CN107827090B - A kind of microwave synthesis method of hexagonal boron nitride whisker - Google Patents
A kind of microwave synthesis method of hexagonal boron nitride whisker Download PDFInfo
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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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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
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- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
Abstract
The invention discloses a kind of microwave synthesis method of hexagonal boron nitride whisker, include the following steps: that, using nitrogen-rich organic object as nitrogen source, inorganic boride is boron source, using carbon fiber as microwave absorption；It is put into crucible after above-mentioned material is mixed, crucible is placed in High-Power Microwave furnace resonant cavity, microwave radiation heating is carried out under negative pressure, so that High-Power Microwave furnace resonant cavity is brought rapidly up to 900 DEG C or more, and insulation reaction, hexagonal boron nitride whisker can directly, rapidly be prepared, by adopting the above technical scheme, it realizes and fast and efficiently prepares boron nitride crystal whisker, and achieve preferable effect.
Description
Technical field
The present invention relates to the technology of preparing scopes of boron nitride crystal whisker, and in particular to and one kind is based on High-Power Microwave heating technique,
Fast and efficiently obtain the preparation method of hexagonal boron nitride whisker.
Background technique
Whisker refers to the fibrous one-dimensional material with certain draw ratio generated with single crystal form.Since its is ideal
Mono-crystalline structures, Atomic Arrangement high-sequential so that the defects of whisker is lower, thus have the function of mechanical property outstanding and
Characteristic.When as enhancing modified material, mechanical strength, toughness of composite material etc. may make to be improved significantly；And due to crystalline substance
It must be used as typical one-dimensional single crystal material, also there is advantage outstanding in terms of the functional characteristics such as heat transfer, conduction.Boron nitride ceramics tool
There are the excellent properties such as high temperature resistant, anti-oxidant, resistant to chemical etching, absorbable neutron, and there is lower dielectric constant and dielectric
Loss, has important application in leading-edge fields such as the thermal protection of carbon fiber surface antioxidant coating, atomic piles.
Boron nitride crystal whisker combines the excellent properties of boron nitride ceramics and crystal whisker materials, in composite material or functional material
Field suffers from important application.Especially for hexagonal boron nitride, since it is very similar with the layer structure of graphite,
There is the title of " white graphite ".But compared to graphite, hexagonal boron nitride has more stable physics, chemical stability.It is at high temperature
Oxidation resistance it is very excellent, be the ideal thermally protective materials of the advanced composite materials such as carbon fiber；And more it is interesting that more
The material of number excellent thermal conductivity generally also has ideal conductive characteristic, although and hexagonal boron nitride also has very high heat
Conductance, but it is non-conductive, there will be important value in terms of the functional applications such as the heat dissipation of ic substrate.Therefore, obtain and
It is one of the important object of material science and field of engineering technology concern using boron nitride crystal whisker.
It is worth noting that, the band gap of boron nitride is very wide, reach 4~6eV, dielectric constant and dielectric loss are respectively
3.2 and 0.2 × 10-3, and without magnetism, it is a kind of excellent electromagnetic wave transparent material, is not responded with microwave, therefore general synthetic nitrogen
Change the method for boron whisker, mainly by plasma method by borine (B2H6) and nitrogen gas is carried out in high frequency hydrogen plasma
Phase reaction, and whisker reinforcement material is generated on graphite matrix.It, will be using microwave technology quickly, efficiently in the present patent application
Ground prepares boron nitride crystal whisker, and achieves preferable effect.
Summary of the invention
The problem to be solved in the present invention is: utilizing High-Power Microwave irradiated heat technology, provides a kind of simple, effective acquisition nitrogen
Change the preparation method of boron whisker.To solve the above problems, " a kind of microwave synthesis side of effective acquisition boron nitride crystal whisker of the invention
Method " includes the following steps:
(1) raw material mixes: melamine (C3N6H6), dicyandiamide (C2N4H4), urea (CON2H4) or thiocarbamide (CSN2H4) etc.
For nitrogen source, with boric acid (H3BO3) or boron oxide (B2O3) be boron source, by the mass ratio of nitrogen source organic matter and carbon fiber be (60~
130): 1, the mass ratio (60~140) of boron source and carbon fiber: 1, it is mixed, above-mentioned material is then put into corundum or quartz
In crucible.
(2) microwave irradiation heats: the ceramic crucible in step (1) being put into the intracavitary center of microwave resonance, is vacuumized
To 5~20kPa；Adjusting microwave power is 4~7kW, is irradiated using High-Power Microwave, raw material is quickly heated up to 900~1200 DEG C,
Keep the temperature 5~25min after natural cooling, using violent energy exchange can directly, boron nitride crystal whisker is rapidly prepared.Institute
It obtains boron nitride crystal whisker product and is rendered as typical one-dimensional shape, length is about 5~60 μm, and diameter is about 0.5~10 μm, draw ratio
In (10~100): 1.
Microwave belongs to wavelength in 1mm~1m, electromagnetic wave of the frequency in 300G~300MHz, most common microwave heating frequency
Predominantly 2.45GHz.High-Power Microwave irradiation under, due to rapidly and efficiently energy transmission with exchange so that reaction mass is interior
It can quickly improve；And the special electromagnetic field environment that microwave irradiation is built and " non-thermal effect ", it will also cause reaction barrier
Change, unique synthesis advantage is shown in terms of material preparation.
Although hexagonal boron nitride has structure extremely similar with graphite, belongs to insulation, non-magnetic material, belong to allusion quotation
The electromagnetic wave transparent material of type does not respond microwave irradiation.The method of conventional synthesis boron nitride crystal whisker, mainly using graphite as
Substrate utilizes the template action of graphite, Pintsch process borine (B2H6) and nitrogen etc., it is anti-by gas phase in high-frequency plasma
It answers and forms hexagonal boron nitride.In the present application, selection and using can Pintsch process organic materials, and utilize carbon fiber
As microwave absorption and form controlling agent, based on violent energy exchange mode, by exciting activation and transient effect,
It realizes and boron nitride crystal whisker is fast and efficiently prepared.
By adopting the above technical scheme, it has the advantages that
(1) raw material is simple, the nitrogen sources such as melamine or dicyandiamide, urea, thiocarbamide organic matter, boric acid (H3BO3) or boron oxide
(B2O3) etc. boron sources and carbon fiber microwave absorption, be all the common material being easy to get.
(2) boron nitride crystal whisker, process flow letter can be obtained by direct microwave irradiation in preparation process simple process
It is single easy to operate.
(3) processing efficient reduces alleviation of the heat transfer to energy exchange and the extent of reaction using special body heat phase
It influences, and violent energy exchange, also provide enhanced combined coefficient.
(4) non-environmental-pollution in preparation process, it is environmental friendly, exhaust gas, waste liquid, waste residue etc. are not generated.
Detailed description of the invention
Scanning electron microscope (SEM) photo of 1 gained boron nitride crystal whisker of Fig. 1 embodiment.
X-ray diffraction (XRD) spectrogram of 1 gained boron nitride crystal whisker of Fig. 2 embodiment.
Specific embodiment
Below by specific embodiment, for a kind of microwave synthesis side of effective acquisition boron nitride crystal whisker of the present invention
Method makees further example explanation.
Comparative example 1 prepares boron nitride crystal whisker using precursor pyrolysis and hot pressing
(Tang Jie, Zhang Mingxia, Wang Chonghai, Xu Hongzhao, Li Chuanshan, the Tang Jian such as the Tang Jie of Shandong Industrial Ceramic Design Institute
Newly, Liu Gang, the preparation and its characterization of boron nitride crystal whisker, modern technologies ceramics, 2011, (2): 3-5), it will be certain first with water-bath
The distilled water of amount is warming up to 70 DEG C or so, and a certain amount of boric acid is added into the distilled water, is stirred continuously and is allowed to be completely dissolved.Again
Water temperature is continued to be heated to 95 DEG C or so, and adds a certain amount of melamine into the above boric acid solution, maintains water temperature 95
DEG C or so and continue with constant speed to be stirred continuously 30min, then cooled to room temperature, stand start to be precipitated after 20h it is white
Color fibre shape crystal.After filtering, drying, boron carbon nitrogen (BCN) precursor compound is obtained.First by this precursor in Muffle furnace
In 500 DEG C calcined, then made annealing treatment at 700 DEG C, finally by precursor in a nitrogen atmosphere in 1800 DEG C or so
Nitridation reaction is carried out, product is finally obtained.Product is observed by means of testing such as SEM, TEM as it can be seen that product is nitridation
Boron whisker, obtain diameter 0.1~3 μm, draw ratio 10~200:1 boron nitride crystal whisker.(Zhao such as the Zhao Lin of Shandong University
Woods, Zhang Yujun, Gong Hongyu, Zhao Dongliang, calcining and the influence except carbon temperature to boron nitride crystal whisker, artificial lens journal, 2010
(4): 922-925), equally using melamine and boric acid as raw material, heating water bath synthesis presoma is first passed through, then again through 1700
DEG C or so high temperature sintering and prepare product.Scanning electron microscope shows that products therefrom is needle-shaped BN whisker.
A kind of boron nitride crystal whisker/silicon nitride ceramic composite material of comparative example 2 and preparation method thereof
Zhang Yujun of Shandong University etc. (Zhang Yujun, Gong Hongyu, Tan's gravel, Zhao Dongliang, Li Jianquan, Zhao Lin, Ma Fuying, one
Kind boron nitride crystal whisker/silicon nitride ceramic composite material and preparation method thereof, application number: CN200910015257.3, publication number:
CN101555156), boron nitride crystal whisker, silicon nitride powder, sintering aid and other additive ball milling mixings are obtained into ceramic slurry；
Using injection forming, or slurry is used to isostatic cool pressing technological forming after dry, powder processed；Molding blank after drying, 5~
It is sintered 1700~1850 DEG C under 8MPa nitrogen atmosphere pressure, under conditions of heat preservation 1~3 hour, boron nitride crystal whisker/silicon nitride is made
Ceramic composite.The composite materials property is excellent, dielectric properties are good, temperature tolerance and ablation resistance are good, can be used for height
The preparation of performance antenna cover；Preparation method is simple, suitable for mass production for the material simultaneously.The patent is to utilize boron nitride
Whisker is modified material and prepares ceramic composite, and the preparation method of non-acquisition boron nitride crystal whisker.
3 high temperature and pressure synthesizing cubic boron nitride of comparative example
Using hexagonal boron nitride as raw material, it is close to or higher than 1700 DEG C in temperature, the high temperature that lowest pressure is 11~12GPa is high
Under the conditions of pressure, hexagonal boron nitride can be switched through as cubic boron nitride.Although being nitrogenized by using alkali and alkaline-earth metal, alkali and alkaline earth
Object, alkaline earth fluoro nitride, boric acid ammonium salt or inorganic fluoride etc. are used as catalyst, can reduce transition temperature and pressure, but
There is still a need for very high temperature and pressures, and the temperature and pressure as needed for making catalyst with boric acid ammonium salt is minimum, it also requires
Apply the high pressure of 5GPa or more at 1500 DEG C.Since the preparation condition of high temperature and pressure is harsh, the device is complicated, leads to preparation cost height
It is high.Especially high temperature and high pressure method mainly prepares this superhard material of cubic boron nitride by raw material of hexagonal boron nitride, not
Prepare hexagonal boron nitride.But it can also be seen that, hexagonal boron nitride is extremely stable from upper, high temperature, high pressure extreme condition under just have
Conversion reaction occurs for benefit, and preparation has certain difficulty.
4 chemical vapour deposition technique of comparative example (CVD)
Preparing function ceramics using CVD method is more common method.Gao et al. (R.Gao, L.Yin, C, Wang,
Y.Qi,N.Lun,L.Zhang,Y.X.Liu,L.Kang,X.Wang,High-yield synthesis of boron
nitride nanosheets with strong ultraviolet cathode luminescence emission,
J.Phys.Chem.C, 2009,113,15160-15165.) with diboron trioxide (B2O3) and melamine (C3H6N6) mixture
As presoma, thickness is prepared in the boron nitride nanosheet of 25~50nm under the conditions of 1100~1300 DEG C using CVD method.But
Ar/H must be used using CVD2Equal protective atmospheres are used as carrier gas, and flow rate of carrier gas is very slow that just to obtain crystallinity ideal
Material, it is tediously long to have accordingly resulted in preparation time, low yield, and Product Form is rendered as the nanometer of two-dimensional layer growth
Piece, rather than along one-dimension oriented fibrous whisker.
Embodiment 1
By melamine (C3N6H6) 130g, boric acid (H3BO3) 120g, carbon fiber 1g, it is uniformly mixed, and above-mentioned material is put
Enter in silica crucible.Crucible is put into togerther the intracavitary center of microwave resonance together with material again, is evacuated to 12kPa；It adjusts
Microwave power is 4kW, is irradiated using High-Power Microwave, and raw material is quickly heated up to 1150 DEG C, keeps the temperature natural cooling after 15min, benefit
With violent energy exchange can directly, boron nitride crystal whisker is rapidly prepared.
Using scanning electron microscope (SEM) and X-ray diffraction (XRD), to obtaining, product carries out pattern and ingredient characterizes, it was demonstrated that institute
Obtaining product is boron nitride crystal whisker.Fig. 1 is the SEM photograph of boron nitride crystal whisker, by photo morphology analysis it is found that boron nitride crystal whisker
Diameter is 0.5~5 μm, and length is 5~30 μm, and draw ratio is in (10~50): between 1.Fig. 2 is the XRD spectra of boron nitride crystal whisker,
(100) characteristic peak at (002) and the higher angle of diffraction near its 27 °, it was demonstrated that products therefrom belongs to hexagonal structure.
Embodiment 2
By dicyandiamide (C2N4H4) 85g, boron oxide (B2O3) 140g, carbon fiber 1g are uniformly mixed, and these materials are put into
In corundum crucible.Then crucible is put into togerther center in micro-wave oven resonant cavity together with material, is evacuated to 20kPa；It adjusts
Section microwave power is 4kW, is irradiated using High-Power Microwave, raw material is quickly heated up to 950 DEG C, micro-wave oven is closed after 10min, to anti-
Product is obtained after answering system to cool to room temperature with the furnace.Pattern is carried out to product and crystalline types carry out characterizing provable, gained
Product is boron nitride crystal whisker.For morphology analysis it is found that the diameter of boron nitride crystal whisker product is 0.5~8 μm, length is 5~40 μm, long
Diameter ratio is in (10~70): between 1.
Embodiment 3
With urea (CON2H4) 120g be nitrogen source, with boron oxide (B2O3) 140g be boron source, using 1g carbon fiber as microwave suction
Agent is received, above-mentioned material is placed in corundum crucible after evenly mixing, then corundum crucible is placed in High-Power Microwave together with material
The resonant cavity center of furnace.Micro-wave oven is evacuated to 15kPa, sets microwave power as 6kW, after temperature up to starting to protect after 1100 DEG C
Temperature closes micro-wave oven after 5min, and reaction system is with furnace natural cooling.
Product is as it can be seen that be attached with a large amount of pale powders in observation crucible on crucible bottom and wall.Pattern is carried out to product
Characterize with crystalline types provable, products therefrom is boron nitride crystal whisker.Morphology analysis is carried out to product it is found that nitridation
The diameter of boron whisker product is 0.5~10 μm, and length is 8~55 μm, and draw ratio is in (10~100): between 1.
Embodiment 4
By thiocarbamide (CSN2H4) 80g, boric acid (H3BO3) 120g and 1g carbon fiber uniformly mixes, it is then placed in quartz
In crucible, then corundum crucible is placed in the resonant cavity center of industrial High-Power Microwave furnace together with material.By microwave stove evacuation
To 5kPa, set microwave power as 7kW, after temperature up to starting to keep the temperature after 1200 DEG C, close micro-wave oven after 5min, reaction system with
Furnace natural cooling.
Product is as it can be seen that form many pale powders, as boron nitride crystal whisker in observation crucible on crucible bottom and wall.Benefit
With SEM electron microscope analysis sample it is found that the diameter of boron nitride crystal whisker is 2~10 μm, length be about 5~60 μm of draw ratios (10~
30): between 1.
Embodiment 5
By melamine (C3N6H6) 130g, boron oxide (B2O3) 70g and 1g carbon fiber uniformly mixes, be then placed in
In corundum crucible, then corundum crucible is placed in the resonant cavity center of industrial High-Power Microwave furnace together with material.Micro-wave oven is taken out
Vacuum sets microwave power as 5kW to 15kPa, after temperature up to starting to keep the temperature after 1050 DEG C, micro-wave oven is closed after 20min, is reacted
System is with furnace natural cooling.
Product is as it can be seen that form many pale powders, as boron nitride crystal whisker in observation crucible on crucible bottom and wall.Benefit
With SEM electron microscope analysis sample it is found that the diameter of boron nitride crystal whisker is 0.5~8 μm, length is about 5~50 μm, and draw ratio is (10
~60): between 1.
Embodiment 6
By dicyandiamide (C3N6H6) 90g, boric acid (H3BO3) 60g and 1g carbon fiber uniformly mixes, it is then placed in quartz
In crucible, then corundum crucible is placed in the resonant cavity center of industrial High-Power Microwave furnace together with material.By microwave stove evacuation
To 250Pa, microwave power is set as 6kW, after temperature up to starting to keep the temperature after 1150 DEG C, micro-wave oven, reaction system are closed after 15min
With furnace natural cooling.
Product in observation crucible is as it can be seen that form the fluffy pale powder of many accumulations, as nitrogen on crucible bottom and wall
Change boron whisker.Using SEM Electronic Speculum progress Morphology analysis product it is found that the diameter of boron nitride crystal whisker is 0.5~10 μm, length
About 5~60 μm, draw ratio is in (10~70): between 1.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of microwave synthesis method of hexagonal boron nitride whisker, which comprises the steps of: be with nitrogen-rich organic object
Nitrogen source, inorganic boride is boron source, using carbon fiber as microwave absorption；It is put into crucible after above-mentioned material is mixed, it will
Crucible is placed in High-Power Microwave furnace resonant cavity, microwave radiation heating is carried out under negative pressure, so that High-Power Microwave furnace resonant cavity is rapid
It is warming up to 900 DEG C or more, and insulation reaction, hexagonal boron nitride whisker can directly, rapidly be prepared.
2. a kind of microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that: the nitrogen source
For at least one of melamine, dicyandiamide, urea or thiocarbamide.
3. a kind of microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that: the boron source
For boric acid and/or boron oxide.
4. a kind of microwave synthesis method of hexagonal boron nitride whisker described in one of -3 according to claim 1, it is characterised in that: institute
The mass ratio for stating nitrogen source and carbon fiber microwave absorption is (60~130): 1.
5. a kind of microwave synthesis method of hexagonal boron nitride whisker described in one of -3 according to claim 1, it is characterised in that: institute
State the mass ratio (60~140) of boron source Yu carbon fiber microwave absorption: 1.
6. a kind of microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that: described is negative
Pressure is 5~20kPa of vacuum degree in resonant cavity.
7. a kind of microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that: the microwave
During irradiated heat, microwave power is 4~7kW.
8. a kind of microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that: the heat preservation
Temperature is 900~1200 DEG C when reaction.
9. a kind of microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that: the heat preservation
Reaction time is 5~25min.
10. a kind of microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that: the earthenware
Crucible is corundum crucible or silica crucible.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1164582A (en) * | 1997-03-07 | 1997-11-12 | 清华大学 | Method for preparation of nitride nanometre whisker by using carbon nanometre tube |
| CN101259960A (en) * | 2008-03-28 | 2008-09-10 | 山东大学 | Method for preparing boron nitride coating carbon nano-tube/nano-wire and boron nitride nano-tube |
| CN103910345A (en) * | 2014-03-24 | 2014-07-09 | 中国科学院深圳先进技术研究院 | Preparation method of boron nitride composite material |
| CN106542509A (en) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | A kind of efficient method for preparing class Graphene carbonitride |
-
2017
- 2017-10-31 CN CN201711039903.0A patent/CN107827090B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1164582A (en) * | 1997-03-07 | 1997-11-12 | 清华大学 | Method for preparation of nitride nanometre whisker by using carbon nanometre tube |
| CN101259960A (en) * | 2008-03-28 | 2008-09-10 | 山东大学 | Method for preparing boron nitride coating carbon nano-tube/nano-wire and boron nitride nano-tube |
| CN103910345A (en) * | 2014-03-24 | 2014-07-09 | 中国科学院深圳先进技术研究院 | Preparation method of boron nitride composite material |
| CN106542509A (en) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | A kind of efficient method for preparing class Graphene carbonitride |
Non-Patent Citations (2)
| Title |
|---|
| 氮化硼晶须氮化工艺及其生长机理;赵林等;《硅酸盐学报》;20140731;第42卷(第7期);全文 |
| 氮化硼晶须的制备及其表征;唐杰等;《现代技术陶瓷》;20110628(第2期);全文 |
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