CN106829888A - Boron nitride nanosheet powder and its magnanimity preparation method - Google Patents
Boron nitride nanosheet powder and its magnanimity preparation method Download PDFInfo
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Abstract
The invention discloses a kind of boron nitride nanosheet powder and its magnanimity preparation method.The preparation method includes：Boron source and nitrogen source predecessor are sufficiently mixed; 1100~1500 DEG C are heated in nitrogenous reaction atmosphere and more than 0.5h is incubated, room temperature is cooled in protective atmosphere afterwards, crude product is obtained; the crude product is post-processed again, obtains the boron nitride nanosheet powder.The purity of the boron nitride nanosheet powder is more than 99%, and wherein boron nitride nanosheet is hexagonal boron nitride nanosheet, and the thickness of the hexagonal boron nitride nanosheet is 1~20 atomic layer, and radial dimension is 1~20 μm.The raw material boron oxide and metal nitride that the present invention is used are cheap and easy to get, reaction can a step complete, process is simple, and feed stock conversion, more than 90%, product purity is more than 99% after pickling.Especially, the present invention can also react the boron nitride nanosheet powder for preparing more than gram level by single batch, realize batch production.
Description
Technical field
Present invention relates particularly to a kind of boron nitride nanosheet powder and its magnanimity preparation method, belong to technical field of inorganic nanometer material.
Background technology
Boron nitride nanosheet (BNNS) has many excellent physicochemical properties, such as excellent electrical insulating property, heat conduction system high
Direct band gap, big specific surface area, good bio-compatibility several, wide, and good chemical inertness, high temperature resistant, antioxygen
Change performance, in graphene electronic device, deep-UV light-emitting, composite, heat sink material, friction material, drug loading, catalysis
The numerous areas such as agent load suffer from being widely applied prospect.
At present, the synthesis of BN mainly has both direction, and one is that the BN nanometer sheets of atomically flating or continuous are grown in substrate
Film.One is the magnanimity preparation of the BN nanometer sheets of powder.
The synthetic method of the BNNS on atomically flating, mainly using chemical vapour deposition technique, is there is the Metal Substrate of catalytic property
Basal surface synthesizes, and these metals include copper (Nano Lett.2010,10,3209-3215；Nano Lett.2012,12,161-166), nickel
(Nano Lett.2010,10,4134-4139), ruthenium monocrystal (ACS Nano, 2011,5 (9) 7303-7309) and platinum (Nano Lett.
2013,13,1834-1839；ACS Nano, 2013,7 (6) 5199-5206), etc..The BN nanometer sheets of these methods synthesis can be with
It is transferred to Si or Si/SiO2In substrate, the substrate as graphene electronic device.Due to the good insulation of boron nitride nanosheet
Property, and Lattice Matching good between Graphene and boron nitride, can cause that graphene device plays better performance.
On the other hand, macroscopically the BN nanometer sheets of powder morphology there is also great demand space.Such as drug loading, ultraviolet
The occasions such as luminous, catalyst load, composite, heat sink material are, it is necessary to the material of powder state.At present, on powder
BN nanometer sheets synthesize, have " method from top to bottom ", will micron-sized BN particles successively peel off, obtain BN nanometer sheets.Such as liquid
Phase stripping method (Adv.Mater.2009,21,2889-2893), mechanical stripping method (Appl.Phys.Lett.2008,92,133107-1-
133107-3.), chemical graft process etc..These method low costs, but the production cycle is more long, complex process, inefficiency, yield
Industrial requirement can not be met.Meanwhile, also there is method (Adv.Mater.2011,23,4072-4076) composite powder of use " chemical bubbling "
Body BN nanometer sheets.The method, as raw material, is decomposed by high-temperature heating and obtains BNNS using ammonia borine.What the method was obtained
BNNS lamellas are larger, and yield is up to 40% but relatively costly, are not suitable for batch and prepare.Meanwhile, CN103043634A is also public
A kind of boron nitride nanosheet raw powder's production technology of cloth, metal boride powder is mixed with ammonium salt powder, and grinding is uniform, sealing
In reactor, 6~48h are reacted in 400~700 DEG C, pickling removes accessory substance, then washes again, alcohol is washed till neutrality, centrifugation point
Through vacuum drying after, Hexagonal boron nitride two-dimensional ultrathin nanometer sheet is obtained.The method synthesis temperature is relatively low, the nanometer sheet lamella for obtaining
Size is small, and crystallinity is poor.
Make a general survey of the production technology of boron nitride nanosheet, cost and relatively low efficiency higher seriously constrain further scientific research with
Practical application.The magnanimity technology of preparing of BN nanometer sheet powders is developed, is of great practical significance.
The content of the invention
In view of the shortcomings of the prior art, it is a primary object of the present invention to provide a kind of boron nitride nanosheet powder and its magnanimity preparation side
Method.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
Some embodiments of the present invention provide a kind of boron nitride nanosheet powder magnanimity preparation method, and it includes：By boron source and nitrogen source
Predecessor is sufficiently mixed, and 1100~1500 DEG C is heated in nitrogenous reaction atmosphere and more than 0.5h is incubated, afterwards in protective atmosphere
Room temperature is cooled to, crude product is obtained, then the crude product is post-processed, obtain the boron nitride nanosheet powder.
Among some embodiments, the boron source is 10 with the mol ratio of the nitrogen source predecessor:1~1:10.
Among some embodiments, the boron source predecessor includes boron oxide；And/or, the nitrogen source predecessor includes nitride metal
Thing.
Among some more specific embodiment, the metal nitride preferably is selected from appointing in magnesium nitride, lithium nitride, CaCl2
Anticipate one or more combination.
Among some embodiments, the boron nitride nanosheet powder magnanimity preparation method includes：Boron source and nitrogen source predecessor are filled
Divide mixing, and 1200~1300 DEG C, and 0.5~4h of insulation are heated in nitrogenous reaction atmosphere.
Among some embodiments, the reaction atmosphere is at least one formation in ammonia atmosphere or ammonia and nitrogen and argon gas
Mixed atmosphere；And/or, the protective atmosphere is nitrogen and/or argon gas atmosphere.
Among some embodiments, described post processing includes：By the crude product pickling, filtering, dry, so as to obtain institute
State boron nitride nanosheet powder.
Among some more specific embodiment, described post processing includes：By the crude product with concentration be 1~3mol/L
Acid solution wash after, filtering, then in 60~80 DEG C of 6~12h of drying, obtain the boron nitride nanosheet powder.
The invention allows for a kind of boron nitride nanosheet powder, its purity is more than 99%, and wherein boron nitride nanosheet is six
Square boron nitride nanosheet, the thickness of the hexagonal boron nitride nanosheet is 1~20 atomic layer, and radial dimension is 1~20 μm.
Among some embodiments, the thickness of the hexagonal boron nitride nanosheet is preferably 1~10 atomic layer, and radial dimension is preferred
It is 1~10 μm.
Compared with prior art, advantages of the present invention includes：
1. it is raw material that the boron nitride nanosheet powder magnanimity preparation method that the present invention is provided uses boron oxide and metal nitride, and its is cheap
It is easy to get, and reaction can step completion, process is simple.
2. raw material reaction efficiency is up to 90% in the boron nitride nanosheet powder magnanimity preparation method that the present invention is provided, and product is pure after pickling
Degree up to 99%.
3. the boron nitride nanosheet powder magnanimity preparation method single batch reaction that the present invention is provided can prepare boron nitride nanometer more than gram level
Piece powder, realizes batch production.
Brief description of the drawings
Fig. 1 is the photo in kind of boron nitride nanosheet powder crude product in the embodiment of the present invention 1；
Fig. 2 is the photo in kind of the boron nitride nanosheet powder in the embodiment of the present invention 1 after purification；
Fig. 3 is the XRD of boron nitride nanosheet in the embodiment of the present invention 1；
Fig. 4 is the TEM figures of boron nitride nanosheet in the embodiment of the present invention 1；
Fig. 5 is the SEM figures of boron nitride nanosheet in the embodiment of the present invention 2；
Fig. 6 is the Raman collection of illustrative plates of boron nitride nanosheet in the embodiment of the present invention 2；
Fig. 7 is the TEM figures of boron nitride nanosheet in the embodiment of the present invention 2；
Fig. 8 is the XRD of boron nitride nanosheet in the embodiment of the present invention 3；
Fig. 9 is the photo in kind of boron nitride nanosheet in the embodiment of the present invention 5.
Specific embodiment
In view of deficiency of the prior art, inventor is able to propose technical side of the invention through studying for a long period of time and largely putting into practice
Case, it relates generally to a kind of boron nitride nanosheet powder and its magnanimity preparation method.
In an exemplary embodiments of the invention, a kind of magnanimity preparation method of boron nitride nanosheet powder is comprised the following steps：
(1) boron source and nitrogen source predecessor are sufficiently mixed, 1100~1500 DEG C is heated in the atmosphere containing ammonia (preferably
1100~1400 DEG C, especially preferably 1200~1300 DEG C) and 0.5~4h of insulation, it is cooled to room under the protection of nitrogen or argon gas
Temperature, obtains white crude.
(2) crude product pickling, filtering, the drying for being obtained step (1), can obtain boron nitride nanosheet of the purity more than 99%
Powder.
By foregoing method, according to the amount and equipment volume of predecessor, the yield of single batch is up to more than gram level.In more excellent synthesis
Under the conditions of, 100g reactants can obtain 30~35g boron nitride nanosheets, and net yield is up to 90%.
Wherein, the boron source, the selection range of nitrogen source and its usage ratio can be as mentioned before.
In one more specifically scheme, the preparation method is related to following chemical reaction (anti-in ammonia with boron oxide and magnesium nitride
As a example by answering)：
B2O3+Mg3N2→2BN+3MgO
2B2O3+Mg3N2→2BN+Mg3(BO3)2
B2O3+2NH3→2BN+3H2O。
Preferably, step (1) includes：By boron source and nitrogen source with mol ratio 10:1~1:10 are sufficiently mixed, in the atmosphere containing ammonia
In be heated to 1100~1500 DEG C and be incubated 0.5~4h, decline in the protection of nitrogen or argon gas and warm to room temperature, obtain white thick producing
Thing.For example, the equation of one of which reaction is：2B2O3+Mg3N2→2BN+Mg3(BO3)2
Pickling described in step (2) is preferably：Washed 3~5 times with 1.0~3.0mol/L dust technologies or watery hydrochloric acid.Through overpickling,
The operation such as filtering, can efficiently remove byproduct of reaction, obtain the BN nanometer sheets of high-purity.
Drying described in step (2) is preferably：6~12h is dried at 60~80 DEG C.
A kind of thickness of the Hexagonal boron nitride two-dimensional ultrathin nanometer sheet (hexagonal boron nitride nanosheet) prepared by the above method is
1~20 atomic layer (preferably 1~10 atomic layer), size is 1~20 μm (preferably 1~10 μm), macroscopically in powder
Form.
Above-mentioned Hexagonal boron nitride two-dimensional ultrathin nanometer sheet can be applied to deep-UV light-emitting, composite, heat sink material, friction material,
The numerous areas such as drug loading, catalyst carrier.
Below in conjunction with some embodiments, the present invention is described in detail.
Embodiment 1 is by B2O3And Mg3N2With 2:1 mol ratio is sufficiently mixed, and takes 1g and is placed in open alumina crucible, Ran Houfang
Enter in tube furnace, be evacuated to 10-3Pa, is passed through the NH of 200 standard milliliters/minute (sccm)3, it is warmed up to 1300 DEG C.
NH is closed after 1300 DEG C of isothermal reaction 180min3, it is passed through the N of 500sccm2, in N2Room temperature is cooled in atmosphere, is taken out, obtained
To crude product.Then use 3mol/L nitric acid, ultrasonic pickling 5h to refilter, dry products therefrom, purity can be obtained 99%
Boron nitride nanosheet powder above.Fig. 1 is the photograph in kind that the present embodiment prepares BN nanometer sheet crude product of the gained without pickling
Piece.Fig. 2 is that the present embodiment BN nanometer sheets (boron nitride nanosheet, BN nanosheet, abbreviation BNNS) after purification are in kind to be shone
Piece.The present embodiment can obtain 90% yield.Fig. 3 is the XRD of the present embodiment gained BNNS powders, it was demonstrated that be six sides
Structure BN.Fig. 4 is the TEM shape appearance figures of the present embodiment gained BNNS powders, it is seen that its size is in micron level.
Embodiment 2 is by B2O3And Mg3N2With 1:1 mol ratio is sufficiently mixed, take it is some be placed in open alumina crucible, Ran Houfang
In entering tube furnace.It is passed through the air that the Ar of 1000 standard milliliters/minute (sccm) is excluded in boiler tube.Then 200sccm Ar again
With 200sccm NH3In be warmed up to 1300 DEG C.NH is closed after 1300 DEG C of isothermal reaction 60min3, it is passed through the Ar of 500sccm
Room temperature is cooled to, crucible is taken out and is obtained crude product.Then by products therefrom use 3mol/L nitric acid, ultrasonic pickling 10h, after
Filter, dry, boron nitride nanosheet powder of the purity more than 99% can be obtained.Fig. 5 is the SEM of the present embodiment gained BN nanometer sheets
Figure, it can be observed that the BN nanometer sheets of flakey.Fig. 6 is the Raman collection of illustrative plates of the BNNS that the present embodiment is obtained, by 1367.9cm- 1Peak can be determined that to be hexagonal structure BN.Fig. 7 is the TEM figures of the BNNS that the present embodiment is obtained, and is clear that
The lattice fringe of BNNS, has illustrated good crystallinity, while it can be seen that about 10-18 atomic layer level thickness of nanometer sheet thickness.
Embodiment 3 is by B2O3And Li3N is with 1:1 mol ratio is sufficiently mixed, take it is some be placed in opening boron nitride crucible in, then
It is put into tube furnace, is evacuated down to 10-3Pa.Then in 300sccm NH3In be warmed up to 1300 DEG C.In 1300 DEG C of isothermal reactions
NH is closed after 60min3, the Ar for being passed through 200sccm is cooled to room temperature, takes out crucible and obtain crude product.Then products therefrom is adopted
Use 3mol/L nitric acid, ultrasonic pickling 5h to refilter, dry, boron nitride nanosheet powder of the purity more than 99% can be obtained.Fig. 8
It is the XRD of the BNNS that the present embodiment is obtained, hexagonal AlN is corresponded to completely.It can be seen that there is good crystallinity.
Embodiment 4 is by B2O3And Ca3N2With 5:2 mol ratios are sufficiently mixed, take it is some be placed in opening boron nitride crucible in, then
It is put into tube furnace, is evacuated down to 10-3Pa.Then in 300sccm NH3In be warmed up to 1300 DEG C.In 1300 DEG C of isothermal reactions
NH is closed after 120min3, the Ar for being passed through 200sccm is cooled to room temperature, takes out crucible and obtain crude product.Then by products therefrom
Using 3mol/L nitric acid, ultrasonic pickling 5h is refiltered, dried, and can obtain boron nitride nanosheet powder of the purity more than 99%.
Embodiment 5 is by B2O3And Mg3N2With 3:1 mol ratio is sufficiently mixed, take it is some be placed in opening boron nitride crucible in, then
It is put into tube furnace, is evacuated down to 10-3Pa.Then in 300sccm NH3In be warmed up to 1400 DEG C.In 1400 DEG C of isothermal reactions
NH is closed after 120min3, the Ar for being passed through 200sccm is cooled to room temperature, takes out crucible and obtain crude product.Then by products therefrom
Using 3mol/L nitric acid, ultrasonic pickling 5h is refiltered, dried, and can obtain boron nitride nanosheet powder of the purity more than 99%.
Fig. 9 is the photo in kind of the BNNS that the present embodiment is obtained.
Embodiment 6 is by B2O3And Mg3N2With 5:2 mol ratios are sufficiently mixed, take it is some be placed in opening boron nitride crucible in, then
It is put into tube furnace, is evacuated down to 10-3Pa.Then in 300sccm NH3In be warmed up to 1500 DEG C.In 1500 DEG C of isothermal reactions
NH is closed after 60min3, the Ar for being passed through 200sccm is cooled to room temperature, takes out crucible and obtain crude product.Then products therefrom is adopted
Use 3mol/L nitric acid, ultrasonic pickling 6h to refilter, dry, boron nitride nanosheet powder of the purity more than 99% can be obtained.
Embodiment 7 is by B2O3And Mg3N2With 2:1 mol ratio is sufficiently mixed, take it is some be placed in opening alumina crucible in, then
It is put into tube furnace, after excluding the air in boiler tube with Ar, in 300sccm NH3In be warmed up to 1200 DEG C.In 1200 DEG C of constant temperature
NH is closed after reaction 60min3, the Ar for being passed through 200sccm is cooled to room temperature, takes out crucible and obtain crude product.Then gained is produced
Thing uses 3mol/L nitric acid, ultrasonic pickling 5h to refilter, dry, and can obtain boron nitride nanosheet powder of the purity more than 99%
Body.
Embodiment 8 is by B2O3And Mg3N2With 1:1 mol ratio is sufficiently mixed, take it is some be placed in opening alumina crucible in, then
It is put into tube furnace, after excluding the air in boiler tube with Ar, in 300sccm NH3In be warmed up to 1100 DEG C.In 1100 DEG C of constant temperature
NH is closed after reaction 180min3, the Ar for being passed through 200sccm is cooled to room temperature, takes out crucible and obtain crude product.Then by gained
Product uses 3mol/L nitric acid, ultrasonic pickling 5h to refilter, dry, and can obtain powder shaped boron nitride nanosheet.
It should be appreciated that above-described embodiment is only explanation technology design of the invention and feature, technique is familiar with its object is to allow
Personage will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention.It is all smart according to the present invention
The equivalent change or modification that refreshing essence is made, should all be included within the scope of the present invention.
Claims (10)
1. a kind of boron nitride nanosheet powder magnanimity preparation method, it is characterised in that including：Boron source and nitrogen source predecessor are fully mixed
Close, 1100~1500 DEG C be heated in nitrogenous reaction atmosphere and more than 0.5h is incubated, be cooled to room temperature in protective atmosphere afterwards,
Crude product is obtained, then the crude product is post-processed, obtain the boron nitride nanosheet powder.
2. boron nitride nanosheet powder magnanimity preparation method according to claim 1, it is characterised in that：The boron source with it is described
The mol ratio of nitrogen source predecessor is 10:1~1:10.
3. boron nitride nanosheet powder magnanimity preparation method according to claim 1 and 2, it is characterised in that：Before the boron source
Driving thing includes boron oxide；And/or, the nitrogen source predecessor includes metal nitride.
4. boron nitride nanosheet powder magnanimity preparation method according to claim 3, it is characterised in that：The metal nitride
Including any one in magnesium nitride, lithium nitride, CaCl2 or two or more combinations.
5. boron nitride nanosheet powder magnanimity preparation method according to claim 1, it is characterised in that including：By boron source and nitrogen
Source predecessor is sufficiently mixed, and 1200~1300 DEG C and 0.5~4h of insulation are heated in nitrogenous reaction atmosphere.
6. boron nitride nanosheet powder magnanimity preparation method according to claim 1, it is characterised in that：The reaction atmosphere is
The mixed atmosphere of at least one formation in ammonia atmosphere or ammonia and nitrogen and argon gas；And/or, the protective atmosphere be nitrogen and/
Or argon gas atmosphere.
7. boron nitride nanosheet powder magnanimity preparation method according to claim 1, it is characterised in that：Described post processing bag
Include：By the crude product pickling, filtering, dry, so as to obtain the boron nitride nanosheet powder.
8. boron nitride nanosheet powder magnanimity preparation method according to claim 7, it is characterised in that：Described post processing bag
Include：With concentration be by the crude product 1~3mol/L acid solution wash after, filtering, then in 60~80 DEG C of 6~12h of drying,
Obtain the boron nitride nanosheet powder.
9. a kind of boron nitride nanosheet powder, its purity is more than 99%, and wherein boron nitride nanosheet is hexagonal nanometer boron nitride
Piece, the thickness of the hexagonal boron nitride nanosheet is 1~20 atomic layer, and radial dimension is 1~20 μm.
10. boron nitride nanosheet powder as claimed in claim 9, it is characterised in that：The thickness of the hexagonal boron nitride nanosheet is
1~10 atomic layer, radial dimension is 1~10 μm.
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Cited By (9)
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| CN107572490A (en) * | 2017-09-11 | 2018-01-12 | 河北工业大学 | A kind of preparation method of controlledly synthesis boron nitride nanosheet |
| CN107686098A (en) * | 2017-08-07 | 2018-02-13 | 武汉理工大学 | Controllable hexagonal boron nitride nanosheet of a kind of number of plies and preparation method thereof |
| CN108394915A (en) * | 2018-06-07 | 2018-08-14 | 苏州大学张家港工业技术研究院 | A kind of preparation method of ultrathin boron nitride nanosheet |
| CN108609588A (en) * | 2018-05-13 | 2018-10-02 | 王子韩 | A kind of preparation method of regular hexagonal hexagonal boron nitride nanosheet |
| 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 |
| CN110817814A (en) * | 2019-12-06 | 2020-02-21 | 桂林理工大学 | Preparation method and product of thin-wall BN micro-tube with one-dimensional hierarchical structure |
| 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 |
| CN114751387A (en) * | 2022-04-11 | 2022-07-15 | 山东大学 | Method for efficiently preparing boron nitride nanosheet |
| CN115259111A (en) * | 2022-05-09 | 2022-11-01 | 上海交通大学 | Preparation method of boron nitride nanotube |
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