CN106082147B - The method that a kind of liquid phase chemical stripping of stabilization prepares boron nitride nanosheet - Google Patents
The method that a kind of liquid phase chemical stripping of stabilization prepares boron nitride nanosheet Download PDFInfo
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- CN106082147B CN106082147B CN201610378822.2A CN201610378822A CN106082147B CN 106082147 B CN106082147 B CN 106082147B CN 201610378822 A CN201610378822 A CN 201610378822A CN 106082147 B CN106082147 B CN 106082147B
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- 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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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses the method that a kind of liquid phase chemical stripping of stabilization prepares boron nitride nanosheet, step includes：(1) after hexagonal boron nitride being mixed to infiltration with strong acid, add in ferrate and be uniformly mixed and reacted；(2) reactant is added drop-wise in distilled water after reacting and is diluted；(3) solution after dilution is centrifuged, the boron nitride powder that removal bulk is not peeled off；(4) supernatant liquid filters to obtain reaction product, is first cleaned with hydrochloric acid, then is washed with deionized water to neutrality, and product drying obtains boron nitride nanosheet.The method of the present invention prepares boron nitride nanosheet by the reaction of strong acid and ferrate, and raw material is easy to get, safety and stability, does not generate pollution, and easy to operate, without the equipment of complex and expensive, yield is higher, good product quality.
Description
Technical field
The invention belongs to inorganic non-metallic material preparation method technical fields, and in particular to a kind of to pass through stable liquid phase
Learn the method that stripping prepares boron nitride nanosheet.
Background technology
2004, Geim and Novoselov of Univ Manchester UK et al. were using a kind of simple " micromechanical forces point
Split method " it is prepared for a kind of two-dimension nano materials of monoatomic layer thickness -- graphene is started with this, graphene and class graphene two
Dimension material is increasingly becoming one of research emphasis.
Hexagonal boron nitride (h-BN) has similar layer structure to graphite, and each layer is alternately arranged by B atoms and N atoms
The hexagonal honeycomb structure infinitely extended is formed, because its color is white, so there is the title of " white graphite ".Boron nitride nanosheet has
There are excellent mechanical property, high thermal conductivity coefficient, high chemical stability and inoxidizability, excellent dielectric properties and good profit
Slip energy, it is wide that these excellent performances make boron nitride nanosheet have in composite material preparation, hydrogen storage, catalyst carrier etc.
General application prospect.In addition, boron nitride nanosheet also has deep-UV light-emitting performance and nonlinear optical property, led in optics
Domain also has certain application prospect.
At present, the method for preparing boron nitride nanosheet mainly has：Mechanical stripping method is (including adhesive tape stripping method, plasma
Etching method, ball-milling method, fluid stripping method etc., L.H.Li, Y.Chen, G.Behan, H.Z.Zhang, M.Petravic,
A.M.Glushenkov, J.Mater.Chem., 2011,21,11862-11866.), chemical stripping method
(G.R.Bhimanapati,D.Kozuch,J.A.Robinson,Nanoscale,2014,6,11671-11675；M.Du,
Y.Z.Wu, X.P.Hao, CrystEngComm, 2013,15,1782-1786.), ultrasonic wave added solvent stripping method
(T.Morishita,H.Okamoto,Y.Katagiri,M.Matsushita,K.Fukumori,Chem.Commun.,2015,
51,12068-12071.), chemical vapour deposition technique (Y.M.Shi, H.Christoph, X.T.Jia, K.K.Kim, A.Reina,
M.Hofmann,A.L.Hsu,K.Zhang,H.N.Li,Y.Z.Juang,M.S.Dresselhaus,L.J.Li,J.Kong,Nano
Lett., 2010,10 (10), 4134-4139.) and solid reaction process etc..Although the above method successfully prepares boron nitride nanometer
Piece, but these methods limit the preparation and application of boron nitride nanosheet there are still some shortcomings.For example, machinery stripping
Generally easily nanometer sheet is caused the defects of certain from method, chemical stripping method is tried sometimes for using dangerous or toxic chemistry
Agent simultaneously generates harmful accessory products, and ultrasonic wave added solvent stripping method takes relatively long, chemical vapour deposition technique and solid reaction process
Generally require the equipment using higher reaction temperature or reaction pressure, complexity and costliness.
On the premise of boron nitride nanosheet structural intergrity and yield is ensured, exploitation one kind is at low cost, equipment is simple, behaviour
Make convenient and safety and stability process of preparing, be still the difficult point of this field research.
The content of the invention
In order to solve the above technical problems, the liquid phase chemical it is an object of the invention to provide a kind of stabilization removes preparation nitridation
The method of boron nanometer sheet.This method is at low cost, and equipment is simple, easy to operate, and safety and stability, yield is higher, good product quality.
To achieve these goals, the present invention adopts the following technical scheme that：
The method that a kind of liquid phase chemical stripping of stabilization prepares boron nitride nanosheet, includes the following steps：
(1) after hexagonal boron nitride being mixed to infiltration with strong acid, add in ferrate and be uniformly mixed and reacted；
(2) reactant after step (1) reaction, which is added in distilled water, is diluted；
(3) the solution centrifugal treating after step (2) is diluted, the boron nitride powder that removal bulk is not peeled off；
(4) step (3) processing after supernatant liquid filter to obtain reaction product, first with acid cleaning, then be washed with deionized water to
Neutrality, product drying, obtains boron nitride nanosheet.
The possible principle of the method for the invention is：Infiltration is mixed with strong acid using boron nitride first, strong acid enters nitrogen
Change the interlayer of boron, tentatively expand interlamellar spacing；Then the ferrate added in can react with the strong acid of interlayer, reaction process
And the product of generation can further expand interlamellar spacing；It is added to after being diluted in distilled water, ferrate can be with H+And H2O
Reaction generation oxygen, the spilling of oxygen help to realize the stripping of boron nitride nanosheet.Through inventor to multiple induction boron nitride
The screening of nanometer sheet stripping reaction finds that the present invention adds in reaction using ferrate and can effectively strut boron nitride layer and layer
The distance between and prevent the reunion of boron nitride nanosheet, be conducive to the stripping of nanometer sheet.
For example, when the ferrate of selection is potassium ferrate, correlated response includes：
FeO4 2-+4H+→Fe3++2H2O+O2↑
4[H3FeO4]++8H3O+→4Fe3++3O2↑+18H2O
4FeO4 2-+10H2O→4Fe(OH)3+3O2↑+8OH-
In preferred embodiments, in step (1), the mass volume ratio of hexagonal boron nitride and strong acid is 1g：20-
The mass ratio of 100ml, hexagonal boron nitride and ferrate is 1g：1-10g.By experimental study, in the proportion, nitridation
Boron nanometer sheet removes the ratio carried out more thoroughly, can obtain large scale and the less boron nitride nanosheet of the number of plies.It needs to illustrate, it should
Proportion belongs to the scope for comparing optimization, and not in the range, although peeling effect is poor, (such as lamella is thicker, it is not thorough to remove
Bottom) or cost raising is removed, but still can realize the peeling effect of boron nitride nanosheet.
In preferred embodiments, in step (1), it is small that hexagonal boron nitride and strong acid are thoroughly mixed infiltration 1-24
When, ferrate is then added in, continues to stir, is uniformly mixed and is reacted；Preferably, reaction condition is mixture at 0-80 DEG C
Be stirred to react 1-24 it is small when.
In preferred embodiments, in step (1), strong acid is the mixed of sulfuric acid, nitric acid, phosphoric acid or their arbitrary proportions
Acid.
In preferred embodiments, in step (1), ferrate is that potassium ferrate, Na2Fe04 or both are arbitrary
The mixture of ratio.
In preferred embodiments, in step (2), reactant is added drop-wise in distilled water is diluted dropwise.It is dilute dropwise
Release the stripping for being more advantageous to nanometer sheet.
In preferred embodiments, in step (4), supernatant liquid filters to obtain reaction product after processing, clear with hydrochloric acid
It washes 2-3 times, then is washed with deionized water until neutrality, after product is when 60 DEG C of drying 10 are small, obtain boron nitride nanosheet.
The present invention achieves following advantageous effect：
(1) the method for the invention carries out the infiltration of boron nitride using strong acid, and strong acid is entered between boron nitride layer, passes through height
The stripping of reaction induced boron nitride nanosheet after ferrite addition, nitrogen can effectively be expanded by adding in reaction using ferrate
Change the distance between boron layer and layer and prevent the reunion of boron nitride nanosheet, be conducive to the stripping of nanometer sheet.
(2) Optimizing Process Parameters of the present invention, under the conditions of the technological parameter of optimization, boron nitride nanosheet removes the ratio carried out
More thoroughly, structural integrity is good, can obtain micron order size and individual layer or the less boron nitride nanosheet of the number of plies.
(3) the method for the invention raw material is easy to get, at low cost, used ferrate asepsis environment-protecting；Equipment is simple, behaviour
Facilitate, reaction temperature is low, and reaction product processing is simple.
(4) stability of the invention, security and the feature of environmental protection are opposite improves, and production cost reduces, and ferrate can be steady
Surely reacted with strong acid, with permanganate compared with the reaction of strong acid, the mechanism reacted and removed is different, which will not
The substance of explosive is generated, and heavy metal ion pollution (Mn will not be generated2+) and toxic gas, and without hydrogen peroxide, it is high
Ferrite can in acid condition, with H+、H2O reaction generation oxygen, the present invention are real on the premise of nanometer chip architecture is not damaged
The preparation of existing nanometer sheet high yield.
Description of the drawings
Fig. 1 is the stereoscan photograph of boron nitride nanosheet prepared by the embodiment of the present invention 1.
Fig. 2 is the low power transmission electron microscope photo of boron nitride nanosheet prepared by the embodiment of the present invention 1.
Fig. 3 is the high power transmission electron microscope photo of boron nitride nanosheet prepared by the embodiment of the present invention 1.
Specific embodiment
Embodiment 1：
(1) by 1g hexagonal boron nitride powders and the 60ml concentrated sulfuric acids be thoroughly mixed infiltration 4 it is small when, then add high ferro
Sour potassium 3g, continues to stir, and is uniformly mixed；
(2) by mixture 20 DEG C be stirred to react 10 it is small when, then reactant is added drop-wise to dropwise in distilled water carry out it is dilute
It releases；
(3) solution after dilution is centrifuged, the boron nitride powder that removal bulk is not peeled off；
(4) filter and obtain reaction product, cleaned 2-3 times with hydrochloric acid, then be washed with deionized water until neutrality, product is 60
DEG C drying 10 it is small when after, obtain boron nitride nanosheet.
The stereoscan photograph of boron nitride nanosheet manufactured in the present embodiment is as shown in Figure 1；Nitridation manufactured in the present embodiment
The low power transmission electron microscope photo of boron nanometer sheet is as shown in Figure 2；The high power transmission electron microscope of boron nitride nanosheet manufactured in the present embodiment
Photo is as shown in Figure 3.
Embodiment 2：
(1) by 1g hexagonal boron nitride powders and 100ml nitric acid be thoroughly mixed infiltration 2 it is small when, then add high ferro
Sour potassium 3g, continues to stir, and is uniformly mixed；
(2) by mixture 30 DEG C be stirred to react 24 it is small when, then reactant is added drop-wise to dropwise in distilled water carry out it is dilute
It releases；
(3) solution after dilution is centrifuged, the boron nitride powder that removal bulk is not peeled off；
(4) filter and obtain reaction product, cleaned 2-3 times with hydrochloric acid, then be washed with deionized water until neutrality, product is 60
DEG C drying 10 it is small when after, obtain boron nitride nanosheet.
Embodiment 3：
(1) by 1g hexagonal boron nitride powders and 100ml sulfuric acid be thoroughly mixed infiltration 6 it is small when, then add high ferro
Sour potassium 5g, continues to stir, and is uniformly mixed；
(2) by mixture 60 DEG C be stirred to react 10 it is small when, reactant is added drop-wise to dropwise in distilled water after cooling and is carried out
Dilution；
(3) solution after dilution is centrifuged, the boron nitride powder that removal bulk is not peeled off；
(4) filter and obtain reaction product, cleaned 2-3 times with hydrochloric acid, then be washed with deionized water until neutrality, product is 60
DEG C drying 10 it is small when after, obtain boron nitride nanosheet.
Embodiment 4：
(1) by 1g hexagonal boron nitride powders and 30ml phosphoric acid be thoroughly mixed infiltration 24 it is small when, then add high ferro
Sour potassium 8g, continues to stir, and is uniformly mixed；
(2) by mixture 40 DEG C be stirred to react 6 it is small when, then reactant is added drop-wise to dropwise in distilled water carry out it is dilute
It releases；
(3) solution after dilution is centrifuged, the boron nitride powder that removal bulk is not peeled off；
(4) filter and obtain reaction product, cleaned 2-3 times with hydrochloric acid, then be washed with deionized water until neutrality, product is 60
DEG C drying 10 it is small when after, obtain boron nitride nanosheet.
Embodiment 5：
(1) by 1g hexagonal boron nitride powders and 60ml sulfuric acid be thoroughly mixed infiltration 4 it is small when, then add ferric acid
Sodium 3g continues to stir, and is uniformly mixed；
(2) by mixture 20 DEG C be stirred to react 10 it is small when, then reactant is added drop-wise to dropwise in distilled water carry out it is dilute
It releases；
(3) solution after dilution is centrifuged, the boron nitride powder that removal bulk is not peeled off；
(4) filter and obtain reaction product, cleaned 2-3 times with hydrochloric acid, then be washed with deionized water until neutrality, product is 60
DEG C drying 10 it is small when after, obtain boron nitride nanosheet.
Although the above-mentioned specific embodiment to the present invention is described, not to the limit of the scope of the present invention
System, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art need not pay
Go out various modifications or changes that creative work can be made still within protection scope of the present invention.
Claims (6)
1. the method that a kind of liquid phase chemical stripping of stabilization prepares boron nitride nanosheet, includes the following steps：
（1）After hexagonal boron nitride is mixed infiltration with strong acid, add in ferrate and be uniformly mixed and reacted；
（2）Step（1）Product after reaction, which is added in distilled water, to be diluted；
（3）By step（2）Solution centrifugal treating after dilution, the boron nitride powder that removal bulk is not peeled off；
（4）By step（3）Supernatant liquid filters to obtain reaction product after processing, is first cleaned, then is washed with deionized water into acid
Property, product drying obtains boron nitride nanosheet；
The step（1）In, the mass volume ratio of hexagonal boron nitride and strong acid is 1g：20-100ml, hexagonal boron nitride and high ferro
The mass ratio of hydrochlorate is 1g：1-10g；
The step（1）In, hexagonal boron nitride and strong acid be thoroughly mixed infiltration 1-24 it is small when, then add in ferrate,
Continue to stir, be uniformly mixed and reacted.
2. method according to claim 1, which is characterized in that step（1）In, strong acid for sulfuric acid, nitric acid, phosphoric acid or they
The nitration mixture of arbitrary proportion.
3. method according to claim 1, which is characterized in that step（1）In, ferrate is potassium ferrate, Na2Fe04
Or both arbitrary proportion mixture.
4. method according to claim 1, which is characterized in that step（1）In, it is described to be uniformly mixed the reaction item reacted
Part for mixture 0-80 DEG C be stirred to react 1-24 it is small when.
5. method according to claim 1, which is characterized in that step（2）In, reactant is added drop-wise in distilled water and carries out dropwise
Dilution.
6. method according to claim 1, which is characterized in that step（4）In, supernatant liquid filters to obtain reaction production after processing
Object is cleaned 2-3 times with hydrochloric acid, then is washed with deionized water until neutrality, after product is when 60 DEG C of drying 10 are small, obtains boron nitride
Nanometer sheet.
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| CN106747530B (en) * | 2017-01-25 | 2020-04-21 | 山东大学 | Boron nitride nanosheet reinforced ceramic matrix composite and preparation method thereof |
| CN107151002B (en) * | 2017-07-18 | 2019-09-06 | 深圳市泽纬科技有限公司 | A method of single layer or few layer boron nitride nanosheet are prepared by intercalator of the concentrated sulfuric acid |
| WO2019051382A1 (en) * | 2017-09-11 | 2019-03-14 | Rogers Corporation | Nanosheet and method for the manufacture thereof |
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| CN115072676A (en) * | 2022-06-22 | 2022-09-20 | 佛山(华南)新材料研究院 | Method for preparing two-dimensional material by mechanical stripping assisted by chemical method |
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