CN107827090A - 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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- CN107827090A CN107827090A CN201711039903.0A CN201711039903A CN107827090A CN 107827090 A CN107827090 A CN 107827090A CN 201711039903 A CN201711039903 A CN 201711039903A CN 107827090 A CN107827090 A CN 107827090A
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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
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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
- C01P2004/00—Particle morphology
- 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, comprise the following steps：Using nitrogen-rich organic thing as nitrogen source, inorganic boride is boron source, and microwave absorption is used as by the use of carbon fiber；It is put into after above-mentioned material is mixed in crucible, crucible is placed in High-Power Microwave stove resonator, microwave radiation heating is carried out under negative pressure, so that High-Power Microwave stove resonator is brought rapidly up to more than 900 DEG C, and insulation reaction, you can directly, hexagonal boron nitride whisker is rapidly prepared, using above-mentioned technical proposal, realize and fast and efficiently prepare boron nitride crystal whisker, and achieve preferable effect.
Description
Technical field
The present invention relates to the technology of preparing category 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 technology
Whisker refers to the fibrous one-dimensional material with certain draw ratio generated with single crystal form.Because its is ideal
Mono-crystalline structures, Atomic Arrangement high-sequential so that the defects of whisker is relatively low, so as to prominent mechanical property and function
Characteristic.During as strengthening material modified, it may be such that mechanical strength, toughness of composite etc. are improved significantly；And due to crystalline substance
Typical one-dimensional single crystal material must be used as, also there is prominent advantage in terms of the functional characteristics such as heat transfer, conduction.Boron nitride ceramics has
There are the excellent properties such as high temperature resistant, anti-oxidant, resistant to chemical etching, absorbable neutron, and there is relatively low 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 or functional material
Field suffers from important application.Especially for hexagonal boron nitride, because it is very similar with the layer structure of graphite, therefore
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 preferable 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 typically also has preferable 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 application of function such as the radiating of ic substrate.Therefore, obtain and
It is one of material science and the important object of field of engineering technology concern using boron nitride crystal whisker.
It is worth noting that, the non-constant width of the band gap of boron nitride, reaches 4~6eV, dielectric constant and dielectric loss are respectively
3.2 and 0.2 × 10-3, and there is no magnetic, 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 enter promoting the circulation of qi in high frequency hydrogen plasma
Phase reaction, and whisker reinforcement material is generated on graphite matrix.In the present patent application, microwave technology will be utilized quick, efficient
Ground prepares boron nitride crystal whisker, and achieves preferable effect.
The content of the invention
The problem to be solved in the present invention is：Utilize High-Power Microwave irradiated heat technology, there is provided a kind of simple, effective acquisition nitrogen
Change the preparation method of boron whisker.A kind of to solve the above problems, " microwave synthesis side of effective acquisition boron nitride crystal whisker of the present invention
Method ", comprise 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 for (60~
130):1, the mass ratio (60~140) of boron source and carbon fiber:1, mixed, above-mentioned material is then put into corundum or quartz
In crucible.
(2) microwave irradiation heats：Ceramic crucible in step (1) is put into microwave resonance intracavitary center, vacuumized
To 5~20kPa；Regulation microwave power is 4~7kW, is irradiated using High-Power Microwave, and raw material is quickly heated up into 900~1200 DEG C,
Be incubated 5~25min after natural cooling, using violent energy exchange can directly, boron nitride crystal whisker is rapidly prepared.Institute
Obtain boron nitride crystal whisker product and be rendered as typical one-dimensional shape, its 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, and frequency is in 300G~300MHz electromagnetic wave, the most frequently used microwave heating frequency
Predominantly 2.45GHz.High-Power Microwave irradiation under, because energy transmission rapidly and efficiently is with exchanging so that reaction mass it is interior
Can quickly it improve；And the special electromagnetic field environment that microwave irradiation is built and " non-thermal effect ", it will also cause reaction barrier
Change, the synthesis advantage of uniqueness is shown in terms of material preparation.
Although hexagonal boron nitride belongs to insulation, non-magnetic material, belongs to allusion quotation with the structure extremely similar to graphite
The electromagnetic wave transparent material of type, microwave irradiation is not responded.The method of conventional synthesis boron nitride crystal whisker, mainly using graphite as
Substrate, utilize the template action of graphite, Pintsch process borine (B2H6) and nitrogen etc., it is anti-by gas phase in high-frequency plasma
Answer and form hexagonal boron nitride.In the present application, selection and using can Pintsch process organic materials, and utilize carbon fiber
As microwave absorption and morphology Control agent, based on violent energy exchange mode, by exciting activation and transient effect,
Realize and boron nitride crystal whisker is fast and efficiently prepared.
Using above-mentioned technical proposal, have the advantages that：
(1) raw material is simple, the nitrogen source such as melamine or dicyandiamide, urea, thiocarbamide organic matter, boric acid (H3BO3) or boron oxide
(B2O3) etc. boron source and carbon fiber microwave absorption, be all the common material being easy to get.
(2) preparation process simple process, direct microwave irradiation is passed through, you can obtain boron nitride crystal whisker, technological process letter
It is single easy to operate.
(3) processing efficient, heat transfer is reduced to energy exchange and the alleviation of the extent of reaction using special body phase heating
Influence, and violent energy exchange, it also provide enhanced combined coefficient.
(4) non-environmental-pollution in preparation process, it is environmental friendly, waste gas, waste liquid, waste residue etc. are not produced.
Brief description of the drawings
ESEM (SEM) photo of the gained boron nitride crystal whisker of Fig. 1 embodiments 1.
X-ray diffraction (XRD) spectrogram of the gained boron nitride crystal whisker of Fig. 2 embodiments 1.
Embodiment
Below by specific embodiment, for a kind of microwave synthesis side of effective acquisition boron nitride crystal whisker of the present invention
Method, make 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 of boron nitride crystal whisker and its sign, modern technologies ceramics, 2011, (2):3-5), 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 a certain amount of melamine is added into above boric acid solution, maintains water temperature 95
DEG C or so and continue with constant speed to be stirred continuously 30min, then naturally cool to room temperature, stand start after 20h to separate out it is white
Color fibre shape crystal.By filtering, after 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, finally obtains product.Product observe by means of testing such as SEM, TEM visible, product is nitridation
Boron whisker, diameter is obtained in 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 except influence of the 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.ESEM shows that products therefrom is needle-like BN whiskers.
2 a kind of boron nitride crystal whisker/silicon nitride ceramic composite material of comparative example 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 isostatic cool pressing technological forming will be used after slurry drying, powder processed；Molding blank after drying, 5~
1700~1850 DEG C under 8MPa nitrogen atmosphere pressure, insulation 1~3 hour under conditions of sinter, be made boron nitride crystal whisker/silicon nitride
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；The preparation method of the material is simple and easy simultaneously, is adapted to batch production.The patent is to utilize boron nitride
Whisker is material modified and prepare ceramic composite, and the preparation method of non-acquisition boron nitride crystal whisker.
The HTHP synthesizing cubic boron nitride of comparative example 3
Using hexagonal boron nitride as raw material, it is close to or higher than 1700 DEG C in temperature, the high temperature that minimum pressure is 11~12GPa is high
Under the conditions of pressure, hexagonal boron nitride can be switched through as cubic boron nitride.Although nitrogenized by using alkali and alkaline-earth metal, alkali and alkaline earth
Thing, alkaline earth fluoro nitride, boric acid ammonium salt or inorganic fluoride etc. are used as catalyst, can reduce transition temperature and pressure, but
Very high temperature and pressure is stilled need, the temperature and pressure as needed for making catalyst with boric acid ammonium salt is minimum, it also requires
Apply more than 5GPa high pressure at 1500 DEG C.Because the preparation condition of HTHP is harsh, equipment is complicated, causes to prepare cost height
It is high.Particularly high temperature and high pressure method, this superhard material of cubic boron nitride mainly is prepared 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 profit, and preparation has certain difficulty.
The chemical vapour deposition technique of comparative example 4 (CVD)
It is more conventional method to prepare function ceramics using CVD.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, boron nitride nanosheet of the thickness in 25~50nm is prepared under the conditions of 1100~1300 DEG C using CVD.But
Ar/H must be used using CVD2Deng protective atmosphere 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 well mixed, and above-mentioned material is put
Enter in silica crucible.Crucible is put into microwave resonance intracavitary center together with material again, is evacuated to 12kPa；Regulation
Microwave power is 4kW, is irradiated using High-Power Microwave, and raw material is quickly heated up into 1150 DEG C, is incubated natural cooling after 15min, profit
With violent energy exchange can directly, boron nitride crystal whisker is rapidly prepared.
Using ESEM (SEM) and X-ray diffraction (XRD), to obtaining, product carries out pattern and composition characterizes, it was demonstrated that institute
It is boron nitride crystal whisker to obtain product.Fig. 1 is the SEM photograph of boron nitride crystal whisker, by photo morphology analysis, boron nitride crystal whisker
A diameter of 0.5~5 μm, 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 well mixed, and these materials are put into
In corundum crucible.Then crucible is put into center in micro-wave oven resonator together with material, is evacuated to 20kPa；Adjust
Section microwave power is 4kW, is irradiated using High-Power Microwave, and raw material is quickly heated up into 950 DEG C, micro-wave oven is closed after 10min, is treated anti-
System is answered to obtain product after cooling 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.Morphology analysis understands that a diameter of 0.5~8 μm of boron nitride crystal whisker product, length is 5~40 μm, long
Footpath 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 fibers as microwave suction
Agent is received, corundum crucible will be inserted after above-mentioned material uniformly mixing, then corundum crucible is positioned over High-Power Microwave together with material
The resonator center of stove.Micro-wave oven is evacuated to 15kPa, sets microwave power as 6kW, after temperature up to starting to protect after 1100 DEG C
Temperature, micro-wave oven is closed after 5min, reaction system is with stove natural cooling.
Product is visible in observation crucible, and a large amount of pale powders are attached with crucible bottom and wall.Pattern is carried out to product
With crystalline types characterize provable, products therefrom is boron nitride crystal whisker.Morphology analysis is carried out to product to understand, nitridation
A diameter of 0.5~10 μm of boron whisker product, length are 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 fibers uniformly mix, and are then placed in quartz
In crucible, then corundum crucible is placed in the resonator center of industrial High-Power Microwave stove together with material.By microwave stove evacuation
To 5kPa, set microwave power as 7kW, after temperature up to starting to be incubated after 1200 DEG C, close micro-wave oven after 5min, reaction system with
Stove natural cooling.
Product is visible in observation crucible, and many pale powders, as boron nitride crystal whisker are formed in crucible bottom and wall.Profit
Understood with SEM electronic microscope photos sample, a diameter of 2~10 μm of boron nitride crystal whisker, 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 fibers uniformly mix, and are then placed in
In corundum crucible, then corundum crucible is placed in the resonator center of industrial High-Power Microwave stove together with material.Micro-wave oven is taken out
Vacuum sets microwave power as 5kW to 15kPa, after temperature up to starting to be incubated after 1050 DEG C, micro-wave oven is closed after 20min, is reacted
System is with stove natural cooling.
Product is visible in observation crucible, and many pale powders, as boron nitride crystal whisker are formed in crucible bottom and wall.Profit
Understand that a diameter of 0.5~8 μm of boron nitride crystal whisker, length is about 5~50 μm, and draw ratio is (10 with SEM electronic microscope photos sample
~60):Between 1.
Embodiment 6
By dicyandiamide (C3N6H6) 90g, boric acid (H3BO3) 60g, and 1g carbon fibers uniformly mix, and are then placed in quartz
In crucible, then corundum crucible is placed in the resonator center of industrial High-Power Microwave stove together with material.By microwave stove evacuation
To 250Pa, microwave power is set as 6kW, and after temperature up to starting to be incubated after 1150 DEG C, micro-wave oven, reaction system are closed after 15min
With stove natural cooling.
Product is visible in observation crucible, and the fluffy pale powder of many accumulations, as nitrogen are formed in crucible bottom and wall
Change boron whisker.Morphology analysis product is carried out using SEM Electronic Speculum to understand, a diameter of 0.5~10 μm of boron nitride crystal whisker, 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 can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent change or modification that Spirit Essence is made, it should all be included within the scope of the present invention.
Claims (10)
1. a kind of microwave synthesis method of hexagonal boron nitride whisker, it is characterised in that comprise the following steps：Using nitrogen-rich organic thing as
Nitrogen source, inorganic boride are boron source, and microwave absorption is used as by the use of carbon fiber；It is put into after above-mentioned material is mixed in crucible, will
Crucible is placed in High-Power Microwave stove resonator, carries out microwave radiation heating under negative pressure so that High-Power Microwave stove resonator is rapid
It is warming up to more than 900 DEG C, and insulation reaction, you can directly, hexagonal boron nitride whisker is rapidly prepared.
A kind of 2. microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that：The nitrogen source
It is at least one of nitrogen source for melamine, dicyandiamide, urea or thiocarbamide etc..
A kind of 3. microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that：The boron source
It is boron source for boric acid and/or boron oxide.
A kind of 4. microwave synthesis method of hexagonal boron nitride whisker according to one of claim 1-3, it is characterised in that：Institute
It is (60~130) to state nitrogen source and the mass ratio of carbon fiber microwave absorption:1.
A kind of 5. microwave synthesis method of hexagonal boron nitride whisker according to one of claim 1-3, it is characterised in that：Institute
State the mass ratio (60~140) of boron source and carbon fiber microwave absorption:1.
A kind of 6. microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that：Described is negative
Press as 5~20kPa of vacuum in resonator.
A kind of 7. 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.
A kind of 8. microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that：The insulation
Temperature is 900~1200 DEG C during reaction.
A kind of 9. microwave synthesis method of hexagonal boron nitride whisker according to claim 1, it is characterised in that：The insulation
Reaction time is 5~25min.
A kind of 10. 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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| CN113979766A (en) * | 2021-10-20 | 2022-01-28 | 哈尔滨工业大学（威海） | BCN/FexOy@CfPreparation process of/C composite structure wave-absorbing material |
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