CN108439356A - A kind of ultrathin boron nitride nanosheet and preparation method thereof - Google Patents
A kind of ultrathin boron nitride nanosheet and preparation method thereof Download PDFInfo
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- CN108439356A CN108439356A CN201810469888.1A CN201810469888A CN108439356A CN 108439356 A CN108439356 A CN 108439356A CN 201810469888 A CN201810469888 A CN 201810469888A CN 108439356 A CN108439356 A CN 108439356A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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
- C01—INORGANIC CHEMISTRY
- 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
Abstract
The present invention relates to a kind of ultrathin boron nitride nanosheets and preparation method thereof.Its technical solution is:The metal salt of the boron source of 1~15wt%, the solid-state nitrogen source of 1~15wt% and 75~95wt% is mixed, mixture is obtained;The mixture is put into corundum crucible, then the corundum crucible is placed in box atmosphere furnace, 1000~1300 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is kept the temperature, obtains intermediate product;The intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid under the conditions of 80~120 DEG C dry 8~10h to get to ultrathin boron nitride nanosheet.The present invention has the characteristics that simple for process, synthesis temperature is low, with short production cycle, yield is high, at low cost, process is easily controllable and industrialization prospect is big, and prepared ultrathin boron nitride nanosheet thickness is small, is evenly distributed and purity height.
Description
Technical field
The invention belongs to the technical fields of boron nitride nanosheet.More particularly to a kind of ultrathin boron nitride nanosheet and its preparation
Method.
Background technology
It the special performance of graphene and its is widely applied and causes people other two-dimensional materials are widely paid close attention to.Two dimension
Boron nitride nanosheet has excellent mechanical property, is visually known as " white graphite alkene " as a kind of analog of graphene.
In addition, boron nitride nanosheet has many special performances for being different from graphene, including electrical insulating property, inoxidizability, thermostabilization
Property and luminescent properties etc., these excellent performances impart the unique application that boron nitride nanosheet is different from graphene.
Compared to graphite, the active force between boron nitride layer is stronger, thus boron nitride nanosheet prepare it is more difficult.Mesh
Before, the preparation method of boron nitride nanosheet mainly has:Mechanical stripping method (Lei W, et al.Boron nitride
colloidal solutions,ultralight aerogels and freestanding membranes through
one-step exfoliation and functionalization[J].Nature communications,2015,6,
8849), liquid phase stripping method (Zhi C, et al.Large-scale fabrication of boron nitride
nanosheets and their utilization in polymeric composites with improved
Thermal and mechanical properties [J] .Advanced Materials, 2009,21,2889) and chemical gas
Phase sedimentation (Wang L, et al.Monolayer hexagonal boron nitride films with large
domain size and clean interface for enhancing the mobility of graphene‐based
Field-effect transistors [J] .Advanced Materials, 2014,26,1559) etc..These preparation methods are all
It comes with some shortcomings:As the production cycle of mechanical stripping method and liquid phase stripping method length, low yield, Product size are small;Chemical gaseous phase
It is sedimentation complex process, of high cost.These disadvantages significantly limit application and the industrialization production of boron nitride nanosheet.
Invention content
The present invention is directed to overcome the deficiencies of existing technologies, and it is an object of the present invention to provide one kind is simple for process, synthesis temperature is low, production
Period is short, yield is high and the preparation method of ultrathin boron nitride nanosheet at low cost, and the ultrathin boron nitride prepared with this method is received
Rice piece thickness is small, is evenly distributed and purity height.
To achieve the above object, the step of the technical solution adopted by the present invention is:
Step 1 mixes the metal salt of the boron source of 1~15wt%, the solid-state nitrogen source of 1~15wt% and 75~95wt%,
Up to mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1000~1300 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is one kind in Boratex, boron oxide and boric acid, and the boron source is technical pure or is that analysis is pure;It is described
Grain size≤200 μm of boron source.
The solid-state nitrogen source is one kind in melamine, azepine cytimidine and dicyanodiamine, and the solid-state nitrogen source is work
Industry is pure or pure to analyze;Grain size≤200 μm of the solid-state nitrogen source.
The metal salt is one or more of sodium chloride, potassium chloride and sodium fluoride, and the metal salt is technical pure or is
It analyzes pure;The grain size of the metal salt≤200 μm.
Due to the adoption of the above technical scheme, the present invention has following good effect and outstanding feature compared with prior art:
1, the present invention uses molten-salt growth method, provides liquid phase reactor environment, reduces synthesis temperature;The raw materials used in the present invention is come
Source is extensively and cheap, and production cost is low, has industrialization prospect.
2, the present invention is simple for process, with short production cycle and easy to operate using synthesis technology from bottom to top.
3, the present invention can accurately control technological parameter, such as raw material proportioning and reaction temperature, readily available various sizes of
Ultrathin boron nitride nanosheet, prepared ultrathin boron nitride nanosheet thickness are that 1~10nm, size uniform and purity are high.
Therefore, the present invention is with simple for process, synthesis temperature is low, with short production cycle, yield is high, at low cost, process is easy to
Control and the big feature of industrialization prospect, prepared ultrathin boron nitride nanosheet thickness is small, is evenly distributed and purity height.
Description of the drawings
Fig. 1 is a kind of XRD diagram of ultrathin boron nitride nanosheet prepared by the present invention;
Fig. 2 is the AFM figures of ultrathin boron nitride nanosheet shown in Fig. 1;
Fig. 3 is the height distribution of corresponding position in Fig. 2.
Specific implementation mode
The present invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System.
It is first that the raw material Unify legislation involved by present embodiment is as follows to avoid repeating, it is no longer superfluous in embodiment
It states:
The boron source is technical pure or is that analysis is pure;Grain size≤200 μm of the boron source.
The solid-state nitrogen source is technical pure or is that analysis is pure;Grain size≤200 μm of the solid-state nitrogen source.
The metal salt is technical pure or is that analysis is pure;The grain size of the metal salt≤200 μm.
Embodiment 1
A kind of ultrathin boron nitride nanosheet and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1 mixes the metal salt of the boron source of 1~9wt%, the solid-state nitrogen source of 1~9wt% and 90~95wt%, i.e.,
Obtain mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1100~1200 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is Boratex.
The solid-state nitrogen source is melamine.
The metal salt is the mixture of sodium chloride and potassium chloride.
Ultrathin boron nitride nanosheet prepared by the present embodiment is after testing:Thickness is 1~4nm.
Embodiment 2
A kind of ultrathin boron nitride nanosheet and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1 mixes the metal salt of the boron source of 1~9wt%, the solid-state nitrogen source of 1~9wt% and 90~95wt%, i.e.,
Obtain mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1100~1200 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is boric acid.
The solid-state nitrogen source is azepine cytimidine.
The metal salt is the mixture of sodium chloride and sodium fluoride.
Ultrathin boron nitride nanosheet prepared by the present embodiment is after testing:Thickness is 1~4nm.
Embodiment 3
A kind of ultrathin boron nitride nanosheet and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1 mixes the metal salt of the boron source of 3~11wt%, the solid-state nitrogen source of 3~11wt% and 85~90wt%,
Up to mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1200~1300 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is Boratex.
The solid-state nitrogen source is dicyanodiamine.
The metal salt is potassium chloride.
Ultrathin boron nitride nanosheet prepared by the present embodiment is after testing:Thickness is 6~10nm.
Embodiment 4
A kind of ultrathin boron nitride nanosheet and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1 mixes the metal salt of the boron source of 3~11wt%, the solid-state nitrogen source of 3~11wt% and 85~90wt%,
Up to mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1200~1300 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is boron oxide.
The solid-state nitrogen source is melamine.
The metal salt is the mixture of sodium chloride, potassium chloride and sodium fluoride.
Ultrathin boron nitride nanosheet prepared by the present embodiment is after testing:Thickness is 1~4nm.
Embodiment 5
A kind of ultrathin boron nitride nanosheet and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1 mixes the metal salt of the boron source of 5~13wt%, the solid-state nitrogen source of 5~13wt% and 80~85wt%,
Up to mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1200~1300 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is boron oxide.
The solid-state nitrogen source is azepine cytimidine.
The metal salt is the mixture of sodium chloride and potassium chloride.
Ultrathin boron nitride nanosheet prepared by the present embodiment is after testing:Thickness is 3~5nm.
Embodiment 6
A kind of ultrathin boron nitride nanosheet and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1 mixes the metal salt of the boron source of 5~13wt%, the solid-state nitrogen source of 5~13wt% and 80~85wt%,
Up to mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1200~1300 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is boric acid.
The solid-state nitrogen source is dicyanodiamine.
The metal salt is the mixture of potassium chloride and sodium fluoride.
Ultrathin boron nitride nanosheet prepared by the present embodiment is after testing:Thickness is 3~5nm.
Embodiment 7
A kind of ultrathin boron nitride nanosheet and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1 mixes the metal salt of the boron source of 7~15wt%, the solid-state nitrogen source of 7~15wt% and 75~80wt%,
Up to mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1000~1100 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is Boratex.
The solid-state nitrogen source is melamine.
The metal salt is sodium fluoride.
Ultrathin boron nitride nanosheet prepared by the present embodiment is after testing:Thickness is 6~10nm.
Embodiment 8
A kind of ultrathin boron nitride nanosheet and preparation method thereof.It is the step of preparation method described in the present embodiment:
Step 1 mixes the metal salt of the boron source of 7~15wt%, the solid-state nitrogen source of 7~15wt% and 75~80wt%,
Up to mixture.
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box
In atmosphere furnace, 1000~1100 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation.
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C
Under the conditions of dry 8~10h, ultrathin boron nitride nanosheet is made.
The boron source is boric acid.
The solid-state nitrogen source is azepine cytimidine.
The metal salt is sodium chloride.
Ultrathin boron nitride nanosheet prepared by the present embodiment is after testing:Thickness is 1~4nm.
Present embodiment has following good effect and outstanding feature compared with prior art:
1, the present invention uses molten-salt growth method, provides liquid phase reactor environment, reduces synthesis temperature;The raw materials used in the present invention is come
Source is extensively and cheap, and production cost is low, has industrialization prospect.
2, the present invention is simple for process, with short production cycle and easy to operate using synthesis technology from bottom to top.
3, the present invention can accurately control technological parameter, such as raw material proportioning and reaction temperature, readily available various sizes of
Ultrathin boron nitride nanosheet.Prepared ultrathin boron nitride nanosheet is as shown in Figure 1, Figure 2 and Figure 3, and Fig. 1 is prepared by embodiment 1
A kind of ultrathin boron nitride nanosheet XRD diagram;Fig. 2 is the AFM figures of ultrathin boron nitride nanosheet shown in Fig. 1;Fig. 3 is in Fig. 2
The height of corresponding position is distributed.As shown in Figure 1, the XRD diffraction maximums of prepared ultrathin boron nitride nanosheet correspond to spreading out for h-BN
Peak is penetrated, purity is high;As shown in Figure 2, prepared ultrathin boron nitride nanosheet thickness is small;From the figure 3, it may be seen that prepared is ultra-thin
Boron nitride nanosheet thickness is 1~4nm.
Ultrathin boron nitride nanosheet prepared by present embodiment is after testing:Pattern in the form of sheets, thickness be 1~
10nm。
Therefore, the present invention is with simple for process, synthesis temperature is low, with short production cycle, yield is high, at low cost, process is easy to
Control and the big feature of industrialization prospect, prepared ultrathin boron nitride nanosheet thickness is small, is evenly distributed and purity height.
Claims (5)
1. a kind of preparation method of ultrathin boron nitride nanosheet, it is characterised in that the step of preparation method is:
Step 1, by the metal salt of the boron source of 1~15wt%, the solid-state nitrogen source of 1~15wt% and 75~95wt% mix to get
Mixture;
Step 2, the mixture is put into corundum crucible, then the corundum crucible for being placed with the mixture is placed in box atmosphere
In stove, 1000~1300 DEG C are heated in the nitrogen atmosphere of circulation, 1~5h is to get intermediate product for heat preservation;
Step 3, the intermediate product is washed with deionized 2~5 times, is separated by solid-liquid separation, obtained solid is in 80~120 DEG C of conditions
Ultrathin boron nitride nanosheet is made in 8~10h of lower drying.
2. the preparation method of ultrathin boron nitride nanosheet according to claim 1, it is characterised in that the boron source is boric acid
One kind in sodium, boron oxide and boric acid, the boron source are technical pure or are that analysis is pure;Grain size≤200 μm of the boron source.
3. the preparation method of ultrathin boron nitride nanosheet according to claim 1, it is characterised in that the solid-state nitrogen source is
One kind in melamine, azepine cytimidine and dicyanodiamine, the solid-state nitrogen source are technical pure or are that analysis is pure;The solid-state
Grain size≤200 μm of nitrogen source.
4. the preparation method of ultrathin boron nitride nanosheet according to claim 1, it is characterised in that the metal salt is chlorine
Change one or more of sodium, potassium chloride and sodium fluoride, the metal salt is technical pure or is that analysis is pure;The grain size of the metal salt
≤ 200 μm.
5. a kind of ultrathin boron nitride nanosheet, it is characterised in that the ultrathin boron nitride nanosheet is according to Claims 1 to 4 item
Any one of ultrathin boron nitride nanosheet prepared by the preparation method of the ultrathin boron nitride nanosheet.
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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 |
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