CN109052343A - A kind of preparation method of ultra-thin hexagonal boron nitride piece - Google Patents
A kind of preparation method of ultra-thin hexagonal boron nitride piece Download PDFInfo
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- CN109052343A CN109052343A CN201811166880.4A CN201811166880A CN109052343A CN 109052343 A CN109052343 A CN 109052343A CN 201811166880 A CN201811166880 A CN 201811166880A CN 109052343 A CN109052343 A CN 109052343A
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- 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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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention is a kind of preparation method of ultra-thin hexagonal boron nitride piece.Method includes the following steps: by sodium borohydride (NaBH4) be put into dioxane, ammonium chloride (NH is added4Cl), stir 1-2 hours, obtain mixed solution；Mixed solution is filtered, clear transparent solutions are obtained, by solution rotary evaporation 1-2 hours at 45~55 DEG C, obtains presoma；Presoma is kept the temperature 1.5~2.5 hours at 700~800 DEG C, is then cooled to room temperature, obtains ultra-thin hexagonal boron nitride piece.Present device is simple, simple process and low cost, the stable structure of product, easy to operate, can in high volume synthesize ultra-thin hexagonal boron nitride piece.
Description
Technical field
Technical solution of the present invention is related to a kind of boron nitride material, in particular to a kind of preparation side of ultra-thin hexagonal boron nitride piece
Method belongs to field of inorganic materials.
Background technique
Boron nitride (BN) material is a kind of important inorganic non-metallic material, is had very important effect and status, because
It is with good electrical insulating property, broad-band gap, high-termal conductivity, chemical stability and thermal expansion coefficient is low, thermal shock resistance is good,
Be widely used in cutting element, grinding-material, heat conductive insulating additive, high-temperaure coating, etc. fields；BN nanometers of materials of activity simultaneously
Material has the unique performances such as good chemical inertness and high-specific surface area, also has very big application latent in terms of adsorption
Power.
Hexagonal boron nitride nanosheet is a kind of novel two-dimension nano materials, has high temperature resistance, high heat conductance, low-heat
The excellent physics and chemical characteristic such as the coefficient of expansion, high anti-oxidation ability, excellent wave, strong resistance to corrosion, broad stopband,
It is widely used in high temperature semiconductors material, photoelectric material, ceramic material and each research field of composite material, becomes and grind now
The focus studied carefully.
There are many methods to prepare hexagonal boron nitride nanosheet material, such as mechanical stripping method, synthetic method, inorganic chemistry
Stripping method etc., the hexagonal boron nitride powder that Pacile et al. is 10um with partial size obtain about 10 using adhesive tape stripping method
The boron nitride nanosheet of atomic layer.Alem et al. pre-processes boron nitride powder first with adhesive tape stripping method, then
Boron nitride flakes are removed with plasma etching method, have prepared the boron nitride nanosheet of single layer or few layer.Yurdakul etc.
People utilizes fluid stripping method, boron nitride powder has been dispersed in the in the mixed solvent of DMP and chloroform, the handle under the high pressure of 207MPa
Mixed solution is pressed into microfluidic fluid receptacles, obtains the boron nitride nanosheet of about 8-12nm thickness.Yi et al. utilizes fluid stripping method, uses
Dimethylformamide solvent as initial dispersion liquid, the boron nitride nanosheet prepared with a thickness of 4-5 layers.Li et al. people utilizes ion
It is inserted into stripping method, NaOH and KOH is mixed, hexagonal boron nitride powder is then uniformly added into, placing into liner is polytetrafluoroethyl-ne
In the pressure cooker of alkene, is heated 2 hours at 180 DEG C, the boron nitride nanosheet of edge convolution has been prepared, with a thickness of 2-4nm.
Du et al. utilizes chemistry functional stripping method, by hexagonal boron nitride powder and NH4F is uniformly mixed, and it is small that 24 are heated at 180 DEG C
When, the boron nitride nanosheet lateral dimension about 4um of acquisition, about three atomic layers of thickness.Zhao Yan et al. is removed using inorganic chemistry
Method, using the mixed solution of the concentrated sulfuric acid and phosphoric acid as reaction dissolvent, by the direct removing of the hexagonal boron nitride powder to block,
Prepare hexagonal boron nitride nanosheet.Meanwhile hexagonal boron nitride particles are prepared using precursor process there are also very much, such as
Melamine and boric acid are added to temperature with the mass ratio of the material 1: 2 and a certain amount of calcium carbonate by Takashi Kawasaki etc.
90 DEG C, relative humidity be 90% mixer in mix 6h, obtain C3H6N6·2H3BO3Presoma, then by presoma in nitrogen
In 1800 DEG C of roasting 2h in atmosphere, hexagonal boron nitride particles are finally obtained.Yuting Wang etc. is used with sodium borohydride and amino
Sulfonic acid is that the ammonia borane of raw material preparation is presoma, is roasted at 1300~1700 DEG C in ammonia, nitrogen, argon atmosphere respectively
It burns, finally prepares hexagonal boron nitride ball of the diameter at several hundred nanometers.This patent provides a kind of presoma pyrolysismethod to prepare
The method of ultra-thin hexagonal boron nitride piece, the product reacted in dioxane solution using ammonium chloride and sodium borohydride as presoma,
Presoma is in H2Reaction preparation sheet ultrathin boron nitride (BN) is carried out under+Ar atmosphere.
Summary of the invention
It is an object of the present invention to propose a kind of simple process, have excellent performance, easy to operate ultra-thin hexagonal boron nitride piece
Preparation method.This method prepares presoma with ammonium chloride and sodium borohydride in dioxane solution, then in H2Under+Ar atmosphere into
Row reaction preparation sheet ultrathin boron nitride (BN).Present device is simple, simple process and low cost, the stable structure of product,
It is easy to operate, can in high volume synthesize ultra-thin hexagonal boron nitride piece.
The technical scheme is that
A kind of preparation method of ultra-thin hexagonal boron nitride piece, comprising the following steps:
(1) by sodium borohydride (NaBH4) be added in dioxane, add ammonium chloride (NH4Cl), stir 1-2 hours,
Obtain mixed solution；
Wherein, every 200mL dioxane adds 0.5~2 mole of sodium borohydride, and molar ratio is sodium borohydride: ammonium chloride=1~
1.1:1.1；
(2) mixed solution is filtered, obtains clear transparent solutions, by solution rotary evaporation 1-2 hours at 45~55 DEG C,
Obtain viscous liquid, i.e. presoma；
(3) presoma is heated to 700~800 DEG C under hydrogen/argon-mixed atmosphere in tube furnace with 5 DEG C of speed per minute
Heat preservation 1.5~2.5 hours, is then cooled to room temperature, obtains ultra-thin hexagonal boron nitride piece.
Agitation revolution in the step (1) is 400-450 rev/min.
In the mixed atmosphere, volume ratio hydrogen: argon gas=1:1.
Sodium borohydride in the step (1): ammonium chloride molar ratio is preferably 1~1.05:1.1.
The beneficial effects of the present invention are:
(1) present invention by presoma be pyrolyzed method, this method be preparation sheet boron nitride provide one newly
The advantages that approach, the designability of this method set molecule, good craftsmanship and realizability, is in one.
(2) the obtained ultra-thin hexagonal boron nitride piece of the present invention takes full advantage of ammonium chloride and sodium borohydride in dioxane
This new presoma of reaction product in solution, then by control Means of Pyrolyzed Precursor temperature, thus be prepared into crystallinity it is higher,
The lesser ultrathin boron nitride piece of crystallite dimension, this method to synthesize big volume production under conditions of being easy to control in simple process
Product.
(3) the ultrathin boron nitride piece prepared through the invention has that high-termal conductivity, high-temperature heat insulation be good, low bulk system
Number, the feature that chemical stability is good, lubricity is excellent, have a wide range of applications in the industrial production.
(4) the method for the present invention instrument equipment is simple, simple process and low cost, the stable structure of product, operation side
Just, ultra-thin hexagonal boron nitride piece can in high volume be synthesized.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is the XRD diagram of gained sample after the sample of the embodiment of the present invention 1 is heated to 700 DEG C of coolings.
Fig. 2 is after the sample of the embodiment of the present invention 4 is heated to 800 DEG C of coolings, and the TEM of gained sample schemes.
Fig. 3 is after the sample of the embodiment of the present invention 4 is heated to 800 DEG C of coolings, and the HRTEM of gained sample schemes.
Specific embodiment
Embodiment 1
(1) 1:1 in molar ratio, weighs 37.83 grams of (1 mole) sodium borohydride powder (NaBH4) be put into and fill 200ml dioxy
In the flask of six ring organic solutions, then weigh 53.49 grams of (1 mole) ammonium chloride (NH4Cl) powder is put into flask, the two powder
Not with dioxane liquid reactions, then mechanical stirring, per minute 400 turns of stirring are stirred 1 hour.
(2) solution in flask is filtered, filters off the sodium chloride of generation, obtains clear transparent solutions, by solution at 50 DEG C
Rotary evaporation 1-2 hours, until viscous liquid (presoma) to be obtained.
(3) it takes a certain amount of presoma to be put into ceramic crucible, then adds hydrogen to add under argon atmospher with every point in tube furnace
The speed that 5 DEG C of clock is heated to 700 DEG C, keeps the temperature 1.5 hours, is cooled to room temperature to get sample to be tested powder is arrived.
Fig. 1 is H at presoma is 700 DEG C in temperature2The XRD spectrum of sample obtained by being reacted in+Ar atmosphere, from
As can be seen that the characteristic peak of sample occurs at 2 θ=26.7 °, 41.5 °, 55.1 ° and 75.9 ° in XRD diagram, this and h-BN
(JCDPS34-0421) (002) crystal face, (100) crystal face, (004) crystal face is corresponding with (110) crystal face.This shows prepared
Sample is BN material, and does not have miscellaneous peak appearance in XRD diagram, so prepared sample purity and crystallinity is all very high.
Embodiment 2
(1) 1:1.1 in molar ratio, weighs 37.83 grams of (1 mole) sodium borohydride powder (NaBH4) be put into and fill 200ml bis-
In the flask of six ring organic solution of oxygen, then weigh 58.839 (1.1 moles) gram ammonium chloride (NH4Cl) powder is put into flask, and two
Person's powder is not with dioxane liquid reactions, and then mechanical stirring, per minute 420 turns of stirring are stirred 1.5 hours.
(2) solution in flask is filtered, filters off the sodium chloride of generation, obtains clear transparent solutions, by solution at 50 DEG C
Rotary evaporation 1-2 hours, until viscous liquid (presoma) to be obtained.
(3) it takes a certain amount of presoma to be put into ceramic crucible, then adds hydrogen to add under argon atmospher with every point in tube furnace
The speed that 5 DEG C of clock is heated to 700 DEG C, keeps the temperature 1.5 hours, is cooled to room temperature to get sample to be tested powder is arrived.
Under this molar ratio, compared with Example 1, the impurity content and block structure of acquired sample are seldom, BN piece
Content and purity all increase.
Embodiment 3
(1) in molar ratio 2: 2.1, weigh 75.66 grams of (2 moles) sodium borohydride powder (NaBH4) be put into and fill 400ml bis-
In the flask of six ring organic solution of oxygen, then weigh 112.329 grams of (2.1 moles) ammonium chloride (NH4Cl) powder is put into flask, and two
Person's powder is not with dioxane liquid reactions, and then mechanical stirring, per minute 440 turns of stirring are stirred 2 hours.
(2) solution in flask is filtered, filters off the sodium chloride of generation, obtains clear transparent solutions, by solution at 50 DEG C
Rotary evaporation 1-2 hours, until viscous liquid (presoma) to be obtained.
(3) it takes a certain amount of presoma to be put into ceramic crucible, then adds hydrogen to add under argon atmospher with every point in tube furnace
The speed that 5 DEG C of clock is heated to 750 DEG C, keeps the temperature 2 hours, is cooled to room temperature to get sample to be tested powder is arrived.
At this temperature, compared with 700 DEG C, the impurity content and block structure of acquired sample are seldom, the content of BN piece
It all increases with purity.
Embodiment 4
(1) in molar ratio 2: 2.1, weigh 75.66 grams of (2 moles) sodium borohydride powder (NaBH4) be put into and fill 400ml bis-
In the flask of six ring organic solution of oxygen, then weigh 112.329 grams of (2.1 moles) ammonium chloride (NH4Cl) powder is put into flask, and two
Person's powder is not with dioxane liquid reactions, and then mechanical stirring, per minute 450 turns of stirring are stirred 2 hours.
(2) solution in flask is filtered, filters off the sodium chloride of generation, obtains clear transparent solutions, by solution at 50 DEG C
Rotary evaporation 1-2 hours, until viscous liquid (presoma) to be obtained.
(3) it takes a certain amount of presoma to be put into ceramic crucible, then adds hydrogen to add under argon atmospher with every point in tube furnace
The speed that 5 DEG C of clock is heated to 800 DEG C, keeps the temperature 2.5 hours, is cooled to room temperature to get sample to be tested powder is arrived.
H at being 800 DEG C in temperature by presoma2Sample obtained by being carried out in the mixed atmosphere of+Ar (1:1) reaction 2 hours
The transmission electron microscope photo of product is as shown in Fig. 2, high-resolution photo is as shown in Figure 3.As can be seen that presoma is in high temperature and H2+ Ar gas
Generated gas by thermal decomposition in atmosphere, the aggregation of gas will lead to the cokled surface of reactant, when gas build to it is enough when, meeting
Make reaction-ure surface is broken to generate hole and fluffy sheets of fibres shape structure, not of uniform size, length is from several hundred nanometers to several
In micron range.Schemed according to the HRTEM of sample, the interplanar distance that can measure prepared BN material is 0.33nm, is nitrogenized with six sides
(002) crystal face of boron (h-BN) is corresponding, this can prove that the product prepared by us is ultra-thin hexagonal AlN piece.
Embodiment 5
(1) in molar ratio 2: 2.1, weigh 75.66 grams of (2 moles) sodium borohydride powder (NaBH4) be put into and fill 400ml bis-
In the flask of six ring organic solution of oxygen, then weigh 112.329 grams of (2.1 moles) ammonium chloride (NH4Cl) powder is put into flask, and two
Person's powder is not with dioxane liquid reactions, and then mechanical stirring, per minute 450 turns of stirring are stirred 2 hours.
(2) solution in flask is filtered, filters off the sodium chloride of generation, obtains clear transparent solutions, by solution at 50 DEG C
Rotary evaporation 1-2 hours, until viscous liquid (presoma) to be obtained.
(3) it takes a certain amount of presoma to be put into ceramic crucible, then adds hydrogen to add under argon atmospher with every point in tube furnace
The speed that 5 DEG C of clock is heated to 850 DEG C, keeps the temperature 2.5 hours, is cooled to room temperature, obtains sample powder.
Obtained product at this temperature, purity and yield are declined, and structural stability weakens, and laminated structure has
It is crushed, performance is not so good as excellent at 800 DEG C.
Boron nitride nanosheet has the structure similar with carbon phase, and the sp2 hybrid structure of the existing soft hexagonal of boron nitride has again
The sp3 hybrid structure of hard diamond-like.Wherein, hexagonal boron nitride (h-BN) is corresponding with hexagonal graphite, cubic boron nitride (c-
BN) corresponding with the zincblende lattce structure of diamond, wherein the c-BN of the h-BN and sp3 hydridization of sp2 hydridization is stable state structure.So
Ultra-thin hexagonal boron nitride piece prepared by the present invention has rock-steady structure.
From above embodiment it will be seen that the method that the present invention uses a kind of pyrolysis of presoma, this method collection point
The designability of son, good craftsmanship and the advantages that realizability in one, be a kind of important method.
Unaccomplished matter of the present invention is well-known technique.
Claims (4)
1. a kind of preparation method of ultra-thin hexagonal boron nitride piece, it is characterized in that the following steps are included:
(1) by sodium borohydride (NaBH4) be added in dioxane, add ammonium chloride (NH4Cl), stir 1-2 hours, obtain
Mixed solution；
Wherein, every 200mL dioxane adds 0.5 ~ 2 mole of sodium borohydride, and molar ratio is sodium borohydride: ammonium chloride=1 ~ 1.1:
1.1；
(2) mixed solution is filtered, obtains clear transparent solutions, by solution rotary evaporation 1-2 hours at 45 ~ 55 DEG C, obtained
Viscous liquid, i.e. presoma；
(3) presoma is heated to 700 ~ 800 DEG C under hydrogen/argon-mixed atmosphere in tube furnace with 5 DEG C of speed per minute, heat preservation
It 1.5 ~ 2.5 hours, is then cooled to room temperature, obtains ultra-thin hexagonal boron nitride piece.
2. the preparation method of ultra-thin hexagonal boron nitride piece as described in claim 1, it is characterized in that stirring in the step (1)
Mixing revolution is 400-450 rev/min.
3. the preparation method of ultra-thin hexagonal boron nitride piece as described in claim 1, it is characterized in that in the mixed atmosphere, body
Product is than hydrogen: argon gas=1:1.
4. the preparation method of ultra-thin hexagonal boron nitride piece as described in claim 1, it is characterized in that in the step (1) mole
Than for sodium borohydride: ammonium chloride=1 ~ 1.05:1.1.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000007310A (en) * | 1998-06-19 | 2000-01-11 | Denki Kagaku Kogyo Kk | Highly filling boron nitride powder |
| JP2004161546A (en) * | 2002-11-13 | 2004-06-10 | National Institute For Materials Science | Processes for forming boron nitride precursor and for manufacturing boron nitride nanotube using boron nitride precursor |
| CN103303867A (en) * | 2013-07-09 | 2013-09-18 | 河北工业大学 | Method for synthesizing ammonia borane |
| CN104386657A (en) * | 2014-11-12 | 2015-03-04 | 河北工业大学 | Preparation method of high-crystallinity boron nitride |
| CN105417506A (en) * | 2015-11-10 | 2016-03-23 | 沈阳化工大学 | Method for preparing hexagonal boron nitride particles by precursor method |
| 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 |
-
2018
- 2018-10-08 CN CN201811166880.4A patent/CN109052343A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000007310A (en) * | 1998-06-19 | 2000-01-11 | Denki Kagaku Kogyo Kk | Highly filling boron nitride powder |
| JP2004161546A (en) * | 2002-11-13 | 2004-06-10 | National Institute For Materials Science | Processes for forming boron nitride precursor and for manufacturing boron nitride nanotube using boron nitride precursor |
| CN103303867A (en) * | 2013-07-09 | 2013-09-18 | 河北工业大学 | Method for synthesizing ammonia borane |
| CN104386657A (en) * | 2014-11-12 | 2015-03-04 | 河北工业大学 | Preparation method of high-crystallinity boron nitride |
| CN105417506A (en) * | 2015-11-10 | 2016-03-23 | 沈阳化工大学 | Method for preparing hexagonal boron nitride particles by precursor method |
| 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 |
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