CN108394915A - A kind of preparation method of ultrathin boron nitride nanosheet - Google Patents
A kind of preparation method of ultrathin boron nitride nanosheet Download PDFInfo
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- CN108394915A CN108394915A CN201810582663.7A CN201810582663A CN108394915A CN 108394915 A CN108394915 A CN 108394915A CN 201810582663 A CN201810582663 A CN 201810582663A CN 108394915 A CN108394915 A CN 108394915A
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- boron nitride
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- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/14—Compounds containing boron and nitrogen, phosphorus, sulfur, selenium or tellurium
- C01B35/146—Compounds containing boron and nitrogen, e.g. borazoles
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- 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
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- 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
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- 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 preparation methods of ultrathin boron nitride nanosheet.Using melamine as nitrogen source, using boric acid as boron source, presoma is obtained by chemical reaction；Obtained boric acid melamine is utilized, under reducing atmosphere, by two step calcine technologies, ultra-thin hexagonal boron nitride nanosheet product is prepared.It is in two-dimensional sheet structure by the boron nitride that preparation method of the present invention obtains, surface has ultra-thin thickness rich in functional groups such as amino and hydroxyls, can be widely applied to multiple ambits such as biology, chemistry, photoelectricity physics and material.Raw material of the present invention is easy to get, of low cost, and synthesis technology is simple, short preparation period, and repeatability is good, can be mass, easy to spread.
Description
Technical field
The present invention relates to a kind of preparation methods of ultrathin boron nitride nanosheet.
Background technology
Boron nitride is the nonmetallic compound being made of nitrogen-atoms and boron atom, and there are mainly four types of different variants：Six sides
Boron nitride（H-BN), water chestnut side's boron nitride（r-BN）, cubic boron nitride (c-BN) and buergerite boron nitride (w-BN).Wherein, six side
Boron nitride also known as " white graphite " have the layer structure of similar graphite, have good electrical insulating property, thermal conductivity, lubricity,
High temperature resistant and chemical resistance, and there is stronger neutron absorption capability, thus, it is widely paid close attention in recent years.It is special
It is not the hexagonal boron nitride large specific surface area of laminated structure, there is abundant fault of construction.These characteristics make super thin hexagonal nitrogen
Change boron nanometer sheet material to have broad application prospects in the multiple fields such as biology, chemistry, material.But super thin hexagonal nitridation at present
The synthetic technological condition of boron nanometer sheet is harsh, to affect the practical application of the material to a certain extent.Thus, it is how high
Effect, the boron nitride superthin section for producing high quality in batches become the critical issue of the field urgent need to resolve.
Currently, the pattern of the hexagonal boron nitride of document report mainly has spherical shape（Adv. Funct. Mater. 2008,18,
3653-3661）, threadiness（Sci. Rep.,2013,3,3208-3215）, it is nanotube-shaped etc.（Mater. Sci. Eng., R,
2010,70,92-111）, very limited for the report of two-dimensional nano piece.It is mainly shelled at present by micromechanics stripping method, chemistry
Platelet boron nitride is prepared from method, high energy electron irradiation method, chemical reaction method, ball-milling method, chemical vapour deposition technique, uses these
The yield for the boron nitride nanosheet that method is prepared is often all very low, and some preparation methods are also asked along with the pollution of sample
Topic, or even also need to the combinations of two methods sometimes and can just prepare ideal two-dimensional sheet boron nitride, complicated for operation, efficiency is low
.Therefore, exploitation is a kind of easy to operate, and the synthesis technology of efficient ultrathin boron nitride nanosheet is of great significance.
Invention content
It is insufficient existing for preparation of the present invention for existing ultrathin boron nitride nanosheet, a kind of of low cost, technique is provided
Simply, the preparation method of reproducible ultrathin boron nitride nanosheet.
To achieve the above object of the invention, the technical solution adopted by the present invention is to provide a kind of system of ultrathin boron nitride nanosheet
Preparation Method includes the following steps：
(a) configuration of presoma
Using melamine as nitrogen source, using boric acid as boron source, the molar ratio of nitrogen source and boron source is 1:1~10:1；First by melamine
Powder is dissolved completely under heating, stirring condition in deionized water, adds boric acid powder, and stirring is obtained to after the reaction was complete
To precursor solution；
(b) centrifugal treating
Suspension is obtained after precursor solution is cooled to room temperature, through centrifugal treating, recycling gained white precipitate obtains after dry
Precursor powder；
(c) calcination processing
Precursor powder is subjected to precalcining under reducing atmosphere, then secondary clacining is carried out after heating up；Cooled to room temperature obtains
To ultrathin boron nitride nanosheet.
Reducing atmosphere described in technical solution of the present invention is carbon atmosphere, carbon monoxide atmosphere, nitrogen atmosphere, ammonia atmosphere, nitrogen
One kind in atmosphere, argon atmospher or their arbitrary combination.
The preferred processing condition of preparation method of the present invention is：
The condition of suspension centrifugal treating is 3000~15000 revs/min of rotating speed, and processing time is 5~30min.
The condition of calcination processing is：Precalcining temperature is 300~700 DEG C, and precalcination time is 0.5~5h；Heating rate
For 3~10 DEG C/min；Secondary clacining temperature is 800~1200 DEG C, and calcination time is 1~6h.
Since above-mentioned technical proposal is used, compared with the prior art, the present invention has the following advantages：
(1) present invention is derived from a wealth of sources using melamine and boric acid as raw material, cheap, effectively controls production cost.
(2) present invention can be obtained platelet boron nitride by the calcining of two steps, need not move through extra process, simple for process, easy
Control, good repetitiveness, production efficiency are high；Simultaneous reactions apparatus structure is simple, easy to operate, is not necessarily to expensive instrument and equipment,
Reduce production cost.
(3) the ultrathin boron nitride nanosheet purity pressed prepared by technical solution of the present invention is high, and thickness is thin, high-quality.
(4) volume production can be achieved, it is easy to spread.
Description of the drawings
Fig. 1 is the XRD spectrum of ultrathin boron nitride nanosheet prepared by the embodiment of the present invention 1.
Fig. 2 is the infrared spectrum of ultrathin boron nitride nanosheet prepared by the embodiment of the present invention 1, and abscissa is detection wave in figure
Long, ordinate is transmitance.
Fig. 3 is the transmission electron microscope collection of illustrative plates of ultrathin boron nitride nanosheet prepared by the embodiment of the present invention 1.
Fig. 4 is the AFM collection of illustrative plates of ultrathin boron nitride nanosheet prepared by the embodiment of the present invention 1.
Fig. 5 is the corresponding A FM height distribution of ultrathin boron nitride nanosheet prepared by the embodiment of the present invention 1.
Specific implementation mode
Technical solution of the present invention is described further with reference to the accompanying drawings and examples.
Embodiment 1
(a) it is raw material to take 4g melamine powders, is dissolved in 150mL deionized waters, is fully stirred under 85 DEG C of water bath condition
It mixes to after being completely dissolved, adds the boric acid powder of 1g, constant temperature stirs 30min, obtains precursor solution；
(b) suspension is obtained after being cooled to room temperature precursor solution, by centrifugal treating, recycling gained white precipitate is dry
After obtain precursor powder；
(c) using double crucible sleeve structure devices, activated carbon is placed in big crucible, precursor powder is placed in small crucible so that preceding
Body powder is driven to be under reducing atmosphere.The device is put into Muffle furnace, first the precalcining 2h at 550 DEG C, then with 6 DEG C/min
Speed be warming up to 900 DEG C, calcine 4h, cooled to room temperature obtains white powder, as ultrathin boron nitride nanosheet.
Referring to attached drawing 1, it is the XRD spectrum of ultrathin boron nitride nanosheet manufactured in the present embodiment.It can from Fig. 1
Go out, the sample that the present embodiment is prepared is pure hexagonal boron nitride.
Referring to attached drawing 2, it is the infrared spectrum of ultrathin boron nitride nanosheet manufactured in the present embodiment.It can from Fig. 2
Go out the vibration band there are B-N, N-B-N in sample（~1384cm-1、~792cm-1）, the vibration peak of-OH（~3431cm-1）, and-
NH2Vibration peak（~3220cm-1）.
Referring to attached drawing 3, it is the transmission electron microscope collection of illustrative plates of ultrathin boron nitride nanosheet manufactured in the present embodiment.It can from Fig. 3
To find out, ultrathin boron nitride nanosheet prepared by the present embodiment structure in the form of sheets.
Referring to attached drawing 4, it is the AFM collection of illustrative plates of ultrathin boron nitride nanosheet manufactured in the present embodiment.
Referring to attached drawing 5, it is the corresponding A FM height distribution of ultrathin boron nitride nanosheet manufactured in the present embodiment.From Fig. 5
As can be seen that the boron nitride nanosheet thinner thickness that the present embodiment is prepared, thickness is less than 7nm.
Embodiment 2
(a) it is raw material to take 4g melamine powders, is dissolved in 150mL deionized waters, is fully stirred under 85 DEG C of water bath condition
It mixes to after being completely dissolved, adds the boric acid powder of 0.5g, constant temperature stirs 30min, obtains precursor solution；
(b) suspension is obtained after being cooled to room temperature above-mentioned precursor solution, by centrifugal treating, recycles gained white precipitate,
Precursor powder is obtained after drying；
(c) using double crucible sleeve structure devices, activated carbon is placed in big crucible, above-mentioned precursor powder is placed in small crucible, is made
Precursor powder is obtained to be under reducing atmosphere.The device is put into Muffle furnace, the precalcining 2h first at 550 DEG C, then with 3
DEG C/speed of min is warming up to 800 DEG C, 4h is calcined, cooled to room temperature obtains white powder, as ultrathin boron nitride nanometer
Piece.
Embodiment 3
(a) it is raw material to take 6g melamine powders, is dissolved in 200mL deionized waters, is fully stirred under 90 DEG C of water bath condition
It mixes to after being completely dissolved, adds the boric acid powder of 1g, constant temperature stirs 30min, obtains precursor solution；
(b) suspension is obtained after being cooled to room temperature above-mentioned precursor solution, by centrifugal treating, recycles gained white precipitate,
Precursor powder is obtained after drying；
(c) using double crucible sleeve structure devices, activated carbon is placed in big crucible, above-mentioned precursor powder is placed in small crucible, is made
Precursor powder is obtained to be under reducing atmosphere.The device is put into Muffle furnace, the precalcining 2h first at 550 DEG C, then with 5
DEG C/speed of min is warming up to 850 DEG C, 4h is calcined, cooled to room temperature obtains white powder, as ultrathin boron nitride nanometer
Piece.
Embodiment 4
(a) it is raw material to take 2g melamine powders, is dissolved in 150mL deionized waters, is fully stirred under 80 DEG C of water bath condition
It mixes to after being completely dissolved, adds the boric acid powder of 1g, constant temperature stirs 30min, obtains precursor solution；
(b) suspension is obtained after being cooled to room temperature above-mentioned precursor solution, by centrifugal treating, recycles gained white precipitate,
Precursor powder is obtained after drying；
(c) using double crucible sleeve structure devices, activated carbon is placed in big crucible, above-mentioned precursor powder is placed in small crucible, is made
Precursor powder is obtained to be under reducing atmosphere.The device is put into Muffle furnace, the precalcining 2h first at 550 DEG C, then with 3
DEG C/speed of min is warming up to 950 DEG C, 4h is calcined, cooled to room temperature obtains white powder, as ultrathin boron nitride nanometer
Piece.
Claims (4)
1. a kind of preparation method of ultrathin boron nitride nanosheet, it is characterised in that include the following steps：
(a) configuration of presoma
Using melamine as nitrogen source, using boric acid as boron source, the molar ratio of nitrogen source and boron source is 1:1~10:1；First by melamine
Powder is dissolved completely under heating, stirring condition in deionized water, adds boric acid powder, and stirring is obtained to after the reaction was complete
To precursor solution；
(b) centrifugal treating
Suspension is obtained after precursor solution is cooled to room temperature, through centrifugal treating, recycling gained white precipitate obtains after dry
Precursor powder；
(c) calcination processing
Precursor powder is subjected to precalcining under reducing atmosphere, then secondary clacining is carried out after heating up；Cooled to room temperature obtains
To ultrathin boron nitride nanosheet.
2. a kind of preparation method of ultrathin boron nitride nanosheet according to claim 1, it is characterised in that：The also Primordial Qi
Atmosphere is carbon atmosphere, carbon monoxide atmosphere, nitrogen atmosphere, ammonia atmosphere, nitrogen atmosphere, one kind in argon atmospher or their arbitrary combination.
3. a kind of preparation method of ultrathin boron nitride nanosheet according to claim 1, it is characterised in that：Suspension centrifuges
The condition of processing is 3000~15000 revs/min of rotating speed, and processing time is 5~30min.
4. a kind of preparation method of ultrathin boron nitride nanosheet according to claim 1, it is characterised in that：At the calcining
The condition of reason is：Precalcining temperature is 300~700 DEG C, and precalcination time is 0.5~5h；Heating rate is 3~10 DEG C/min；
Secondary clacining temperature is 800~1200 DEG C, and calcination time is 1~6h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052343A (en) * | 2018-10-08 | 2018-12-21 | 河北工业大学 | A kind of preparation method of ultra-thin hexagonal boron nitride piece |
| WO2019232765A1 (en) * | 2018-06-07 | 2019-12-12 | 苏州大学张家港工业技术研究院 | Preparation method for ultrathin boron nitride nanosheet |
| CN112919431A (en) * | 2021-02-07 | 2021-06-08 | 辽东学院 | High-yield and high-crystallinity hexagonal boron nitride nanosheet and preparation method thereof |
| CN112938911A (en) * | 2021-03-24 | 2021-06-11 | 云南华谱量子材料有限公司 | Preparation method of boron nitride nanosheet |
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| CN103910344A (en) * | 2014-03-24 | 2014-07-09 | 中国科学院深圳先进技术研究院 | Preparation method of hexagonal boron nitride |
| CN106829888A (en) * | 2015-12-04 | 2017-06-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Boron nitride nanosheet powder and its magnanimity preparation method |
| CN107376825A (en) * | 2017-08-22 | 2017-11-24 | 中国科学院过程工程研究所 | A kind of hexagonal boron nitride material and its production and use |
-
2018
- 2018-06-07 CN CN201810582663.7A patent/CN108394915A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103910344A (en) * | 2014-03-24 | 2014-07-09 | 中国科学院深圳先进技术研究院 | Preparation method of hexagonal boron nitride |
| CN106829888A (en) * | 2015-12-04 | 2017-06-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Boron nitride nanosheet powder and its magnanimity preparation method |
| CN107376825A (en) * | 2017-08-22 | 2017-11-24 | 中国科学院过程工程研究所 | A kind of hexagonal boron nitride material and its production and use |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019232765A1 (en) * | 2018-06-07 | 2019-12-12 | 苏州大学张家港工业技术研究院 | Preparation method for ultrathin boron nitride nanosheet |
| CN109052343A (en) * | 2018-10-08 | 2018-12-21 | 河北工业大学 | A kind of preparation method of ultra-thin hexagonal boron nitride piece |
| CN112919431A (en) * | 2021-02-07 | 2021-06-08 | 辽东学院 | High-yield and high-crystallinity hexagonal boron nitride nanosheet and preparation method thereof |
| CN112938911A (en) * | 2021-03-24 | 2021-06-11 | 云南华谱量子材料有限公司 | Preparation method of boron nitride nanosheet |
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Application publication date: 20180814 |