CN104891456B - A kind of one-dimensional α Si3N4Nano material and preparation method thereof - Google Patents
A kind of one-dimensional α Si3N4Nano material and preparation method thereof Download PDFInfo
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Abstract
A kind of one-dimensional α Si3N4Nano material and preparation method thereof, the one-dimensional α Si3N4Nano material is made in accordance with the following methods：（1）Alumina ceramic plate removing surface is clean, it is cleaned by ultrasonic, then dry；（2）Alumina ceramic plate level after treatment is suspended from the crucible equipped with silicon monoxide powder, it is continually fed into the reacting furnace of nitriding gas after evacuation, after 1200~1600 DEG C being heated to the speed of 5~15 DEG C/min, 0.5~6h of insulation, then 1000 DEG C are cooled to the speed of 1~10 DEG C/min, cool to room temperature with the furnace, obtain one-dimensional α Si3N4Nano material.The one-dimensional α Si of the present invention3N4Nano material yield is larger, and product is mainly monocrystalline phase α Si3N4, product is easily separated with raw material；Product morphology is controllable, and better crystallinity degree, defect is few, there is preferable mechanical property；Whole technical process is extremely easy, easily operated, low cost.
Description
Technical field
The present invention relates to a kind of one-dimensional α-Si3N4Nano material and preparation method thereof, and in particular to one kind is with aluminum oxide as base
One-dimensional α-the Si at bottom3N4Nano material and preparation method thereof.
Background technology
With the high speed development of space technology, its performance to high performance material under extreme conditions proposes harsher
Requirement.Silicon nitride（Si3N4）It is that a kind of remaining unchanged under the high temperature conditions can keep mechanical property higher, with good anti-corruption
The ceramic material of the excellent properties such as corrosion, wearability, thermal shock resistance, it generally has a two kinds of crystal structures, i.e. α phases and β phases, and α-
Si3N4Compared with β-Si3N4Dielectric constant is lower.One-dimensional nano structure material（Nanotube, nanometer rods, nano wire, nanobelt etc.）Due to
Its good mechanical property and photoelectric characteristic and receive more and more attention, and 1-dimention nano α-Si3N4Material crystalline degree is good,
There is good mechanical behavior under high temperature, while dielectric constant is relatively low, have very big application prospect in high temperature wave-transparent material field.
The synthetic method of 1-dimention nano silicon nitride material can substantially be classified as：Vapor growth method, liquid-phase growth method and mould
Plate method.And wherein vapor growth method has process is simple compared with liquid-phase growth method and template, low cost and other advantages also have more phases
Close document report.Vapor growth method includes：a）Vapor-liquid-solid（VLS）Growth, i.e., given birth to by the effect of metallic catalyst
The one-dimensional silicon nitride nano-material of length, such as D. Liu are obtained in 1200 DEG C on the monocrystalline silicon piece for be coated with nickel in a nitrogen atmosphere
Beta-silicon nitride nanowire（D. Liu, et al. Xi. Nanotechnology Materials and Devices
Conference(NMDC), 2011）, F. Wang etc. are prepared into by adding ferric nitrate in tetraethyl orthosilicate and phenolic resin
Xerogel, in a nitrogen atmosphere in having obtained beta-silicon nitride nanowire at 1200 DEG C（F. Wang, et al. Materials
Letters, 2006, 60:330-333）；b）Gas phase-solid phase（VS）Growth, i.e., in the case of no catalyst, in matrix
Upper direct forming core growth of one-dimensional silicon nitride nano-material, such as T. Xie 1200 DEG C with ammonia and the gas of the mixed gas of nitrogen
Direct-Nitridation silicon wafer has obtained beta-silicon nitride nanowire under atmosphere（T.Xie,et al. Physical.Status.Solidi.(a)
202, 2005, 10:1919-1924）, F. Chen etc. process silica flour under the conditions of liquid nitrogen, and with its be raw material at 1300 DEG C,
Beta-silicon nitride nanowire is obtained under nitrogen atmosphere（F. Chen, et al. ScriptaMaterialia, 2009, 60:737-
740）, Q.S Wang etc. then carry out the synthesis of beta-silicon nitride nanowire using DC arc discharge plasma apparatus（Q.S Wang,
et al. Journal of Crystal Growth, 2010, 312:2133-2136）；c）Fabricated by Oxide-assisted Growth Mechanism, such as J.
Wang etc. pre-oxidizes nano silica fume, has synthesized beta-silicon nitride nanowire in 1390 DEG C in a nitrogen atmosphere（J. Wang, et al.
Materials Letters, 2014, 124:249-252）；d）It is sub- that carbothermic reduction reaction, as carbon mix generation with oxide
Oxidation phase gaseous material, then with the one-dimensional silicon nitride nano-material needed for gas reaction generation, such as G.Y.Li is by SiO2Powder
End mixes with chopped strand, in a nitrogen atmosphere in obtaining beta-silicon nitride nanowire at 1430 DEG C（G.Y. Li,et al.
Applied Physics, 2008, 93: 471-475）；e）Solution-liquid-gas phase-solid phase（SLGS）Growth, i.e., by altogether
The reaction of brilliant drop and gaseous material is separated out, and in the Surface Creation nano wire of eutectic drop, such as C.S. Zheng with silica flour,
Polytetrafluorethylepowder powder and metal dust are raw material, reacted in high-pressure combustion vessel thus obtained SiC particulate and
The mixture of beta-silicon nitride nanowire（C.S.Zheng, et al. Ceramics International, 2012, 38:4549-
4554）.More than many synthetic methods lay particular emphasis on control to one-dimensional silicon nitride nano-material size, therefore its yield often compared with
It is low, meanwhile, its feed preparation process, process regulation is also relative complex, and its product is more towards photoelectric device aspect
Application, it is difficult to industrialized production, it is more difficult to meet high temperature wave-transparent material for measure demand.Therefore, a kind of technique letter is invented
Single, the larger one-dimensional silicon nitride nano-material synthetic route of yield has great significance for high temperature wave-transparent material development.
Also there is the method for preparing one-dimensional silicon nitride nano-material as raw material with SiO in the prior art, such as G.Z. Shen,
Block SiO with 99.99% in vertical Efco-Northrup furnace is raw material, and the diverse location in graphite crucible inwall is obtained respectively
The one-dimensional silicon nitride nano-material of different-shape, including micro belt, nanometer saw, nanobelt, nano wire etc.（G.Z.Shen, et
al. Chemical A European Journal, 2006,12, 2987-2993.）；L.W. Yin etc. is also by vertical
Efco-Northrup furnace, with SiO and NH3It is raw material, with graphite as substrate, the nanobelt of silicon nitride has been obtained at 1400 DEG C（L.W.
Yin, et al. Applied Physics Letters, 2003, 83:3584.）；But above two method is with graphite
Or graphite crucible is substrate, be difficult to avoid that when separating can residual minim in the product carbon, so as to cause the liter of dielectric loss
Height, this is unfavorable for the application in electromagnetic wave transparent material；Y.H. Gao etc. is logical at 1380 DEG C by adding activated carbon in SiO powder
Cross and prepared silicon nitride nanometer rod with the reaction of nitrogen, but its product is long in graphite crucible bottom, it is difficult to separated with raw material, and
Yield is small（Y.H. Gao, et al. Microscopy and Microanalysis ,2002, 8, 5-10.）, equally not
Application beneficial to product in electromagnetic wave transparent material.
The content of the invention
The technical problems to be solved by the invention are the drawbacks described above for overcoming prior art to exist, there is provided one kind prepares work
Skill is simple, not carbon containing in the reactant or base material of use, product yield one-dimensional α-Si higher3N4Nano material and its
Take aluminum oxide as the preparation method of substrate Direct-Nitridation silicon monoxide.
The technical solution adopted for the present invention to solve the technical problems is as follows：A kind of one-dimensional α-Si3N4Nano material, according to
Following methods are made：
（1）Selection alumina ceramic plate is substrate, and alumina ceramic plate removing surface is clean, is placed in absolute ethyl alcohol and surpasses
Sound is cleaned, and is then dried；
（2）By step（1）Alumina ceramic plate level after treatment is suspended from the crucible equipped with silicon monoxide powder, is being taken out
It is continually fed into the reacting furnace of nitriding gas after vacuum, with 5~15 DEG C/min（It is preferred that 7~11 DEG C/min）Speed be heated to
After 1200~1600 DEG C, 0.5~6h is incubated（It is preferred that 1~3.5h）, then with 1~10 DEG C/min（It is preferred that 3~6 DEG C/min）Speed
Degree is cooled to 1000 DEG C, cools to room temperature with the furnace, obtains one-dimensional α-Si3N4Nano material.
Further, step（1）In, the purity >=90wt% of the alumina ceramic plate.Aluminium oxide ceramics substrate is conducive to carrying
α-Si high3N4Enhancing Nucleation Density of the monodimension nanometer material in crystal growth, because it does not contain carbon so that the product of preparation is more
It is pure；
Further, step（1）In, the frequency of the ultrasonic cleaning is 20~80 kHz（It is preferred that 25~60 kHz）, the time
It is 0.5~24h.Concentration >=95% of the absolute ethyl alcohol.Ultrasonic cleaning is conducive to removal aluminium oxide ceramics in preparation, processing, fortune
The surface impurity introduced during defeated and storage.
Further, the time of the ultrasonic cleaning is 2~3h.
Further, step（1）In, the dry temperature is 50~200 DEG C, and the dry time is 2~10h.It is dry
Effect is the ethanol of alumina ceramic face attachment and the moisture for adsorbing in atmosphere when removal is cleaned by ultrasonic.
Further, the dry temperature is 100~150 DEG C, and the dry time is 3~5h.
Further, step（2）In, purity >=95% of the silicon monoxide powder.
Further, step（2）In be evacuated to≤10Pa.
Further, step（2）In, the nitriding gas are nitrogen and/or ammonia, and flow is 100~800mL/min（It is excellent
Select 150~500mL/min）, it is normal pressure~1.0MPa to control air pressure（It is preferred that 0.1~0.5MPa）.The purity of the nitrogen, ammonia
≥99%。
Step（2）In, the heating rate, holding temperature, time, the factor range such as rate of temperature fall is advantageously selected for crystalline substance
The growth of body, if can not cause within the above range, the pattern of product, thing are equal to change.
The principle of the inventive method is：Silicon monoxide is decomposed at high temperature, and it is anti-that nitridation then occurs with nitriding atmosphere
Should, generation α-Si3N4Crystal, α-Si3N4Crystal forming core on alumina substrates first, then grows along preferential direction, forms one
Dimension nano material.
Work as step（2）It is heated to α-Si at 1400 DEG C or so3N4Form be beta-silicon nitride nanowire, be heated to 1500 DEG C of left sides
α-Si when right3N4Form be the mixture of beta-silicon nitride nanowire and nanobelt, be heated to α-Si at 1600 DEG C or so3N4Shape
State be silicon nitride nano band, wherein a diameter of 50~400nm of nano wire, 1 μm of nanometer bandwidth ＜, nanometer tape thickness be 50~
The length of 300nm, nano wire and nanobelt is hundreds of microns~several millimeters rank, and shape is can reach by the control to temperature
The regulation and control of looks, size, different shape, the material of feature are that later application lays the foundation.
The inventive method is pioneering with alumina ceramic plate as substrate, and research shows, its surface provides for the growth of nano wire
Abundant forming core point, white fluffy product can be covered with alumina ceramic plate surface, and product is mainly monocrystalline phase α-Si3N4,
Yield is larger, one-dimensional α-Si3N4Nano material reaches millimeter magnitude, still belongs to rare；Compared to existing graphite base advantage more
Substantially, on alumina ceramic plate surface, product can be easily separated product production with raw material；Due to being free of in raw material and base material
Carbon, so product α-Si3N4In it is also not carbon containing, advantageously ensure that the dielectric properties of product；Product morphology is controllable, can form nonwoven
Fibrofelt, better crystallinity degree, defect is few, there is preferable mechanical property；Whole technical process is extremely easy, easily operated, initial feed
Be easily obtained, low cost, a large amount of single shape products can be prepared in one-time process.
Brief description of the drawings
Fig. 1 is the one-dimensional α-Si of the gained of the embodiment of the present invention 13N4The stereoscan photograph of nano material；
Fig. 2 is the one-dimensional α-Si of the gained of the embodiment of the present invention 13N4The XRD spectrum of nano material；
Fig. 3 is the one-dimensional α-Si of the gained of the embodiment of the present invention 13N4The transmission electron microscope photo of nano material；
Fig. 4 is the single one-dimensional α-Si of the gained of the embodiment of the present invention 23N4The stereoscan photograph of nano material；
Fig. 5 is the one-dimensional α-Si of the gained batch of the embodiment of the present invention 23N4The stereoscan photograph of nano material；
Fig. 6 is the one-dimensional α-Si of the gained of the embodiment of the present invention 23N4The optical photograph of nano material；
Fig. 7 is the one-dimensional α-Si of the gained of the embodiment of the present invention 33N4The stereoscan photograph of nano material.
Specific embodiment
With reference to embodiment and accompanying drawing, the invention will be further described.
The alumina ceramic plate that the embodiment of the present invention is used and the chemical reagent that other are used, unless otherwise specified,
Obtained by routine business approach.
Embodiment 1
（1）By alumina ceramic plate（Purity is 96%）Removing surface is clean, is placed in absolute ethyl alcohol（Purity is 97%）In,
Under 28 kHz frequencies, it is cleaned by ultrasonic 2 h, then at 150 DEG C, dries 3h；
（2）By step（1）Alumina ceramic plate level after treatment is suspended from equipped with silicon monoxide powder（Purity is 99.9%）
Alumina crucible on, be placed in after being evacuated to 10Pa and be continually fed into nitrogen（Purity is 99.999%）Graphite furnace in, flow is
180mL/min, controls air pressure for 0.1MPa, after being heated to 1500 DEG C with the speed of 7 DEG C/min, 2h is incubated, then with 3 DEG C/min
Speed be cooled to 1000 DEG C, cool to room temperature with the furnace, obtain one-dimensional α-Si3N4Nano material.
As shown in figure 1, prepared one-dimensional α-Si3N4Nano material has two kinds of forms of beta-silicon nitride nanowire and nanobelt,
The diameter of nano wire is about 50~400nm, 1 μm of the width ＜ of nanobelt, and thickness is about 300nm；As shown in Fig. 2 prepared
Beta-silicon nitride nanowire and nanobelt be mainly α phases；As shown in figure 3, prepared beta-silicon nitride nanowire has preferably crystallization, it is brilliant
Lattice are complete, and almost without defect, the interplanar distance of (010) crystal face is 0.672nm, is fitted like a glove with theoretical value.
Embodiment 2
（1）By alumina ceramic plate（Purity is 94%）Removing surface is clean, is placed in absolute ethyl alcohol（Purity is 96%）In,
Under 40 kHz frequencies, it is cleaned by ultrasonic 2.5 h, then at 100 DEG C, dries 5h；
（2）By step（1）Alumina ceramic plate level after treatment is suspended from equipped with silicon monoxide powder（Purity is 99%）'s
On alumina crucible, it is placed in after being evacuated to 10Pa and is continually fed into nitrogen（Purity is 99.999%）Graphite furnace in, flow is
360 mL/min, control air pressure for 0.1MPa, after being heated to 1400 DEG C with the speed of 8 DEG C/min, are incubated 3h, then with 5 DEG C/
The speed of min is cooled to 1000 DEG C, cools to room temperature with the furnace, obtains one-dimensional α-Si3N4Nano material.
Prepared one-dimensional α-Si3N4Nano material form is beta-silicon nitride nanowire, and nanowire diameter is about 200nm, is such as schemed
Shown in 4.
As shown in figure 5, the length of high-volume nano wire is more than 300 μm；As shown in fig. 6, alumina base basal surface is given birth to
Nanowire length long is up to 3mm.For this area is applied, the diameter or width general control of monodimension nanometer material is being received
Rice magnitude, and length is then that the longer the better, the one-dimensional silicon nitride nano-material that the present invention reaches several millimeters magnitude still belongs to rare.
Embodiment 3
（1）By alumina ceramic plate（Purity is 98%）Removing surface is clean, is placed in absolute ethyl alcohol（Purity is 97%）In,
Under 59 kHz frequencies, it is cleaned by ultrasonic 3h, then at 120 DEG C, dries 4h；
（2）By step（1）Alumina ceramic plate level after treatment is suspended from equipped with silicon monoxide powder（Purity is
99.99%）Alumina crucible on, be placed in after being evacuated to 10Pa and be continually fed into ammonia（Purity is 99.999%）Graphite furnace
In, flow is 410 mL/min, controls air pressure for 0.1MPa, after being heated to 1600 DEG C with the speed of 10 DEG C/min, is incubated 1h, so
1000 DEG C are cooled to the speed of 4 DEG C/min afterwards, room temperature is cooled to the furnace, one-dimensional α-Si are obtained3N4Nano material.
Prepared one-dimensional α-Si3N4Nano material Main Morphology is silicon nitride nano band, and nanometer bandwidth is 300nm, thick
It is 100 nm or so to spend, as shown in Figure 7.
Claims (16)
1. a kind of one-dimensional α-Si3N4Nano material, it is characterised in that be made in accordance with the following methods：
（1）Selection alumina ceramic plate is substrate, and alumina ceramic plate removing surface is clean, is placed in ultrasound in absolute ethyl alcohol clear
Wash, be then dried；The frequency of the ultrasonic cleaning is 25~60 kHz, and the time is 2~3h；
（2）By step（1）Alumina ceramic plate level after treatment is suspended from the crucible equipped with silicon monoxide powder, is being vacuumized
It is continually fed into the reacting furnace of nitriding gas afterwards, after being heated to 1200~1600 DEG C with the speed of 7~11 DEG C/min, insulation 1.0
~3.5h, is then cooled to 1000 DEG C with the speed of 3~6 DEG C/min, cools to room temperature with the furnace, obtains one-dimensional α-Si3N4Nanometer material
Material.
2. one-dimensional α-Si according to claim 13N4Nano material, it is characterised in that：Step（1）In, the aluminium oxide ceramics
Purity >=the 90wt% of piece.
3. one-dimensional α-Si according to claim 1 or claim 23N4Nano material, it is characterised in that：Step（1）In, it is described dry
Temperature is 50~200 DEG C, and the dry time is 2~10h.
4. one-dimensional α-Si according to claim 33N4Nano material, it is characterised in that：The dry temperature is 100~150
DEG C, the dry time is 3~5h.
5. one-dimensional α-Si according to claim 1 or claim 23N4Nano material, it is characterised in that：Step（2）In, an oxidation
Purity >=95% of Si powder.
6. one-dimensional α-Si according to claim 33N4Nano material, it is characterised in that：Step（2）In, the silicon monoxide powder
Purity >=95% at end.
7. one-dimensional α-Si according to claim 43N4Nano material, it is characterised in that：Step（2）In, the silicon monoxide powder
Purity >=95% at end.
8. one-dimensional α-Si according to claim 1 or claim 23N4Nano material, it is characterised in that：Step（2）In be evacuated to≤
10Pa。
9. one-dimensional α-Si according to claim 33N4Nano material, it is characterised in that：Step（2）In be evacuated to≤10Pa.
10. one-dimensional α-Si according to claim 43N4Nano material, it is characterised in that：Step（2）In be evacuated to≤
10Pa。
11. one-dimensional α-Si according to claim 53N4Nano material, it is characterised in that：Step（2）In be evacuated to≤
10Pa。
12. one-dimensional α-Si according to claim 1 or claim 23N4Nano material, it is characterised in that：Step（2）In, the nitridation gas
Body is nitrogen and/or ammonia, and flow is 100~800mL/min, and it is normal pressure~1.0MPa to control air pressure.
13. one-dimensional α-Si according to claim 33N4Nano material, it is characterised in that：Step（2）In, the nitriding gas
It is nitrogen and/or ammonia, flow is 100~800mL/min, it is normal pressure~1.0MPa to control air pressure.
14. one-dimensional α-Si according to claim 43N4Nano material, it is characterised in that：Step（2）In, the nitriding gas
It is nitrogen and/or ammonia, flow is 100~800mL/min, it is normal pressure~1.0MPa to control air pressure.
15. one-dimensional α-Si according to claim 53N4Nano material, it is characterised in that：Step（2）In, the nitriding gas
It is nitrogen and/or ammonia, flow is 100~800mL/min, it is normal pressure~1.0MPa to control air pressure.
16. one-dimensional α-Si according to claim 83N4Nano material, it is characterised in that：Step（2）In, the nitriding gas
It is nitrogen and/or ammonia, flow is 100~800mL/min, it is normal pressure~1.0MPa to control air pressure.
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