CN109437129A - One one step preparation method of two-dimentional amination boron nitride - Google Patents
One one step preparation method of two-dimentional amination boron nitride Download PDFInfo
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- CN109437129A CN109437129A CN201811539004.1A CN201811539004A CN109437129A CN 109437129 A CN109437129 A CN 109437129A CN 201811539004 A CN201811539004 A CN 201811539004A CN 109437129 A CN109437129 A CN 109437129A
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- boron nitride
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- 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
- C01B21/0646—Preparation by pyrolysis of boron and nitrogen containing compounds
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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
- C01P2004/01—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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The present invention provides an one step preparation method of two-dimentional amination boron nitride.Using Sodamide and boron oxide as precursors, heating reaction obtains tripartite's boron nitride；It is put into ball grinder after tripartite's boron nitride powder is mixed with urea, pours nitrogen as gas is protected, ball milling under room temperature obtains two-dimentional amination boron nitride.Urea not only facilitates removing in the method disclosed in the present; and protection boron nitride nanosheet; prevent the extensive formation of its excessive mechanical damage and lattice defect; the two-dimentional boron nitride nanosheet that the ABC mode that removing tripartite's boron nitride obtains arranges; lamella is more easily peelable to be opened; amino in boron nitride surface modification can greatly improve the dispersion performance of boron nitride in the solution, have prepare it is simple, at low cost, be easy to the characteristics of industrialized mass production.
Description
Technical field
The present invention relates to two-dimensional functionalized boron nitride preparation fields, more particularly to one kind is by one step ball milling system of tripartite's boron nitride
The method of standby two dimension amination boron nitride nanosheet.
Background technique
Tripartite's boron nitride chemical stability is high, and aerial oxidation resistance temperature has very high resistance close to 900 DEG C
Rate, luminous position can be used as the insulating film, ultraviolet or deep of excellent high-temperature refractory, electronic device in ultraviolet light wave band
Ultraviolet luminescent material etc. also has very wide application in terms of high temperature, high-power, high-speed semiconductor device and heat sink material
Prospect.
Hexagonal boron nitride, each layer are all by B atom and N atom according to sp2Hybrid form is alternately arranged the unlimited of composition
The hexagon of extension, these atomic layers are again along C axis direction according to ABAB ..., and mode arranges, lattice constant a=b=0.25nm, c
=0.66nm between B and N atom altogether by covalently bonded, is then mutually tied with Van der Waals force between layers in same layer
It closes.Tripartite's boron nitride belongs to trigonal system, its structure and hexagonal boron nitride is closely similar, and each layer is equally by B atom and N
Atom is according to sp2Hybrid form is alternately arranged the hexagonal mesh of composition infinitely extended, and difference is these atomic layers in the axis side C
Upwards according to ABCABC ..., mode is arranged, lattice constant a=b=0.25nm, c=1.00nm, in each layer, B and N atom
Between by very strong covalently bonded altogether, then combined between layers with weak Van der Waals force.Remove tripartite's boron nitride and
The monoatomic layer BN structure that hexagonal boron nitride is formed is just the same, removes few layer of two-dimentional boron nitride nanosheet of formation respectively with AB
It is arranged with ABC mode.Different stack manners means the difference of structure and performance, brings referring to graphene difference stacking form
The change of various physico-chemical properties, the two-dimentional boron nitride nanosheet that the ABC mode that removing tripartite's boron nitride obtains arranges is class one zone
The new material for the two-dimentional boron nitride nanosheet not arranged in the AB mode that removing hexagonal boron nitride obtains.In addition, boron nitride is chemical
Property is stablized, and surface lacks active group, thus dispersibility in a solvent is very poor, and which greatly limits the application necks of boron nitride
Domain.
Summary of the invention
An a kind of one step preparation method of two-dimentional amination boron nitride is proposed, more particularly to one kind is by one step of tripartite's boron nitride
The method that ball milling prepares two-dimentional amination boron nitride nanosheet.For graphene, the removing difficulty of boron nitride is higher, this is
Since the electronegativity difference of B atom and N atom goes back the active force between atomic layer in addition to Van der Waals force in boron nitride structure
Active force with part ion keyness matter is referred to as lip-lip and acts on.Hexagonal boron nitride is similar with tripartite's boron nitride structure,
But hexagonal boron nitride is more common, AB stack manner makes the B atom of interlayer and N atom face and is alternately present, Ci Zhongjie
Structure is more stable, and binding force is stronger.B atom and N atom between tripartite's boron nitride layer is without face one by one, it will be appreciated that is six side's nitrogen
Change the dislocation form of boron, this namely more rare reason of tripartite's boron nitride is analyzed, tripartite's boron nitride lamella from energy point of view
It is more easily peelable to open.Electrophilic B atom can be by-NH2Base group modification, and the boron nitride nanosheet after modification has very
Good water solubility.Amination boron nitride improves the dispersibility of boron nitride in a solvent, and dispersion, carrying and buffer action are effective
The reunion for preventing nano particle is proposed, by the available the second best in quality aeroge of dehydration and almost transparent film.
The present invention adopts the following technical scheme:
One one step preparation method of two-dimentional amination boron nitride, includes the following steps:
(1) it using Sodamide and boron oxide as precursors, is put into autoclave, heating is reacted, and product is with dense
After hydrochloric acid and deionized water cleaning, it is dried for standby in vacuum drying oven；
(2) it is put into ball grinder after mixing tripartite's boron nitride powder with urea, pours nitrogen as protection gas, under room temperature
Ball milling obtains two-dimentional amination boron nitride.
The mole ratio of Sodamide and boron oxide in step (1) is 12: 5.
Heating in step (1) rises to 600 DEG C from room temperature with the rate of 10 DEG C/min, in 600 DEG C of maintenance 6-8h.
Drying temperature in step (1) is 60-80 DEG C, time 4-8h.
The mass ratio of tripartite's boron nitride powder and urea in step (2) is 1: 40-1: 80.
Ball-milling Time in step (2) is 10-30h, revolving speed 500-700r/min.
The present invention has the advantage that
(1) the two-dimentional boron nitride nanosheet that the ABC mode that removing tripartite's boron nitride obtains arranges is different from conventional method and shells
The two-dimentional boron nitride nanosheet that the AB mode obtained from hexagonal boron nitride arranges, and lamella is more easily peelable opens.
(2) amino in boron nitride surface modification can greatly improve the dispersion performance of boron nitride in the solution.
(3) urea not only facilitates removing, and protects boron nitride nanosheet, prevents its excessive mechanical damage and lattice
The extensive formation of defect.
(4) have prepare it is simple, at low cost, be easy to the characteristics of industrialized mass production.
Detailed description of the invention
Fig. 1 is hexagonal boron nitride crystal structure schematic diagram.
Fig. 2 is tripartite's boron nitride crystal structural schematic diagram.
Fig. 3 is the transmission electron microscope picture that the method for the present invention prepares two-dimentional amination boron nitride.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) 4.73g Sodamide and 3.5g boron oxide are put into autoclave, rise to 600 from room temperature with the rate of 10 DEG C/min
℃。
(2) in 600 DEG C of maintenance 6h.
(3) after cleaning product concentrated hydrochloric acid and deionized water, it is put into vacuum drying oven, is heated to 60 DEG C, maintains 4h.
(4) it is put into ball grinder after mixing tripartite's boron nitride powder that mass ratio is 1: 40 with urea, pours nitrogen work
To protect gas.
(5) ball milling 20h under room temperature, revolving speed 700r/min obtain two-dimentional amination boron nitride.
Fig. 3 includes the transmission electron microscope picture that the present embodiment prepares two-dimentional amination boron nitride.
Embodiment 2
(1) 4.73g Sodamide and 3.5g boron oxide are put into autoclave, rise to 600 from room temperature with the rate of 10 DEG C/min
℃。
(2) in 600 DEG C of maintenance 8h.
(3) after cleaning product concentrated hydrochloric acid and deionized water, it is put into vacuum drying oven, is heated to 60 DEG C, maintains 4h.
(4) it is put into ball grinder after mixing tripartite's boron nitride powder that mass ratio is 1: 40 with urea, pours nitrogen work
To protect gas.
(5) ball milling 20h under room temperature, revolving speed 700r/min obtain two-dimentional amination boron nitride.
Embodiment 3
(1) 4.73g Sodamide and 3.5g boron oxide are put into autoclave, rise to 600 from room temperature with the rate of 10 DEG C/min
℃。
(2) in 600 DEG C of maintenance 6h.
(3) after cleaning product concentrated hydrochloric acid and deionized water, it is put into vacuum drying oven, is heated to 80 DEG C, maintains 4h.
(4) it is put into ball grinder after mixing tripartite's boron nitride powder that mass ratio is 1: 40 with urea, pours nitrogen work
To protect gas.
(5) ball milling 20h under room temperature, revolving speed 700r/min obtain two-dimentional amination boron nitride.
Embodiment 4
(1) 4.73g Sodamide and 3.5g boron oxide are put into autoclave, rise to 600 from room temperature with the rate of 10 DEG C/min
℃。
(2) in 600 DEG C of maintenance 6h.
(3) after cleaning product concentrated hydrochloric acid and deionized water, it is put into vacuum drying oven, is heated to 60 DEG C, maintains 4h.
(4) it is put into ball grinder after mixing tripartite's boron nitride powder that mass ratio is 1: 60 with urea, pours nitrogen work
To protect gas.
(5) ball milling 20h under room temperature, revolving speed 700r/min obtain two-dimentional amination boron nitride.
Embodiment 5
(1) 4.73g Sodamide and 3.5g boron oxide are put into autoclave, rise to 600 from room temperature with the rate of 10 DEG C/min
℃。
(2) in 600 DEG C of maintenance 6h.
(3) after cleaning product concentrated hydrochloric acid and deionized water, it is put into vacuum drying oven, is heated to 60 DEG C, maintains 4h.
(4) it is put into ball grinder after mixing tripartite's boron nitride powder that mass ratio is 1: 40 with urea, pours nitrogen work
To protect gas.
(5) ball milling 30h under room temperature, revolving speed 600r/min obtain two-dimentional amination boron nitride.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (6)
1. an one step preparation method of two-dimentional amination boron nitride, includes the following steps:
(1) it using Sodamide and boron oxide as precursors, is put into autoclave, heating is reacted, product concentrated hydrochloric acid
After deionized water cleaning, it is dried for standby in vacuum drying oven；
(2) it is put into ball grinder after mixing tripartite's boron nitride powder with urea, pours nitrogen and be used as protection gas, ball under room temperature
Mill, obtains two-dimentional amination boron nitride.
2. preparation method according to claim 1, which is characterized in that mole of Sodamide and boron oxide in step (1)
Number is than being 12: 5.
3. preparation method according to claim 1, which is characterized in that the heating in step (1) is with the rate of 10 DEG C/min
600 DEG C are risen to from room temperature, in 600 DEG C of maintenance 6-8h.
4. preparation method according to claim 1, which is characterized in that the drying temperature in step (1) is 60-80 DEG C, when
Between be 4-8h.
5. preparation method according to claim 1, which is characterized in that tripartite's boron nitride powder and urea in step (2)
Mass ratio be 1: 40-1: 80.
6. preparation method according to claim 1, which is characterized in that the Ball-milling Time in step (2) is 10-30h, revolving speed
For 500-700r/min.
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| CN201811539004.1A CN109437129A (en) | 2018-11-29 | 2018-11-29 | One one step preparation method of two-dimentional amination boron nitride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110004712A (en) * | 2019-04-08 | 2019-07-12 | 上海电力学院 | A kind of preparation method of the high-intensitive heat conducting film based on Kevlar nanofiber |
| CN113512398A (en) * | 2021-04-27 | 2021-10-19 | 南京林业大学 | Aldehyde-free high-thermal-conductivity adhesive and preparation method and application thereof |
| CN115449257A (en) * | 2022-09-15 | 2022-12-09 | 中山火炬职业技术学院 | Amidated boron nitride-graphene oxide heat-conducting and insulating ink and preparation method and application thereof |
| CN116903978A (en) * | 2023-08-23 | 2023-10-20 | 常州贺斯特科技股份有限公司 | Modified boron nitride/carboxylated cellulose/PVA composite heat conduction interface material and preparation method thereof |
-
2018
- 2018-11-29 CN CN201811539004.1A patent/CN109437129A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110004712A (en) * | 2019-04-08 | 2019-07-12 | 上海电力学院 | A kind of preparation method of the high-intensitive heat conducting film based on Kevlar nanofiber |
| CN110004712B (en) * | 2019-04-08 | 2021-09-07 | 上海电力学院 | Preparation method of high-strength heat-conducting film based on Kevlar nanofibers |
| CN113512398A (en) * | 2021-04-27 | 2021-10-19 | 南京林业大学 | Aldehyde-free high-thermal-conductivity adhesive and preparation method and application thereof |
| CN115449257A (en) * | 2022-09-15 | 2022-12-09 | 中山火炬职业技术学院 | Amidated boron nitride-graphene oxide heat-conducting and insulating ink and preparation method and application thereof |
| CN116903978A (en) * | 2023-08-23 | 2023-10-20 | 常州贺斯特科技股份有限公司 | Modified boron nitride/carboxylated cellulose/PVA composite heat conduction interface material and preparation method thereof |
| CN116903978B (en) * | 2023-08-23 | 2024-03-26 | 常州贺斯特科技股份有限公司 | Modified boron nitride/carboxylated cellulose/PVA composite heat conduction interface material and preparation method thereof |
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Application publication date: 20190308 |