CN110116995A - The preparation method of boron nitride nanometer stick - Google Patents
The preparation method of boron nitride nanometer stick Download PDFInfo
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- CN110116995A CN110116995A CN201810117459.8A CN201810117459A CN110116995A CN 110116995 A CN110116995 A CN 110116995A CN 201810117459 A CN201810117459 A CN 201810117459A CN 110116995 A CN110116995 A CN 110116995A
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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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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention belongs to technical field of nano material, and in particular to a kind of preparation method of boron nitride nanometer stick.The preparation method of the boron nitride nanometer stick includes the following steps: to provide boron source, nitrogen source, catalysts and solvents；Hydro-thermal reaction is carried out after the boron source, the nitrogen source, the catalyst and the solvent are mixed, obtains reaction product；By the reaction product centrifugal treating, boron nitride nanometer stick is obtained.It is reduced costs using cheap, less toxic or nontoxic presoma to improve the safety of experiment in the preparation method；Whole preparation process has the characteristics that low temperature is controllable, and has finally obtained that object is mutually single, boron nitride nanometer stick of high-purity.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of preparation method of boron nitride nanometer stick.
Background technique
In semicon industry, with the continuous extension of Moore's Law, industry to broad stopband, high saturated velocity, high-termal conductivity,
The requirement of high-breakdown-voltage is higher and higher, and correspondingly, semiconductor material is from the first generation, the silicon (forbidden band of second generation low energy gap
Band gap Eg=1.12eV), GaAs (Eg=1.42eV) developed to the third generation silicon carbide (Eg=3.25eV, 4H-SiC),
Gallium nitride (Eg=3.44eV).Boron nitride (BN) is a kind of semiconductor material with wide forbidden band, and hexagonal phase (P63/mmc) has class stone
Ink structure (Eg=5.9eV), also referred to as white graphite have the function of thermally conductive, insulation and lubrication；Its cubic phase (F 3m) has eka-gold
Hard rock structure (Eg=6.6eV) has the characteristics that thermally conductive, insulation, hardness are high.As with more broad stopband BN (Eg > 5eV),
It will play bigger effect in the manufacture of super large-scale integration, the especially implementation of 5G technology.
Boron nitride (BN) nanostructure common at present is mainly nanometer sheet and nanotube, such as patent CN103626141A
Acid, potassium permanganate, hydrogen peroxide and hexagonal boron nitride powder one are reacted, BN nanometer sheet, patent are prepared for using chemical stripping
CN105036096A is prepared for high-purity BN nanotube using reaction gas vortex, and patent CN103803513A is with carbon nanotube
Template is prepared for BN nanotube using chemical vapour deposition technique.And the preparation of BN nanometer rods is then more rare, patent
CN102120568A uses precursor pyrolysis and hot pressing, grown BN nanometer rods of the diameter less than 50 nanometers in carbon nanotube.Existing
Have in technology, used raw material or solvent, as concentrated nitric acid has strong corrosive, dimethylbenzene, toluene or dimethylformamide tool
There is certain bio-toxicity, borazine has the shortcomings that inflammable and explosive and expensive.In addition, the prior art is needed 1000
DEG C or more make presoma cracking can just obtain BN nanometer rods, energy consumption is larger.Therefore, the prior art is to be improved.
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency of the prior art, a kind of preparation side of boron nitride nanometer stick is provided
Method, it is intended to which the preparation condition for solving existing boron nitride nanometer stick is very harsh, and there is risk and technology at high cost to ask
Topic.
For achieving the above object, The technical solution adopted by the invention is as follows:
The present invention provides a kind of preparation method of boron nitride nanometer stick, includes the following steps:
Boron source, nitrogen source, catalysts and solvents are provided；
Hydro-thermal reaction is carried out after the boron source, the nitrogen source, the catalyst and the solvent are mixed, reaction is obtained and produces
Object；
By the reaction product centrifugal treating, boron nitride nanometer stick is obtained.
The preparation method of boron nitride nanometer stick provided by the invention is a kind of to prepare boron nitride using mild hydro-thermal reaction
The method of nanometer rods uses cheap, less toxic or nontoxic presoma in this method, so that the safety of experiment is improved,
It reduces costs；Whole preparation process has the characteristics that low temperature is controllable, and has finally obtained that object is mutually single, nitridation of high-purity
Boron nanometer rods.
Detailed description of the invention
Fig. 1 is the phenogram of the BN nanometer rods prepared in the embodiment of the present invention 1；Wherein, a) be low power BN nanometer rods SEM
Image, b) it is the BN nanometer rods SEM image amplified, illustration is corresponding XRD spectra；It c) is the TEM image of BN nanometer rods；D) it is
The high-resolution lattice fringe of BN nanometer rods, illustration are corresponding FFT diffraction image.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
The embodiment of the invention provides a kind of preparation methods of boron nitride nanometer stick, include the following steps:
S01: boron source, nitrogen source, catalysts and solvents are provided；
S02: carrying out hydro-thermal reaction after the boron source, the nitrogen source, the catalyst and the solvent are mixed, and obtains anti-
Answer product；
S03: by the reaction product centrifugal treating, boron nitride nanometer stick is obtained.
The preparation method of boron nitride nanometer stick provided in an embodiment of the present invention is a kind of to utilize mild hydro-thermal reaction preparation
The method of boron nitride nanometer stick uses cheap, less toxic or nontoxic presoma in this method, to improve the peace of experiment
Quan Xing is reduced costs；Whole preparation process has the characteristics that low temperature is controllable, and has finally obtained that object is mutually single, high-purity
Boron nitride nanometer stick.
Further, in above-mentioned steps S01: the boron source is boron-containing compound, specifically includes boric acid, Boratex, boron
At least one of sour ammonium, phenyl boric acid and triethyl borate, but be not limited to above-mentioned several.The nitrogen source includes amino acid；Wherein,
The amino acid specifically includes at least one of glycine, glutamic acid, sarcosine, tryptophan and phenylalanine, but is not limited to
It is above-mentioned several.The catalyst includes halide；Wherein, the halide specifically includes sodium chloride, sodium fluoride, ammonium fluoride and chlorine
Change at least one of ammonium, but is not limited to above-mentioned several.And the solvent includes water and/or organic solvent, i.e. solvent can be
Water is also possible to organic solvent, is also possible to the mixed solvent of water and organic solvent；Wherein, the water can be deionized water；
The organic solvent may include at least one of ethyl alcohol, isopropanol, dimethylformamide and methanol, but be not limited to above-mentioned several
Kind.
Further, in above-mentioned steps S02: the boron source, the nitrogen source, the range of the molar ratio of the catalyst are
10:(30-60): 1；Specifically, boron source, nitrogen source, the molar ratio of catalyst can be 10:30:1 or 10:40:1 or 10:60:1
Deng.In the range of the molar ratio, catalyst can preferably be catalyzed boron source and nitrogen source is reacted.Further, described
The molal volume ratio of boron source and the solvent is (0.005-0.01) mol:10mL, specifically, mole of boron source and the solvent
Volume ratio is 0.005mol:10mL or 0.01mol:10mL etc..In the molal volume than in range, nitrogen source or boron source can be fine
Dissolution in a solvent, be more advantageous to subsequent hydro-thermal reaction.It in one embodiment, can be by boron source, nitrogen source, catalyst
1h is mixed in glass beaker with solvent, obtains precursor solution.
Further, in above-mentioned steps S02: the temperature of the hydro-thermal reaction is 260-300 DEG C；The hydro-thermal reaction
Mixing speed be 200-500rpm；The time of the hydro-thermal reaction is 12-24h；The hydro-thermal reaction in inert gas into
Row.Further, the inert gas is available but is not limited to nitrogen, argon gas, any one in carbon dioxide.
In one embodiment, precursor solution is transferred in hydrothermal reaction kettle, it is close that polytetrafluoro stirring magneton is added
Envelope opens gas valve, leads to inert gas 10min, closes gas valve.(mixing speed 200- under magnetic stirring
500rpm), reaction kettle is gradually heated to 260-300 DEG C, keeps the temperature 12-24h；The hydrothermal reaction condition makes the effect of hydro-thermal reaction
Fruit is best.
Further, in above-mentioned steps S03: the centrifugal treating includes: that acid solution is first added to carry out at the first centrifugation
Reason adds water and carries out the second centrifugal treating.In one embodiment, the reaction product of hydro-thermal reaction in step S02 is turned
Centrifuge tube is moved to, diluted acid is added and is centrifuged 2-5 times up to solvent is washed Cheng Wuse, adds deionized water and is centrifuged 2-5 times until upper
Clear liquid pH value is 7 or so.So obtain the boron nitride nanometer stick of higher purity.Further, above-mentioned first centrifugal treating
Centrifugal speed is 4000-10000rpm (rpm)；The centrifugal speed of above-mentioned second centrifugal treating is 4000-10000rpm.
Further, include the steps that after the centrifugal treating dry.In one embodiment, it can will be centrifuged
The centrifugation product obtained after processing dries 12h or so in a vacuum drying oven.
The present invention successively carried out test of many times, and it is further detailed as reference pair invention progress now to lift A partial experiment result
Thin description, is described in detail combined with specific embodiments below.
Embodiment 1
A kind of preparation method of BN nanometer rods, this method comprises the following steps:
S11: 1h is mixed in Boratex, glycine, sodium chloride and water in glass beaker, obtains precursor solution；
S12: precursor solution is transferred in hydrothermal reaction kettle, and polytetrafluoro stirring magneton sealing is added, opens breather valve
Door is passed through inert gas 10min, closes gas valve.(mixing speed 200-500rpm) under magnetic stirring, hydro-thermal is anti-
It answers kettle to be gradually heated to 260-300 DEG C, keeps the temperature 12-24h；
S13: after to hydro-thermal reaction, hydrothermal reaction kettle being placed in air and is cooled to room temperature, and is opened reaction kettle, will be produced
Object is transferred to centrifuge tube, diluted acid centrifugation (centrifugal speed 4000-10000rpm) is added 2-5 times until solvent is washed Cheng Wuse, then
Deionized water centrifugation (centrifugal speed 4000-10000rpm) is added 2-5 times until supernatant pH value is centrifuged 7 or so by product
12h is dried in a vacuum drying oven.
BN nanometer rods manufactured in the present embodiment characterize: relevant SEM (scanning electron microscope) image, XRD
(X-ray diffraction) spectrogram, TEM (transmission electron microscope) image, FFT (Fast Fourier Transform (FFT)) diffraction image are as shown in Figure 1.
It will be seen from figure 1 that the BN nanorod diameter that the present embodiment reacts is in 18-40 nanometer range, draw ratio is in 13-32 model
In enclosing, size is than more uniform.XRD is the results show that product is crystalline state orthorhombic phase BN (a=0.86nm, b=0.774nm, the c of pure phase
=0.635nm；α=β=γ=90 °) (illustration in Fig. 1 b).The pattern (Fig. 1 c) and scanning that transmission electron microscope (TEM) is observed
The consistent appearance that Electronic Speculum (SEM) is observed also is club shaped structure.And the high-resolution TEM lattice fringe and FFT diffraction of BN nanometer rods
Spot (Fig. 1 d) is consistent with XRD result, also illustrates the higher crystallinity of product and purity.I.e. it is mutually single to have obtained object for the present embodiment
One, the boron nitride nanometer stick of high-purity.
Embodiment 2
A kind of preparation method of BN nanometer rods, this method comprises the following steps:
S21: being mixed 1h for the mixed solvent of ammonium borate, glutamic acid, ammonium fluoride and water and ethyl alcohol in glass beaker,
Obtain precursor solution；
S22: precursor solution is transferred in hydrothermal reaction kettle, and polytetrafluoro stirring magneton sealing is added, opens breather valve
Door is passed through inert gas 10min, closes gas valve.(mixing speed 200-500rpm) under magnetic stirring, hydro-thermal is anti-
It answers kettle to be gradually heated to 260-300 DEG C, keeps the temperature 12-24h；
S23: after to hydro-thermal reaction, hydrothermal reaction kettle being placed in air and is cooled to room temperature, and is opened reaction kettle, will be produced
Object is transferred to centrifuge tube, diluted acid centrifugation (centrifugal speed 4000-10000rpm) is added 2-5 times until solvent is washed Cheng Wuse, then
Deionized water centrifugation (centrifugal speed 4000-10000rpm) is added 2-5 times until supernatant pH value will be centrifuged product 7 or so
12h is dried in a vacuum drying oven.
Embodiment 3
A kind of preparation method of BN nanometer rods, this method comprises the following steps:
S31: 1h is mixed in boric acid, tryptophan, ammonium chloride and water in glass beaker, obtains precursor solution；
S32: precursor solution is transferred in hydrothermal reaction kettle, and polytetrafluoro stirring magneton sealing is added, opens breather valve
Door is passed through inert gas 10min, closes gas valve.(mixing speed 200-500rpm) under magnetic stirring, hydro-thermal is anti-
It answers kettle to be gradually heated to 260-300 DEG C, keeps the temperature 12-24h；
S33: after to hydro-thermal reaction, hydrothermal reaction kettle being placed in air and is cooled to room temperature, and is opened reaction kettle, will be produced
Object is transferred to centrifuge tube, diluted acid centrifugation (centrifugal speed 4000-10000rpm) is added 2-5 times until solvent is washed Cheng Wuse, then
Deionized water centrifugation (centrifugal speed 4000-10000rpm) is added 2-5 times until supernatant pH value will be centrifuged product 7 or so
12h is dried in a vacuum drying oven.
Embodiment 4
A kind of preparation method of BN nanometer rods, this method comprises the following steps:
S41: triethyl borate, glutamic acid, sodium fluoride are mixed in glass beaker with the mixed solvent of water and isopropanol
1h is stirred, precursor solution is obtained；
S42: precursor solution is transferred in hydrothermal reaction kettle, and polytetrafluoro stirring magneton sealing is added, opens breather valve
Door is passed through inert gas 10min, closes gas valve.Under magnetic stirring, hydrothermal reaction kettle is gradually heated to 260-300
DEG C, keep the temperature 12-24h；
S43: after to hydro-thermal reaction, hydrothermal reaction kettle being placed in air and is cooled to room temperature, and is opened reaction kettle, will be produced
Object is transferred to centrifuge tube, diluted acid centrifugation (centrifugal speed 4000-10000rpm) is added 2-5 times until solvent is washed Cheng Wuse, then
Deionized water centrifugation (centrifugal speed 4000-10000rpm) is added 2-5 times until supernatant pH value will be centrifuged product 7 or so
12h is dried in a vacuum drying oven.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of preparation method of boron nitride nanometer stick, which comprises the steps of:
Boron source, nitrogen source, catalysts and solvents are provided；
Hydro-thermal reaction is carried out after the boron source, the nitrogen source, the catalyst and the solvent are mixed, obtains reaction product；
By the reaction product centrifugal treating, boron nitride nanometer stick is obtained.
2. the preparation method of boron nitride nanometer stick as described in claim 1, which is characterized in that the boron source includes boric acid, boron
At least one of sour sodium, ammonium borate, phenyl boric acid and triethyl borate.
3. the preparation method of boron nitride nanometer stick as described in claim 1, which is characterized in that the nitrogen source includes amino acid；
Wherein, the amino acid includes at least one of glycine, glutamic acid, sarcosine, tryptophan and phenylalanine.
4. the preparation method of boron nitride nanometer stick as described in claim 1, which is characterized in that the catalyst includes halogenation
Object；Wherein, the halide includes at least one of sodium chloride, sodium fluoride, ammonium fluoride and ammonium chloride.
5. the preparation method of boron nitride nanometer stick as described in claim 1, which is characterized in that the solvent include water and/or
Organic solvent；Wherein, the organic solvent includes at least one of ethyl alcohol, isopropanol, dimethylformamide and methanol.
6. the preparation method of boron nitride nanometer stick as described in any one in claim 1-5, which is characterized in that the boron source, institute
State nitrogen source, the range of the molar ratio of the catalyst is 10:(30-60): 1.
7. the preparation method of boron nitride nanometer stick as described in claim 1, which is characterized in that the temperature of the hydro-thermal reaction is
260-300℃；And/or
The time of the hydro-thermal reaction is 12-24h；And/or
The mixing speed of the hydro-thermal reaction is 200-500rpm；And/or
The hydro-thermal reaction carries out in inert gas.
8. the preparation method of boron nitride nanometer stick as described in claim 1, which is characterized in that the centrifugal treating includes: elder generation
Acid solution is added and carries out the first centrifugal treating, adds water and carries out the second centrifugal treating.
9. the preparation method of boron nitride nanometer stick as claimed in claim 8, which is characterized in that first centrifugal treating from
Heart speed is 4000-10000rpm；And/or
The centrifugal speed of second centrifugal treating is 4000-10000rpm.
10. the preparation method of boron nitride nanometer stick as described in claim 1, which is characterized in that after the centrifugal treating also
Include the steps that dry.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110577197A (en) * | 2018-06-11 | 2019-12-17 | 中国科学院深圳先进技术研究院 | Preparation method of boron nitride nanosheet |
| CN114558602A (en) * | 2022-01-26 | 2022-05-31 | 天津大学 | Copper-loaded porous boron nitride nanorod catalyst and preparation method and application thereof |
| CN114852976A (en) * | 2022-06-09 | 2022-08-05 | 桂林理工大学 | Hollow boron nitride short rod and preparation method thereof |
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| CN1597499A (en) * | 2004-09-01 | 2005-03-23 | 山东大学 | Phase selection in-situ synthesis method used for controlling boron nitride object phase |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110577197A (en) * | 2018-06-11 | 2019-12-17 | 中国科学院深圳先进技术研究院 | Preparation method of boron nitride nanosheet |
| CN114558602A (en) * | 2022-01-26 | 2022-05-31 | 天津大学 | Copper-loaded porous boron nitride nanorod catalyst and preparation method and application thereof |
| CN114558602B (en) * | 2022-01-26 | 2023-08-01 | 天津大学 | Copper-loaded porous boron nitride nanorod catalyst and preparation method and application thereof |
| CN114852976A (en) * | 2022-06-09 | 2022-08-05 | 桂林理工大学 | Hollow boron nitride short rod and preparation method thereof |
| CN114852976B (en) * | 2022-06-09 | 2023-06-23 | 桂林理工大学 | Hollow boron nitride short rod and preparation method thereof |
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