CN110510604A - A kind of graphene/boron nitride stratiform heterojunction structure and preparation method thereof - Google Patents
A kind of graphene/boron nitride stratiform heterojunction structure and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to field of inorganic nano material, and in particular to a kind of graphene/boron nitride stratiform heterojunction structure and preparation method thereof.The composite heterogenous junction structure that the program proposes, graphene surface are covered by boron nitride, and lateral length is 30~80 μm.Stable dispersions are formed through processing the described method includes: sequentially adding dispersing agent and graphene in deionized water, adding boron oxide, constant temperature is stirred to thick muddy at a certain temperature, is coated on corundum boat surface, is obtained presoma after vacuum drying；It places it in vacuum tube furnace, is passed through ammonia again after continuous heating to certain temperature in argon atmosphere and is reacted to obtain primary product, layered heterogeneous structure material can be obtained after processing.Present invention process is simple, is not required to any metallic catalyst, and material purity height, good crystallinity have gathered the excellent properties of both graphene and boron nitride, provided technical solution for two-dimensional material industrialized production.
Description
Technical field
The present invention relates to two-dimension nano materials preparation technical fields, and in particular to a kind of graphene/boron nitride laminated hetero
Structure and preparation method thereof.
Background technique
Recently as the successful preparation of the two-dimension nano materials such as graphene and its constantly discovering for various aspects excellent properties,
Stratified nano materials are increasingly becoming the hot spot of research.In these materials, graphene and two-dimentional boron nitride nanostructure occupy act
The status of sufficient weight.
Graphene is a kind of typical two-dimensional material, and atom is bound to each other to form the honeycomb crystal lattice of monoatomic layer, tool
There is high electron mobility that it is made to have extensive potential using value in electronic device, interaction has more by force in layer
Good mechanical property additionally has high conductivity, the advantages characteristics such as high heat conductance.The dilute peculiar property of graphite also causes
The interest of the stratified material of people's structure dilute for class graphite.Two-dimensional hexagonal boron nitride nanosheet is similar with graphene-structured, phase
Equal number of electronics is shared between adjacent atom, is combined between lamella by Van der Waals force, except with knot similar with graphene
Structure feature and physical property, such as high-intensitive, high thermal conductivity, high temperature resistant etc., also with anti-oxidant, band gap is wide, thermal expansion coefficient is low, changes
Learn the advantageous properties such as high stability, neutron irradiation shielding, super-hydrophobic, piezoelectric property and good biocompatibility.Therefore, hexagonal
Boron nitride nanosheet gradually occupies status finally in fields such as high-strength functional composite material, biomedicines, has wide
Application prospect.By graphene and boron nitride nanometer material perfect combination, using the two characteristic enhancing with it is complementary, will open more
The gate of application field, such as heat transfer, digital switch field will show bigger practical advantages.Therefore, graphene/boron nitride
The controllable preparation and mass production of composite material become the important research direction of nanometer material science.
Existing technical solution is usually to prepare graphene and boron nitride using substep, is then transferred to corresponding substrate table
Face is compound come what is both realized, and solvent or transfer agent used in transfer process are easy to cause graphene and boron nitride interface
Pollution, and then the performances such as electricity, optics for influencing composite material.Also there is portion of techniques scheme that high thermal decomposition is added in predecessor
It is also easy to produce the melamine of hypertoxic cyanide, preparation process complexity is difficult to control, will cause centainly to environment and operator
Harm.In conclusion seeking one kind under the premise of how as much as possible retaining graphene and the respective excellent attribute of boron nitride
Simple and effective, environmental-friendly preparation method is come to obtain graphene/boron nitride heterojunction structure be urgently to be resolved at present key
Technical problem.
Summary of the invention
In view of this, present invention aims to overcome that deficiency existing for prior art scheme, provides a kind of graphene/nitridation
Boron layer shape heterojunction structure and preparation method thereof.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of graphene/boron nitride stratiform heterojunction structures, cover graphene with two-dimensional layer boron nitride,
Form graphene/boron nitride MULTILAYER COMPOSITE heterojunction structure of atomic-level thickness.
Preferably, the graphene/boron nitride MULTILAYER COMPOSITE heterojunction structure lateral length is 50~70 μm.
The present invention provides above-mentioned graphene/boron nitride stratiform heterojunction structure preparation methods, comprising the following steps:
(1) it prepares presoma: sequentially adding dispersing agent and graphene in deionized water, after the processing of ultrasonic magnetic agitation
Stable dispersions are formed, boron oxide is added, constant temperature is stirred to thick muddy at a certain temperature, is coated on corundum boat table
Face obtains presoma after vacuum drying；
(2) presoma obtained by step (1) graphene/boron nitride stratiform heterojunction structure preparation and purification: is placed in vacuum
In tube furnace, it is passed through ammonia again after continuous heating to certain temperature in argon atmosphere and is reacted, room is then naturally cooled to
Temperature, obtains primary product, and graphene/boron nitride stratiform heterojunction structure can be obtained after processing.
Preferably, dispersing agent is lauryl sodium sulfate in the step (1), and dispersant concentration is 1~2mg/ml.
Preferably, the mass ratio of graphene and dispersing agent is 1:2~4 in the step (1).
Preferably, in the step (1) magnetic agitation time be 12~for 24 hours.
Preferably, sonication treatment time is 3~10h in the step (1).
Preferably, graphene and boron oxide mass ratio are 1:18.5~50 in the step (1).
Preferably, the assigned temperature of magnetic agitation is 80 DEG C in the step (1).
Preferably, drying temperature is 60 DEG C in the step (1), drying time 12h.
Preferably, tube furnace with the heating rate of 5 DEG C/min rises to 800~1300 DEG C in the step (2), the reaction time
2~6h.
Preferably, the rate that is passed through of argon gas is 200~300ml/min in the step (2), and the rate that is passed through of ammonia is 20
~80ml/min.
Preferably, the processing of the primary product of the step (2) are as follows: with deionized water washed product 3~5 times of 80 DEG C,
Until pH value is 7, obtained solid powder is placed in 60 DEG C of dry 12h in vacuum oven.
Compared with the existing technology, beneficial effects of the present invention: (1) technical solution provided by the invention can be directly in graphite
The surface of alkene thin layer uniformly and stably covers single layer or multilayer two-dimension layered nitride boron nano flake, obtains atomic-level thickness
Graphene/boron nitride stratiform heterojunction structure, avoid the breakage occurred in previous graphene transfer process and transfer agent or
The pollution of surface and interface caused by solvent.(2) present invention utilizes ten using the mixture of graphene and boron oxide as presoma
Sodium dialkyl sulfate is dispersing agent, and using argon gas as carrier gas, for ammonia as reaction gas, preparation method is simple, is not necessarily to high compression ring
Border, it is low for equipment requirements, it is easy to accomplish industrialization；Chemical reaction reagent used is cheap and easy to get, and either forerunner's drug is with after
Phase product is all environmentally friendly.(3) graphene of atomic-level thickness prepared by the present invention/boron nitride stratiform heterojunction structure is shown
Higher stability and excellent physicochemical characteristic, and repeatability is good, in the great application prospect in two-dimensional functional material field.
Detailed description of the invention
Fig. 1 is graphene/boron nitride stratiform heterojunction structure Raman map prepared by embodiment 1.
Fig. 2 is graphene/boron nitride stratiform heterojunction structure transmission electron microscope picture prepared by embodiment 1.
Fig. 3 is graphene/boron nitride stratiform heterojunction structure transmission electron microscope High-Resolution Map prepared by embodiment 1
Picture.
Fig. 4 is graphene/boron nitride stratiform heterojunction structure transmission electron microscope High-Resolution Map prepared by embodiment 1
Picture.
Specific embodiment
Below with reference to embodiment, the present invention is described in more detail, but protection scope of the present invention is not limited only to these realities
Apply example.
Embodiment 1
It weighs 20mg lauryl sodium sulfate to be dissolved in 10ml deionized water, forms solution for standby；Weigh 10mg graphene
Ultrasound 3h after above-mentioned solution magnetic agitation 12h is added, is formed and stablizes graphene dispersing solution；Again by 230mg boron oxide at 80 DEG C
It is added in above-mentioned dispersion liquid, corundum boat surface is evenly applied to after temperature constant magnetic stirring to thick muddy in 60 DEG C of drying 12h
It is spare；It dried corundum boat is placed in tube furnace is passed through the protection of 250ml/min argon gas and risen to the heating rate of 5 DEG C/min
1200 DEG C of ammonias heat preservation 3h for being passed through 50ml/min are taken out after reaction substance and are washed with 80 DEG C of hot water to pH value close to 7, to its into
Row filtration drying obtains graphene/boron nitride stratiform heterojunction structure.
Fig. 1 is prepared graphene/boron nitride stratiform heterojunction structure raman spectrum, is gone out in figure in 1345 or so position
Showed boron nitride typical case's Raman peak position, be superimposed with the peak graphene D make herein peak value it is obvious compared to typical graphite alkene peak strength
Enhancing.In addition there are also the peak the G peak position of graphene and the short graphene 2D characteristic peaks to broaden of change.Product is graphite as shown in Figure 1
Alkene nitrogenizes boron compound.Fig. 2 is prepared graphene/boron nitride stratiform heterojunction structure transmission electron microscope image, reaction
The stratiform pattern of prepared product.
Embodiment 2
In embodiment 1, reaction temperature becomes 1000 DEG C from 1200 DEG C, other steps are same as Example 1, and class can be obtained
Graphene/boron nitride stratiform the heterojunction structure being similar in embodiment 1.Fig. 3 is prepared graphene/boron nitride stratiform heterojunction structure
Transmission electron microscope High-Resolution Map, can be clearly seen that two-phase product the distribution of respective lattice and apparent stratiform knot
Structure.
Embodiment 3
In embodiment 1, the quality of graphene and boron oxide increases separately as 20mg and 460mg, other steps and implements
Example 1 is identical, can still obtain the graphene/boron nitride stratiform heterojunction structure being similar in embodiment 1.Fig. 4 be prepared graphene/
The transmission electron microscope High-Resolution Map of boron nitride stratiform heterojunction structure, it can be seen that the overlapping appearance structure of stratiform and obvious crystalline substance
Lattice distribution.
Embodiment 4
In embodiment 1, the reaction time becomes 5h from 3h, other steps are same as Example 1, can obtain being similar to and implement
Graphene/boron nitride stratiform heterojunction structure in example 1.
Embodiment 5
In embodiment 1, argon flow is changed to 300ml/min, and ammonia flow is changed to 30ml/min, other steps and implementation
Example 1 is identical, and similar graphene/boron nitride stratiform heterojunction structure can be obtained.
Embodiment 6
In embodiment 1, ultrasonic time becomes 6h from 3h, other steps are same as Example 1, can obtain being similar to and implement
Graphene/boron nitride stratiform heterojunction structure in example 1.
Comparative example 1
In embodiment 1, boron oxide quality individually increases 1000mg, and other conditions remain unchanged, operating procedure and implementation
Example 1 is identical, is unable to get above-mentioned graphene/boron nitride stratiform heterojunction structure.
Comparative example 2
In embodiment 1, ammonia flow is changed to 120ml/min, other steps are same as Example 1, is unable to get similar
Graphene/boron nitride stratiform heterojunction structure.
Comparative example 3
In embodiment 1, reaction temperature becomes 1400 DEG C from 1200 DEG C, other steps are same as Example 1, is unable to get
Similar graphene/boron nitride stratiform heterojunction structure.
Comparative example 4
In embodiment 1, the reaction time is changed to 1h by 3h, other steps are same as Example 1, is unable to get similar graphite
Alkene/boron nitride stratiform heterojunction structure.
The present invention provides the graphene of a kind of atomic-level thickness/boron nitride stratiform heterojunction structures and preparation method thereof, and
It is not limited only to the operation of specific experiment described in specification and embodiments.Therefore it is all according to described in scope of the present invention patent
The equivalence changes/variation made of predecessor, operating process and principle or sequence change, should be included in the guarantor of the invention patent
It protects in range.
Claims (10)
1. a kind of graphene/boron nitride stratiform heterojunction structure, which is characterized in that graphene surface is covered by boron nitride in the structure
Lid, forms a kind of graphene/boron nitride MULTILAYER COMPOSITE heterojunction structure of atomic-level thickness, and lateral length is 30~80 μm.
2. a kind of graphene described in claim 1/boron nitride stratiform heterojunction structure preparation method, which is characterized in that including
Following steps:
(1) it prepares presoma: sequentially adding dispersing agent and graphene in deionized water, formed after the processing of ultrasonic magnetic agitation
Stable dispersions add boron oxide, and constant temperature is stirred to thick muddy at a certain temperature, are coated on corundum boat surface, very
Presoma is obtained after sky is dry；
(2) graphene/boron nitride stratiform heterojunction structure preparation and purification: the corundum boat of presoma will be housed obtained by step (1)
It is placed in vacuum tube furnace, is passed through ammonia again after continuous heating to certain temperature in argon atmosphere and is reacted, it is then natural
It is cooled to room temperature, obtains primary product, graphene/boron nitride stratiform heterojunction structure can be obtained after processing.
3. graphene according to claim 2/boron nitride stratiform heterojunction structure preparation method, which is characterized in that described
Dispersing agent in step (1) is lauryl sodium sulfate, and dispersant concentration is 0.05~2mg/ml, the graphene and dispersing agent
Mass ratio be 1:0.05~4.
4. graphene according to claim 2/boron nitride stratiform heterojunction structure preparation method, which is characterized in that described
The time of magnetic agitation described in step (1) be 12~for 24 hours, sonication treatment time be 1~10h.
5. graphene according to claim 2/boron nitride stratiform heterojunction structure preparation method, which is characterized in that described
Graphene and boron oxide mass ratio are 1:18.5~100 in step (1), and the assigned temperature of the magnetic agitation after boron oxide is added is
80 DEG C~100 DEG C.
6. graphene according to claim 2/boron nitride stratiform heterojunction structure preparation method, which is characterized in that described
Vacuum drying temperature is 60 DEG C in step (1), drying time 12h.
7. graphene according to claim 2/boron nitride stratiform heterojunction structure preparation method, which is characterized in that described
Tube furnace rises to 600~1300 DEG C with the heating rate of 5 DEG C/min in step (2), 1.5~6h of reaction time.
8. graphene according to claim 2/boron nitride stratiform heterojunction structure preparation method, which is characterized in that described
The rate that is passed through of argon gas is 150~300ml/min in step (2), and the rate that is passed through of ammonia is 20~100ml/min.
9. graphene according to claim 2/boron nitride stratiform heterojunction structure preparation method, which is characterized in that described
The processing of primary product in step (2) are as follows: with 80 DEG C of deionized water washed products 3~5 times until pH value is 7, will obtain
Solid powder be placed in 60 DEG C of dry 12h in vacuum oven.
10. being made described in a kind of graphene/boron nitride stratiform heterojunction structure or claim 2~9 any one described in claim 1
Preparation Method preparation has the application of graphene/boron nitride stratiform heterogeneous structure material.
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| CN111944484A (en) * | 2020-08-04 | 2020-11-17 | 上海船舶工艺研究所(中国船舶工业集团公司第十一研究所) | Cubic boron nitride intercalated graphene non-metallic material and preparation method thereof |
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