CN107641789A - Boron nitride nanosheet continuous film, its preparation method and application - Google Patents
Boron nitride nanosheet continuous film, its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of boron nitride nanosheet continuous film, its preparation method and application.The preparation method includes：Precursor film is covered in substrate, afterwards in nitrogenous reaction atmosphere pyroreaction, the boron nitride nanosheet continuous film is made；The precursor film includes at least three kinds of elements, and two kinds of elements therein are respectively boron, oxygen element, the combination of any one or more of remaining element in lithium, beryllium, magnesium, calcium, strontium, barium, aluminium, gallium, indium, zinc, titanium and silicon.The preparation method of the present invention can synthesize the continuous nanometer sheet of boron nitride (i.e. boron nitride nanosheet continuous film) directly in the substrates such as Si, participation without metallic catalyst, without any transfering process, technique is simply controllable, cost is cheap, and the boron nitride nanosheet continuous film obtained can be directly as the growth substrate of the two-dimension nano materials such as graphene, and then is beneficial to substrate and/or grid of structure graphene device etc., with huge application prospect, batch production can be realized.
Description
Technical field
The present invention relates to a kind of nano film material, more particularly to a kind of boron nitride nanosheet continuous film and its preparation side
Method and application, belong to technical field of inorganic nanometer material.
Background technology
Graphene causes the extensive concern of global scientist as the two dimensional crystal material found earliest.Because it has
High carrier mobility, the performance such as chemical inertness is good, mechanical strength is high, in electronic device, the energy, composite, biology doctor
The fields such as medicine have huge application prospect.Especially, graphene can be widely used in semicon industry, break through device size
The limitation of the limit is expected to replace silicon materials.But the graphene actually synthesized, the performance of theoretical prediction is extremely difficult to, such as
Carrier mobility is relatively low etc..Reason is, on the one hand the graphene crystalline size of synthesis is too small, the number of plies is on the high side or defect too
It is more etc.；On the other hand, graphene is processed into device, it is necessary to invest backing material use, and between backing material and graphene
Lattice mismatch so that graphene can not play itself advantage very well.
Boron nitride nanosheet (BNNS) has the hexatomic ring planar structure similar to graphene, and lattice constant and graphene are most
For matching, it is referred to as " white graphite alkene ".And BNNS has excellent electrical insulating property, high thermal conductivity factor and good chemistry
Inertia, high temperature resistant, antioxygenic property more feature, suffer from being widely applied prospect in numerous areas, applied to semiconductor row
The graphene of high quality can be gone out during industry as substrate growth, so as to give play to graphene optimal performance.Except graphene, transition gold
The performance for belonging to the two-dimensional materials such as disulphide, black phosphorus plays, it is also desirable to BN backing materials.
At present, synthesize boron nitride (BN) nanometer sheet method be mainly chemical vapour deposition technique, these methods dependent on copper,
The BN nanometer sheets of the catalytic action synthesis of the metallic substrates such as nickel, ruthenium are grown on metal substrate surface, it is necessary to are transferred in silicon base
Device can just be made.In addition, also there is researcher to synthesize boron nitride nanosheet on a silicon substrate, but this method still needs
Silicon substrate bottom sediments layer of metal is as catalyst, with the presence of metal between silicon base and boron nitride nanosheet after having grown, not
Directly it can be used in the devices together with silicon chip.
The content of the invention
It is a primary object of the present invention to provide a kind of boron nitride nanosheet continuous film, its preparation method and application, with
Overcome deficiency of the prior art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
The embodiments of the invention provide a kind of preparation method of boron nitride nanosheet continuous film, it includes：In substrate
Precursor film is covered, is heated to 1000~1400 DEG C and insulation reaction in nitrogenous reaction atmosphere afterwards, the nitridation is made
Boron nanometer sheet continuous film；The precursor film includes at least three kinds of elements, and two kinds of elements therein are respectively boron, oxygen member
Element, any one or two or more group of remaining element in lithium, beryllium, magnesium, calcium, strontium, barium, aluminium, gallium, indium, zinc, titanium and silicon
Close.
A kind of boron nitride nanosheet continuous film prepared by foregoing any method is additionally provided in the embodiment of the present invention,
It is formed by the hexagonal boron nitride nanosheet monocrystalline aggregation that size is 1~50 μm, and thickness is between 1~100 atomic layer.
The purposes of the boron nitride nanosheet continuous film is additionally provided in the embodiment of the present invention.
Compared with prior art, the preparation method of boron nitride nanosheet continuous film provided by the invention can be directly in base
The continuous nanometer sheet of boron nitride (i.e. boron nitride nanosheet continuous film) is synthesized on bottom (such as silicon base), without metallic catalyst
Participate in, without any transfering process, technique is simply controllable, and cost is cheap, and the boron nitride nanosheet continuous film obtained
Can be directly as the growth substrate of the two-dimension nano materials such as graphene, and then it is beneficial to the substrate and/or grid of structure graphene device
Pole etc., there is huge application prospect, batch production can be realized.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, the embodiment of the present invention is entered below
Row describes in detail.What embodiments of the present invention were merely exemplary, and the present invention is not limited to these embodiments.
A kind of preparation method for boron nitride nanosheet continuous film that the one side of the embodiment of the present invention provides includes：
Precursor film is covered in substrate, is heated to 1000~1400 DEG C and insulation reaction in nitrogenous reaction atmosphere afterwards, institute is made
State boron nitride nanosheet continuous film.
Wherein, the precursor film includes at least three kinds of elements, and two kinds of elements therein are respectively boron, oxygen element, its
Remaining element is selected from lithium (Li), beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Si), barium (Ba), aluminium (Al), gallium (Gai), indium (In), zinc
(Zn), any one in titanium (Ti) and silicon (Si) or two or more combinations.
Further, the composition of the precursor film can be expressed as (MxOy)m·(B2O3)n, wherein m/n is 1:10~
1000:1, if M is monovalent metallic ion (such as lithium etc.), x=2y, and if M be bivalent metal ion (such as beryllium, magnesium, calcium,
Strontium, barium, zinc etc.), then x=y, if M is trivalent metal ion (such as aluminium, gallium, indium, titanium etc.), 2y=3x, if M is the silicon of tetravalence
Ion, then y=2x.
More preferable, the precursor film is formed directly into the substrate surface.
In some preferred embodiments, the predecessor that the precursor film includes is (Al2O3)m·(B2O3)n, wherein
M/n is 1:1~1000:1.
In some preferred embodiments, the predecessor that the precursor film includes is (SiO2)m·(B2O3)n, wherein
M/n is 1:1~1000:1..
In some more specific case study on implementation, the preparation method includes：
(1) one layer of precursor film is deposited in substrate；
(2) containing ammonia and or the atmosphere of nitrogen under carry out pyroreaction, it is continuously thin to obtain the boron nitride nanosheet
Film.
As one of more preferable case study on implementation, the preparation side includes：Using magnetron sputtering method, deposited in substrate
One layer of BxSi1-xO precursor films, thickness is in 1-500nm；Then pyroreaction is carried out under the atmosphere containing ammonia, obtains institute
State boron nitride nanosheet continuous film.
In some preferred embodiments, described preparation method includes：The precursor film is covered in substrate, it
More than 1000~1400 DEG C and insulation reaction 10min, such as 10min~300min are heated in nitrogenous reaction atmosphere afterwards, from
And form the boron nitride nanosheet continuous film in the substrate surface.
In some preferred embodiments, described preparation method includes：Covered in substrate (such as silicon base) described
Precursor film, 1000~1400 DEG C and insulation reaction are heated in nitrogenous reaction atmosphere afterwards, so as in the substrate table
Face forms the boron nitride nanosheet continuous film, and forms metal in the substrate and boron nitride nanosheet continuous film
The insulating medium layer such as oxide skin(coating) or silicon oxide layer, so not only without prejudice to being even advantageous to the design and making of subsequent device.
In these foregoing embodiments, representative reaction equation is as follows：
(Al2O3)m·(B2O3)n+2nNH3---mAl2O3+2nBN+3nH2O
(SiO2)m·(B2O3)n+2nNH3---mSiO2+2nBN+3nH2O。
In some embodiments, described preparation method includes：Using magnetron sputtering, electron beam evaporation plating, hot evaporation, arteries and veins
At least one of impulse light deposition, molecular beam epitaxy and ald mode in the substrate surface deposit to be formed it is described before
Drive thing film.
More preferable, the thickness of the precursor film is 1~500nm.
Wherein, the nitrogenous reaction atmosphere is selected from what ammonia and/or nitrogen or ammonia and/or nitrogen were formed with diluent gas
Mixed atmosphere, the diluent gas include inert gas (such as argon gas), but not limited to this.
Wherein, the substrate includes silicon (Si) substrate or silica (Si/SiO2) substrate.
It is more preferable, non-metal catalyst layer between the boron nitride nanosheet continuous film and substrate.
Further, the boron nitride nanosheet continuous film is directly grown in the substrate surface.
The other side of the embodiment of the present invention additionally provides the boron nitride nanosheet prepared by foregoing any method and connected
Continuous film, it is assembled (similar polycrystal splices form, there is crystal boundary) by the hexagonal boron nitride nanosheet monocrystalline that size is 1~50 μm
Form, thickness is between 1~100 atomic layer.
The other side of the embodiment of the present invention additionally provides the boron nitride nanosheet prepared by foregoing any method and connected
The purposes of continuous film, such as preparing two-dimension nano materials or comprising the purposes in the device of two-dimension nano materials.
Wherein, the two-dimension nano materials include graphene.
In some case study on implementation, the boron nitride nanosheet continuous film can be directly synthesized on a silicon substrate, without
Any transfering process.And the boron nitride nanosheet continuous film can form graphite directly as the substrate of graphene growth
The substrate and/or grid of alkene device, technique is simply controllable, there is huge application prospect in terms of graphene device, can realize
Batch production.
Below in conjunction with some embodiments the technical solution of the present invention is further explained explanation.
Embodiment 1：Using magnetron sputtering method, in the thick Al of silicon substrate bottom sediments about 100nm18O4O33(i.e. 9Al2O3·2B2O3)
Film, it is then placed in tube furnace, the air passed first into the Ar exclusion boiler tubes of 1000 standard milliliters/minute (sccm), so
Afterwards in 200sccm Ar and 200sccm NH3NH is closed after 1300 DEG C and isothermal reaction 4h are warming up in atmosphere3, finally it is passed through
500sccm Ar is cooled to room temperature, the boron nitride nanosheet continuous film of die size is made, to this in a manner of infrared, Raman etc.
Boron nitride nanosheet continuous film is analyzed, and as a result turns out to be boron nitride.Again to the boron nitride nanosheet in a manner of TEM, SEM etc.
Continuous film is observed, and is formed it can be found that it is assembled by the hexagonal boron nitride nanosheet monocrystalline that size is 1~50 μm, thickness is situated between
In 1~100 atomic layer.
Embodiment 2：Using e-beam evaporation, in the SiO of B doping thick 4 inches of silicon substrate bottom sediments about 500nm2It is thin
Film (wherein B doping is 5at%), is then placed in tube furnace and is evacuated to 10-3Pa, then in 200sccm Ar and
200sccm NH3NH is closed after 1100 DEG C and isothermal reaction 2h are warming up in atmosphere3, the Ar for being finally passed through 500sccm is cooled to room
Temperature, the boron nitride nanosheet continuous film that length and width dimensions are 4 inches is made.
Embodiment 3：Using e-beam evaporation, silicon substrate bottom sediments 200nm Ca3B2O6(i.e. 3CaOB2O3) film, then
It is put into tube furnace, is evacuated down to 10-3Pa.Then in 300sccm NH3In be warming up to 1400 DEG C and isothermal reaction 1h after close
NH3, the Ar for being finally passed through 200sccm is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 4：Using e-beam evaporation, silicon substrate bottom sediments 200nm Mg3B2O6(i.e. 3MgOB2O3) film, then
It is put into tube furnace, is evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1300 DEG C and isothermal reaction 1h after close
NH3, the Ar for being finally passed through 200sccm is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 5：Using e-beam evaporation, silicon substrate bottom sediments 100nm ZnB4O7Film, it is then placed in tube furnace,
It is evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1300 DEG C and isothermal reaction 1h after close NH3, finally it is passed through
200sccm Ar is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 6：Using e-beam evaporation, silicon substrate bottom sediments 200nm Li2B4O7Film, it is then placed in tube furnace,
It is evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1200 DEG C and isothermal reaction 1h after close NH3, finally it is passed through
200sccm Ar is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 7：Using e-beam evaporation, silicon substrate bottom sediments 200nm GaBO3(i.e. Ga2O3·B2O3) film, then
It is put into tube furnace, is evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1250 DEG C and isothermal reaction 1h after close
NH3, the Ar for being finally passed through 200sccm is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 8：Using e-beam evaporation, silicon substrate bottom sediments 300nm InBO3(i.e. In2O3·B2O3) film, then
It is put into tube furnace, is evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1200 DEG C and isothermal reaction 1h after close
NH3, the Ar for being finally passed through 200sccm is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 9：Using e-beam evaporation, silicon substrate bottom sediments 200nm H2BeB4O8Film, it is then placed in tube furnace
In, it is evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1200 DEG C and isothermal reaction 1h after close NH3, finally lead to
The Ar for entering 200sccm is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 10：Using e-beam evaporation, silicon substrate bottom sediments 100nm Ba3B2O6(i.e. 3BaOB2O3) film, so
After be put into tube furnace, be evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1250 DEG C and isothermal reaction 1h after close
Close NH3, the Ar for being finally passed through 200sccm is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 11：Using e-beam evaporation, silicon substrate bottom sediments 100nm Sr3B2O6(i.e. 3SrOB2O3) film, so
After be put into tube furnace, be evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1300 DEG C and isothermal reaction 1h after close
Close NH3, the Ar for being finally passed through 200sccm is cooled to room temperature, and the boron nitride nanosheet continuous film of die size is made.
Embodiment 12：Using e-beam evaporation, silicon substrate bottom sediments 200nm TiBO3(i.e. Ti2O3·B2O3) film, then
It is put into tube furnace, is evacuated down to 10-3Pa, then in 300sccm NH3In be warming up to 1400 DEG C and isothermal reaction 1h after close
NH3, the Ar for being finally passed through 200sccm is cooled to room temperature, and the boron nitride nanosheet continuous film of die size 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 (10)
- A kind of 1. preparation method of boron nitride nanosheet continuous film, it is characterised in that including：It is thin that predecessor is covered in substrate Film, 1000~1400 DEG C and insulation reaction are heated in nitrogenous reaction atmosphere afterwards, it is continuous that the boron nitride nanosheet is made Film；The precursor film includes at least three kinds of elements, and two kinds of elements therein are respectively boron, oxygen element, and remaining element selects From any one in lithium, beryllium, magnesium, calcium, strontium, barium, aluminium, gallium, indium, zinc, titanium and silicon or two or more combinations.
- 2. preparation method according to claim 1, it is characterised in that：The precursor film is formed directly into the substrate Surface.
- 3. preparation method according to claim 1, it is characterised in that：The composition for the predecessor that the precursor film includes For (MxOy)m·(B2O3)n, wherein M in lithium, beryllium, magnesium, calcium, strontium, barium, aluminium, gallium, indium, zinc, titanium and silicon any one or Two or more combinations, m/n=1:10~1000:1, if M is monovalent metallic ion, x=2y, if M is bivalent metal ion, Then x=y, if M is trivalent metal ion, 2y=3x, if M is tetravalence Si ions, y=2x.
- 4. the preparation method according to claim 1 or 3, it is characterised in that including：It is thin that the predecessor is covered in substrate Film, 1000~1400 DEG C and insulation reaction are heated in nitrogenous reaction atmosphere afterwards, so as to form institute in the substrate surface Boron nitride nanosheet continuous film is stated, and metal oxide layer is formed in the substrate and boron nitride nanosheet continuous film Or silicon oxide layer.
- 5. preparation method according to claim 1, it is characterised in that including：Steamed using magnetron sputtering, electron beam evaporation plating, heat At least one of plating, pulsed laser deposition, molecular beam epitaxy and ald mode deposits to be formed in the substrate surface The precursor film.
- 6. preparation method according to claim 1, it is characterised in that：The thickness of the precursor film is 1~500nm.
- 7. preparation method according to claim 1, it is characterised in that：The nitrogenous reaction atmosphere is selected from ammonia and/or nitrogen The mixed atmosphere that gas or ammonia and/or nitrogen are formed with diluent gas, the diluent gas include inert gas；It is and/or described Substrate includes silicon base or oxidation silicon base.
- 8. preparation method according to claim 1, it is characterised in that：The boron nitride nanosheet continuous film and substrate it Between non-metal catalyst layer.
- 9. boron nitride nanosheet continuous film prepared by the method as any one of claim 1-8, it is 1~50 by size μm hexagonal boron nitride nanosheet monocrystalline aggregation form, thickness is between 1~100 atomic layer.
- 10. boron nitride nanosheet continuous film described in claim 9 is in preparing two-dimension nano materials or comprising two-dimension nano materials Device in purposes, the two-dimension nano materials include graphene or transition metal dichalcogenide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610584210.9A CN107641789B (en) | 2016-07-22 | 2016-07-22 | Boron nitride nanosheet continuous film, and preparation method and application thereof |
| AU2016415516A AU2016415516A1 (en) | 2016-07-22 | 2016-12-16 | Boron nitride nanomaterial, and preparation method and use thereof |
| PCT/CN2016/110420 WO2018014494A1 (en) | 2016-07-22 | 2016-12-16 | Boron nitride nanomaterial, and manufacturing method and application thereof |
| JP2018567595A JP6657429B2 (en) | 2016-07-22 | 2016-12-16 | Method for producing boron nitride nanomaterial |
| US16/306,758 US20190127222A1 (en) | 2016-07-22 | 2016-12-16 | Boron Nitride Nanomaterial, and Preparation Method and Use Thereof |
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| CN117900467A (en) * | 2024-03-19 | 2024-04-19 | 天津大学 | Boron nitride nanosheets and preparation method thereof |
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