CN104891456A - One-dimensional alpha-Si3N4 nano material and preparation method thereof - Google Patents
One-dimensional alpha-Si3N4 nano material and preparation method thereof Download PDFInfo
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- CN104891456A CN104891456A CN201510299826.7A CN201510299826A CN104891456A CN 104891456 A CN104891456 A CN 104891456A CN 201510299826 A CN201510299826 A CN 201510299826A CN 104891456 A CN104891456 A CN 104891456A
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Abstract
The invention provides a one-dimensional alpha-Si3N4 nano material and a preparation method thereof. The preparation method of the one-dimensional alpha-Si3N4 nano material comprises the following steps: (1) cleaning the surface of an aluminum oxide ceramic sheet, performing ultrasonic cleaning and then drying; (2) horizontally suspending the cleaned aluminum oxide ceramic sheet over a crucible filled with silicon monoxide powder; heating in a reaction furnace (which is vacuumized and continuously fed with nitriding gas in advance) at a speed of 5-15 DEG C/min to 1200-1600 DEG C, holding the temperature for 0.5-6h and then cooling to 1000 DEG C at a speed of 1-10 DEG C/min; and cooling to room temperature in the reaction furnace, thus obtaining the one-dimensional alpha-Si3N4 nano material. The yield of the one-dimensional alpha-Si3N4 nano material is high; the product is mainly composed of monocrystal-phase alpha-Si3N4; the product can be easily separated from raw materials; the product is controllable in morphology, good in crystallinity, few in defects and good in mechanical property; the whole process course is very simple and convenient, is easy to operate and low in cost.
Description
Technical field
The present invention relates to a kind of one dimension α-Si
3n
4nano material and preparation method thereof, being specifically related to a kind of take aluminum oxide as the one dimension α-Si of substrate
3n
4nano material and preparation method thereof.
Background technology
Along with the high speed development of spationautics, it proposes harsher requirement to high performance material performance under extreme conditions.Silicon nitride (Si
3n
4) be a kind ofly still can keep higher mechanical property under the high temperature conditions, have the stupalith of the excellent properties such as good erosion resistance, wear resistance, thermal shock resistance, it has two kinds of crystalline structure usually, i.e. α phase and β phase, and α-Si
3n
4comparatively β-Si
3n
4specific inductivity is lower.One-dimensional nano structure material (nanotube, nanometer rod, nano wire, nano belt etc.) receives increasing concern due to its good mechanical property and photoelectric characteristic, and 1-dimention nano α-Si
3n
4material crystalline degree is good, has good mechanical behavior under high temperature, and specific inductivity is lower simultaneously, has very large application prospect in high temperature wave-transparent material field.
The synthetic method of 1-dimention nano silicon nitride material roughly can classify as: vapor growth method, liquid-phase growth method and template.And wherein vapor growth method comparatively liquid-phase growth method and template have technique simple, low cost and other advantages, also has more pertinent literature to report.Vapor growth method comprises: a) vapor-liquid-solid (VLS) growth, namely by the acting growth one dimension silicon nitride nano-material of metal catalyst, as D. Liu etc. obtains beta-silicon nitride nanowire (D. Liu in 1200 DEG C in a nitrogen atmosphere on the monocrystalline silicon piece being coated with nickel, et al. Xi. Nanotechnology Materials and Devices Conference (NMDC), 2011), F. Wang etc. are prepared into xerogel by adding iron nitrate in tetraethoxy and resol, beta-silicon nitride nanowire (F. Wang is obtained in a nitrogen atmosphere at 1200 DEG C, et al. Materials Letters, 2006, 60:330-333), b) gas phase-solid phase (VS) growth, namely when there is no catalyzer, direct forming core growth of one-dimensional silicon nitride nano-material on matrix, as the Direct-Nitridation silicon wafer under 1200 DEG C of atmosphere with the mixed gas of ammonia and nitrogen such as T. Xie obtains beta-silicon nitride nanowire (T.Xie, et al. Physical.Status.Solidi. (a) 202, 2005, 10:1919-1924), F. Chen etc. process silica flour under liquid nitrogen condition, and be that raw material is at 1300 DEG C with it, beta-silicon nitride nanowire (F. Chen is obtained under nitrogen atmosphere, et al. ScriptaMaterialia, 2009, 60:737-740), Q.S Wang etc. then adopt DC arc discharge plasma apparatus to carry out synthesis (the Q.S Wang of beta-silicon nitride nanowire, et al. Journal of Crystal Growth, 2010, 312:2133-2136), c) Fabricated by Oxide-assisted Growth Mechanism, if J. Wang etc. is by nano silica fume preoxidation, has synthesized beta-silicon nitride nanowire (J. Wang, et al. Materials Letters, 2014,124:249-252) in 1390 DEG C in a nitrogen atmosphere, d) carbothermic reduction reaction, is carbon and mixes with oxide compound to produce and sub-be oxidized phase gaseous substance, the one dimension silicon nitride nano-material needed for then generating with gas reaction, if G.Y.Li etc. is by SiO
2powder mixes with chopped strand, obtains beta-silicon nitride nanowire (G.Y. Li, et al. Applied Physics, 2008,93:471-475) in a nitrogen atmosphere at 1430 DEG C, e) solution-liquid-gas phase-solid phase (SLGS) growth, namely separated out by the reaction of eutectic drop and gaseous substance, and at the Surface Creation nano wire of eutectic drop, as C.S. Zheng etc. with silica flour, polytetrafluorethylepowder powder and metal-powder for raw material, carry out reacting in high-pressure combustion vessel thus the mixture (C.S.Zheng obtaining SiC particle and beta-silicon nitride nanowire, et al. Ceramics International, 2012,38:4549-4554).Many synthetic methods all lay particular emphasis on the control to one dimension silicon nitride nano-material size above, therefore its output is often lower, simultaneously, its feed preparation process, process regulation is relative complex also, its product is more the application towards photoelectric device aspect, is difficult to suitability for industrialized production, is more difficult to meet the demand of high temperature wave-transparent material for amount.Therefore, invent a kind of technique simply, the one dimension silicon nitride nano-material synthetic route that output is larger has great significance for high temperature wave-transparent material development.
Also having with SiO in prior art is the method that one dimension silicon nitride nano-material prepared by raw material, as G.Z. Shen etc., in vertical high frequency furnace with the block SiO of 99.99% for raw material, obtain the one dimension silicon nitride nano-material of different-shape respectively at the different positions of plumbago crucible inwall, comprise micro belt, nanometer is sawed, the nano belt, (G.Z.Shen such as nano wire, et al. Chemical A European Journal, 2006,12,2987-2993.); L.W. Yin etc. are also by vertical high frequency induction furnace, with SiO and NH
3for raw material, take graphite as substrate, obtain the nano belt (L.W. Yin, et al. Applied Physics Letters, 2003,83:3584.) of silicon nitride at 1400 DEG C; But above-mentioned two kinds of methods all with graphite or plumbago crucible for substrate, being difficult to when being separated to avoid can the carbon of residual minim in the product, thus causes the rising of dielectric loss, and this is unfavorable for the application at electromagnetic wave transparent material; Y.H. Gao etc. by adding gac in SiO powder, at 1380 DEG C by having prepared silicon nitride nanometer rod with the reaction of nitrogen, but its product length is bottom plumbago crucible, be difficult to be separated with raw material, and little (Y.H. Gao, the et al. Microscopy and Microanalysis of output, 2002,8,5-10.), be unfavorable for the application of product in electromagnetic wave transparent material equally.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the above-mentioned defect that prior art exists, and provides a kind of preparation technology simple, equal not carbon containing in the reactant of employing or base material, the one dimension α-Si that product production is higher
3n
4nano material and 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 dimension α-Si
3n
4nano material, make in accordance with the following methods:
(1) choosing alumina ceramic plate is substrate, and alumina ceramic plate removing surface is clean, is placed in dehydrated alcohol ultrasonic cleaning, then carries out drying;
(2) the alumina ceramic plate level after step (1) process is suspended from the crucible that silicon monoxide powder is housed, continue after evacuation to pass in the Reaktionsofen of nitriding gas, with 5 ~ 15 DEG C/min(preferably 7 ~ 11 DEG C/min) heating rate to 1200 ~ 1600 DEG C after, insulation 0.5 ~ 6h(preferably 1 ~ 3.5h), then with 1 ~ 10 DEG C/min(preferably 3 ~ 6 DEG C/min) speed be cooled to 1000 DEG C, cool to room temperature with the furnace, obtain one dimension α-Si
3n
4nano material.
Further, in step (1), the purity >=90wt% of described alumina ceramic plate.Alumina-ceramic substrate is conducive to improving α-Si
3n
4the Enhancing Nucleation Density of monodimension nanometer material in crystal growth, because it is not containing carbon, makes the product of preparation purer;
Further, in step (1), the frequency of described ultrasonic cleaning is 20 ~ 80 kHz(preferably 25 ~ 60 kHz), the time is 0.5 ~ 24h.Concentration >=95% of described dehydrated alcohol.Ultrasonic cleaning is conducive to removing alumina-ceramic at the surface impurity prepared, process, transport and introduce in storage process.
Further, the time of described ultrasonic cleaning is 2 ~ 3h.
Further, in step (1), the temperature of described drying is 50 ~ 200 DEG C, and the dry time is 2 ~ 10h.Dry effect is the ethanol that when removing ultrasonic cleaning, alumina ceramic face adheres to and the moisture adsorbed in atmosphere.
Further, the temperature of described drying is 100 ~ 150 DEG C, and the dry time is 3 ~ 5h.
Further, in step (2), purity >=95% of described silicon monoxide powder.
Further ,≤10Pa is evacuated in step (2).
Further, in step (2), described nitriding gas is nitrogen and/or ammonia, and flow is 100 ~ 800mL/min(preferably 150 ~ 500mL/min), controlling air pressure is normal pressure ~ 1.0MPa(preferably 0.1 ~ 0.5MPa).Purity >=99% of described nitrogen, ammonia.
In step (2), described temperature rise rate, holding temperature, time, the selection of the factor range such as rate of temperature fall is conducive to the growth of crystal, if can not cause in above-mentioned scope, the pattern of product, thing are equal to change.
The principle of the inventive method is: silicon monoxide at high temperature decomposes, and then with nitriding atmosphere generation nitrogenizing reaction, generates α-Si
3n
4crystal, α-Si
3n
4crystal is forming core first on alumina substrates, then along preferential direction growth, forms monodimension nanometer material.
α-the Si when step (2) is heated to about 1400 DEG C
3n
4form be beta-silicon nitride nanowire, α-Si when being heated to about 1500 DEG C
3n
4form be the mixture of beta-silicon nitride nanowire and nano belt, α-Si when being heated to about 1600 DEG C
3n
4form be silicon nitride nano band, wherein the diameter of nano wire is 50 ~ 400nm, nano belt width < 1 μm, nano belt thickness is 50 ~ 300nm, the length of nano wire and nano belt is hundreds of micron ~ several millimeters of ranks, by can reach the regulation and control of pattern, size to the control of temperature, the material of different shape, feature is that later application lays the foundation.
The inventive method is pioneering is substrate with alumina ceramic plate, and research shows, its surface is that the growth of nano wire provides abundant forming core point, and can cover with white fluffy product on alumina ceramic plate surface, product is mainly monocrystalline phase α-Si
3n
4, output is comparatively large, one dimension α-Si
3n
4nano material reaches a millimeter magnitude, still belongs to rare; More obvious compared to existing graphite base advantage, product production is on alumina ceramic plate surface, and product is easily separated with raw material; Due to not carbon containing in starting material and base material, so product α-Si
3n
4in also not carbon containing, be conducive to the dielectric properties ensureing product; Product morphology is controlled, and can form non-woven fibrofelt, better crystallinity degree, defect is few, has good mechanical property; Whole technological process is extremely easy, easy handling, and initial feed is easy to acquisition, cost is low, can prepare a large amount of single shape product in one-time process.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 gained one dimension α-Si
3n
4the stereoscan photograph of nano material;
Fig. 2 is the embodiment of the present invention 1 gained one dimension α-Si
3n
4the XRD figure spectrum of nano material;
Fig. 3 is the embodiment of the present invention 1 gained one dimension α-Si
3n
4the transmission electron microscope photo of nano material;
Fig. 4 is the single one dimension α of the embodiment of the present invention 2 gained-Si
3n
4the stereoscan photograph of nano material;
Fig. 5 is the embodiment of the present invention 2 gained batch one dimension α-Si
3n
4the stereoscan photograph of nano material;
Fig. 6 is the embodiment of the present invention 2 gained one dimension α-Si
3n
4the optical photograph of nano material;
Fig. 7 is the embodiment of the present invention 3 gained one dimension α-Si
3n
4the stereoscan photograph of nano material.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
The alumina ceramic plate that the embodiment of the present invention uses and other chemical reagent used, if no special instructions, all obtained by routine business approach.
embodiment 1
(1) alumina ceramic plate (purity is 96%) removing surface is clean, be placed in dehydrated alcohol (purity is 97%), under 28 kHz frequencies, ultrasonic cleaning 2 h, then at 150 DEG C, dry 3h;
(2) the alumina ceramic plate level after step (1) process is suspended from the alumina crucible that silicon monoxide powder (purity is 99.9%) is housed, be placed in the graphite furnace continuing to pass into nitrogen (purity is 99.999%) after being evacuated to 10Pa, flow is 180mL/min, control air pressure is 0.1MPa, with after the heating rate to 1500 of 7 DEG C/min DEG C, insulation 2h, is then cooled to 1000 DEG C with the speed of 3 DEG C/min, cool to room temperature with the furnace, obtain one dimension α-Si
3n
4nano material.
As shown in Figure 1, prepared one dimension α-Si
3n
4nano material has beta-silicon nitride nanowire and nano belt two kinds of forms, and the diameter of nano wire is about 50 ~ 400nm, the width < of nano belt 1 μm, and thickness is for being about 300nm; As shown in Figure 2, prepared beta-silicon nitride nanowire and nano belt are mainly α phase; As shown in Figure 3, prepared beta-silicon nitride nanowire has good crystallization, and lattice perfection does not almost have defect, and the spacing of (010) crystal face is 0.672nm, fits like a glove with theoretical value.
embodiment 2
(1) alumina ceramic plate (purity is 94%) removing surface is clean, be placed in dehydrated alcohol (purity is 96%), under 40 kHz frequencies, ultrasonic cleaning 2.5 h, then at 100 DEG C, dry 5h;
(2) the alumina ceramic plate level after step (1) process is suspended from the alumina crucible that silicon monoxide powder (purity is 99%) is housed, be placed in the graphite furnace continuing to pass into nitrogen (purity is 99.999%) after being evacuated to 10Pa, flow is 360 mL/min, control air pressure is 0.1MPa, with after the heating rate to 1400 of 8 DEG C/min DEG C, insulation 3h, is then cooled to 1000 DEG C with the speed of 5 DEG C/min, cool to room temperature with the furnace, obtain one dimension α-Si
3n
4nano material.
Prepared one dimension α-Si
3n
4nano material form is beta-silicon nitride nanowire, and nanowire diameter is about 200nm, as shown in Figure 4.
As shown in Figure 5, the length of nano wire in enormous quantities is all more than 300 μm; As shown in Figure 6, the epontic nanowire length of alumina substrate can reach 3mm.For the application of this area, the diameter of monodimension nanometer material or width general control are in nanometer scale, and length is then that the longer the better, and the one dimension silicon nitride nano-material that the present invention reaches several millimeters of magnitudes still belongs to rare.
embodiment 3
(1) alumina ceramic plate (purity is 98%) removing surface is clean, be placed in dehydrated alcohol (purity is 97%), under 59 kHz frequencies, ultrasonic cleaning 3h, then at 120 DEG C, dry 4h;
(2) the alumina ceramic plate level after step (1) process is suspended from the alumina crucible that silicon monoxide powder (purity is 99.99%) is housed, be placed in the graphite furnace continuing to pass into ammonia (purity is 99.999%) after being evacuated to 10Pa, flow is 410 mL/min, control air pressure is 0.1MPa, with after the heating rate to 1600 of 10 DEG C/min DEG C, insulation 1h, is then cooled to 1000 DEG C with the speed of 4 DEG C/min, cool to room temperature with the furnace, obtain one dimension α-Si
3n
4nano material.
Prepared one dimension α-Si
3n
4nano material Main Morphology is silicon nitride nano band, and nano belt width is 300nm, and thickness is about 100 nm, as shown in Figure 7.
Claims (9)
1. an one dimension α-Si
3n
4nano material, is characterized in that, makes in accordance with the following methods:
(1) choosing alumina ceramic plate is substrate, and alumina ceramic plate removing surface is clean, is placed in dehydrated alcohol ultrasonic cleaning, then carries out drying;
(2) the alumina ceramic plate level after step (1) process is suspended from the crucible that silicon monoxide powder is housed, continue after evacuation to pass in the Reaktionsofen of nitriding gas, with behind heating rate to 1200 ~ 1600 of 5 ~ 15 DEG C/min DEG C, insulation 0.5 ~ 6h, then 1000 DEG C are cooled to the speed of 1 ~ 10 DEG C/min, cool to room temperature with the furnace, obtain one dimension α-Si
3n
4nano material.
2. one dimension α-Si according to claim 1
3n
4nano material, is characterized in that: in step (1), the purity>=90wt% of described alumina ceramic plate.
3. one dimension α-Si according to claim 1 or 2
3n
4nano material, is characterized in that: in step (1), and the frequency of described ultrasonic cleaning is 20 ~ 80 kHz, and the time is 0.5 ~ 24h.
4. one dimension α-Si according to claim 3
3n
4nano material, is characterized in that: the time of described ultrasonic cleaning is 2 ~ 3h.
5. according to the described one dimension α of one of Claims 1 to 4-Si
3n
4nano material, is characterized in that: in step (1), and the temperature of described drying is 50 ~ 200 DEG C, and the dry time is 2 ~ 10h.
6. one dimension α-Si according to claim 5
3n
4nano material, is characterized in that: the temperature of described drying is 100 ~ 150 DEG C, and the dry time is 3 ~ 5h.
7. according to the described one dimension α of one of claim 1 ~ 6-Si
3n
4nano material, is characterized in that: in step (2), purity>=95% of described silicon monoxide powder.
8. according to the described one dimension α of one of claim 1 ~ 7-Si
3n
4nano material, is characterized in that: step is evacuated to≤10Pa in (2).
9. according to the described one dimension α of one of claim 1 ~ 8-Si
3n
4nano material, is characterized in that: in step (2), and described nitriding gas is nitrogen and/or ammonia, and flow is 100 ~ 800mL/min, and controlling air pressure is normal pressure ~ 1.0MPa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047742A (en) * | 2020-09-03 | 2020-12-08 | 中钢南京环境工程技术研究院有限公司 | Low-cost preparation method of large-size silicon nitride nanobelt aerogel |
| CN114874016A (en) * | 2022-04-26 | 2022-08-09 | 滁州用朴新材料科技有限公司 | High-toughness and high-hardness silicon nitride ceramic cutter and preparation method thereof |
| CN115414798A (en) * | 2022-08-19 | 2022-12-02 | 电子科技大学长三角研究院(湖州) | Preparation method and application of silicon nitride-based ceramic separation membrane with micro-nano composite fiber structure |
| CN115537928A (en) * | 2022-09-19 | 2022-12-30 | 福建镓镒半导体材料有限公司 | Silicon nitride single crystal material and preparation method thereof |
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| JP2005170701A (en) * | 2003-12-09 | 2005-06-30 | National Institute For Materials Science | Method for producing single crystal alpha and beta silicon nitride nanoribbons |
| JP2005272208A (en) * | 2004-03-24 | 2005-10-06 | National Institute For Materials Science | METHOD FOR MANUFACTURING NANOBELT OF alpha-TYPE SILICON NITRIDE |
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| CN1164582A (en) * | 1997-03-07 | 1997-11-12 | 清华大学 | Method for preparation of nitride nanometre whisker by using carbon nanometre tube |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047742A (en) * | 2020-09-03 | 2020-12-08 | 中钢南京环境工程技术研究院有限公司 | Low-cost preparation method of large-size silicon nitride nanobelt aerogel |
| CN114874016A (en) * | 2022-04-26 | 2022-08-09 | 滁州用朴新材料科技有限公司 | High-toughness and high-hardness silicon nitride ceramic cutter and preparation method thereof |
| CN115414798A (en) * | 2022-08-19 | 2022-12-02 | 电子科技大学长三角研究院(湖州) | Preparation method and application of silicon nitride-based ceramic separation membrane with micro-nano composite fiber structure |
| CN115414798B (en) * | 2022-08-19 | 2024-03-29 | 电子科技大学长三角研究院(湖州) | Preparation method and application of silicon nitride-based ceramic separation membrane with micro-nano composite fiber structure |
| CN115537928A (en) * | 2022-09-19 | 2022-12-30 | 福建镓镒半导体材料有限公司 | Silicon nitride single crystal material and preparation method thereof |
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