thickness.The average thickness of the boron nitride powder of original purchase
Degree is hundreds of nanometers, and lateral dimension is 1um or so, and after the embodiment of the present invention is peeled off, the thickness and size of boron nitride are all
Reduced.Illustrate using urea assisting ultrasonic method, by block boron nitride powder peel off into the relatively thin nanometer sheet of lamella be can
Go and effective.
Embodiment 2
(1) in the ratio of 1g hexagonal boron nitride powders and 200ml water, hexagonal boron nitride and water are mixed, Ran Houzai
Add the urea 100g (mass ratioes 100 with hexagonal boron nitride powder:1), continue to stir, mixture is made.
(2) mixture is placed in ice bath under the conditions of power is 200w (500w × 40%), ultrasonically treated 4 hours.
(3) finally, it is that 3000rpm centrifuges 30min with rotating speed by obtained dispersion liquid, removes unstripped boron nitride powder
End.Take supernatant liquor to be filtered, the product being filtrated to get is cleaned 2-3 times with deionized water, product is in 60 DEG C of drying process
After 8h, that is, obtain boron nitride nanosheet.
Embodiment 3
(1) in the ratio of 1g hexagonal boron nitride powders and 50ml water, hexagonal boron nitride and water is mixed, then added again
Enter the urea 20g (mass ratioes 20 with hexagonal boron nitride powder:1), continue to stir, mixture is made.
(2) mixture is placed in ice bath under the conditions of power is 200w (500w × 40%), ultrasonically treated 10 hours.
(3) finally, it is that 3000rpm centrifuges 30min with rotating speed by obtained dispersion liquid, removes unstripped boron nitride powder
End.Take supernatant liquor to be filtered, the product being filtrated to get is cleaned 2-3 times with deionized water, product is in 60 DEG C of drying process
After 8h, that is, obtain boron nitride nanosheet.
Embodiment 4
(1) in the ratio of 1g hexagonal boron nitride powders and 150ml water, hexagonal boron nitride and water are mixed, Ran Houzai
Add the urea 80g (mass ratioes 80 with hexagonal boron nitride powder:1), continue to stir, mixture is made.
(2) mixture is placed in ice bath under the conditions of power is 200w (500w × 40%), ultrasonically treated 2 hours.
(3) finally, it is that 3000rpm centrifuges 30min with rotating speed by obtained dispersion liquid, removes unstripped boron nitride powder
End.Take supernatant liquor to be filtered, the product being filtrated to get is cleaned 2-3 times with deionized water, product is in 60 DEG C of drying process
After 8h, that is, obtain boron nitride nanosheet.
Embodiment 5
(1) in the ratio of 1g hexagonal boron nitride powders and 100ml water, hexagonal boron nitride and water are mixed, Ran Houzai
Add the urea 40g (mass ratioes 40 with hexagonal boron nitride powder:1), continue to stir, mixture is made.
(2) mixture is placed in ice bath under the conditions of power is 200w (500w × 40%), ultrasonically treated 6 hours.
(3) finally, it is that 3000rpm centrifuges 30min with rotating speed by obtained dispersion liquid, removes unstripped boron nitride powder
End.Take supernatant liquor to be filtered, the product being filtrated to get is cleaned 2-3 times with deionized water, product is in 60 DEG C of drying process
After 8h, that is, obtain boron nitride nanosheet.
Described above is the preferred embodiment of the present invention, can not limit the right model of the present invention with this certainly
Enclose, it is noted that for those skilled in the art, under the premise without departing from the principles of the invention, may be used also
To make some improvement and variation, these are improved and variation is also considered as protection scope of the present invention.
Claims (6)
1. a kind of method that utilization urea assisting ultrasonic prepares hexagonal boron nitride nanosheet, it is characterised in that comprise the following steps:
Step 1: pressing hexagonal boron nitride powder and water according to 1g:50-200ml ratio is mixed and stirred for, then by urea with
The mass ratio 20-100 of hexagonal boron nitride powder:1 ratio adds urea, continues to stir, mixture is made;
Step 2: mixture made from step one is placed in ice bath, it is ultrasonically treated 2-10 hours, obtain dispersion liquid;
Step 3: dispersion liquid made from step 2 is centrifuged, then take supernatant liquor to be filtered, the product being filtrated to get is used
Deionized water is cleaned, and product obtains boron nitride nanosheet after drying.
2. the method for hexagonal boron nitride nanosheet is prepared using urea assisting ultrasonic as claimed in claim 1, it is characterised in that:
In the step one, hexagonal boron nitride powder is with water according to 1g:100ml ratio mixing.
3. the method for hexagonal boron nitride nanosheet is prepared using urea assisting ultrasonic as claimed in claim 1, it is characterised in that:
In the step 2, the power of ice-bath ultrasonic process is 200w.
4. the method for hexagonal boron nitride nanosheet is prepared using urea assisting ultrasonic as claimed in claim 1, it is characterised in that:
In the step 3, centrifugal condition is that rotating speed is 3000rpm centrifugations 30min.
5. the method for hexagonal boron nitride nanosheet is prepared using urea assisting ultrasonic as claimed in claim 1, it is characterised in that:
In the step 3, deionized water is cleaned 2-3 times.
6. the method for hexagonal boron nitride nanosheet is prepared using urea assisting ultrasonic as claimed in claim 1, it is characterised in that:
In the step 3, drying condition be 60 DEG C at a temperature of handle 8h.
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Cited By (9)
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CN108559131A (en) * | 2018-05-11 | 2018-09-21 | 四川大学 | A kind of edge hydroxylating method of modifying of six sides layered nitride boron |
CN109573965A (en) * | 2018-12-26 | 2019-04-05 | 合肥学院 | A kind of preparation method of hydroxyl modification boron nitride nanosheet dispersion liquid |
CN110004712A (en) * | 2019-04-08 | 2019-07-12 | 上海电力学院 | A kind of preparation method of the high-intensitive heat conducting film based on Kevlar nanofiber |
CN110902661A (en) * | 2019-12-23 | 2020-03-24 | 潍坊春丰新材料科技有限公司 | Nanoscale boron nitride powder for spraying field and manufacturing process thereof |
CN111807335A (en) * | 2020-07-08 | 2020-10-23 | 陕西科技大学 | Microwave-assisted method for preparing boron nitride nanosheets |
CN112759375A (en) * | 2019-11-05 | 2021-05-07 | 宜兴市中电耐磨耐火科技有限公司 | High-absorptivity and high-thermal-conductivity silicon carbide wear-resistant castable and preparation process thereof |
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Cited By (12)
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CN108559131A (en) * | 2018-05-11 | 2018-09-21 | 四川大学 | A kind of edge hydroxylating method of modifying of six sides layered nitride boron |
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CN110004712A (en) * | 2019-04-08 | 2019-07-12 | 上海电力学院 | A kind of preparation method of the high-intensitive heat conducting film based on Kevlar nanofiber |
CN110004712B (en) * | 2019-04-08 | 2021-09-07 | 上海电力学院 | Preparation method of high-strength heat-conducting film based on Kevlar nanofibers |
CN112759375A (en) * | 2019-11-05 | 2021-05-07 | 宜兴市中电耐磨耐火科技有限公司 | High-absorptivity and high-thermal-conductivity silicon carbide wear-resistant castable and preparation process thereof |
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CN112852023A (en) * | 2021-01-13 | 2021-05-28 | 武汉理工大学 | Preparation method of biomass high-dielectric nano composite film |
CN113213437A (en) * | 2021-05-31 | 2021-08-06 | 陕西科技大学 | Boron nitride nanosheet and preparation method thereof |
CN117304773A (en) * | 2023-11-30 | 2023-12-29 | 成都虹润制漆有限公司 | Low-surface-treatment graphene anticorrosive paint and preparation method thereof |
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Application publication date: 20170818 |