CN101870470A - Preparation method of SiC nanowire in hierarchical structure - Google Patents
Preparation method of SiC nanowire in hierarchical structure Download PDFInfo
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- CN101870470A CN101870470A CN 201010193691 CN201010193691A CN101870470A CN 101870470 A CN101870470 A CN 101870470A CN 201010193691 CN201010193691 CN 201010193691 CN 201010193691 A CN201010193691 A CN 201010193691A CN 101870470 A CN101870470 A CN 101870470A
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Abstract
The invention discloses a preparation method of a SiC nanowire in a hierarchical structure, which comprises the following steps: preparing an SiC precursor mixed gel; drying and grinding the mixed gel into powder; putting the dry gel powder into a graphite crucible, putting into a high-temperature atmosphere furnace, vacuumizing and feeding argon as the protective gas; increasing the temperature of the high-temperature atmosphere furnace, and then insulating the heat and sintering; and naturally cooling the furnace to room temperature to obtain the SiC nanowire in the hierarchical structure. The preparation method of the SiC nanowire in the hierarchical structure has simple process and low cost, does not produce harmful gas polluting the environment, can effectively control the product appearance, and has wide application prospect in semi-conductor devices, nano composite materials, solar cells and catalysts.
Description
Technical field
The present invention relates to a kind of preparation method of SiC nano wire, especially relate to a kind of preparation method of SiC nanowire in hierarchical structure.
Background technology
The SiC nano wire has caused investigator's extensive concern with light, electricity and the mechanical property of the uniqueness that is better than its bulk material, has huge potential using value at the electronics and the optoelectronic areas of high temperature, high frequency, large power semiconductor device and nanoscale.Because performance and its pattern of material are closely related, therefore controlling SiC nano wire pattern and developing its application has become a present research focus.SiC nanowire in hierarchical structure is owing to have unique shape characteristic, can be used for manufacturing the photodecomposition catalyst of electromagnetic wave absorber/strainer, nanodevice member, solar cell, water and nano composite material etc.
At present, the method that is used for synthetic SiC nano wire has a lot, as carbothermic method, physical evaporation method, laser ablation method, pyrolysis precursor method and hydrothermal synthesis method etc.But the SiC nano wire of method for preparing generally presents slick surface, and shaggy nano wire particularly SiC nanowire in hierarchical structure report seldom, and the drawback that has complex process and be difficult to pattern is control effectively.Studies show that: hierarchy can realize effectively that with branched structure one dimension semiconductor nano material electronics separates with the hole, prolong carrier lifetime, thereby improve the electricity conversion (M.J.Bierman, S.Jin, Energy Environ.Sci.2 (2009) 1005-1120.) of nano material.Just because the excellent specific property of SiC nanowire in hierarchical structure and huge potential using value thereof, need that a kind of technology of exploitation is simple, cost is low, pollution-free, and can realize preparation method effective control of product pattern.
Summary of the invention
In order to solve SiC nanowire in hierarchical structure preparation difficulty, the object of the present invention is to provide technology simple and can effectively control the preparation method of a kind of SiC nanowire in hierarchical structure of pattern.。
The present invention is achieved by the following technical solutions, and concrete steps are as follows:
A, tetraethoxy are dissolved in the Virahol, add dilute hydrochloric acid to quicken teos hydrolysis, add carbon black particle then, magnetic agitation preparation mixed gel;
B, gel grind to form powdery 80～120 ℃ of dryings;
C, dry gel powder is put into plumbago crucible, place in the high-temperature atmosphere furnace, vacuumize and charge into argon gas as protection gas;
D, high-temperature atmosphere furnace are warmed up to 1400～1600 ℃, heat preservation sintering 1～9h with the speed of 3～15 ℃/min;
E, naturally cool to room temperature, promptly get SiC nanowire in hierarchical structure with stove.
Among the described step a, tetraethoxy: the mol ratio of carbon black particle is 1: 0.2～5, tetraethoxy: Virahol: the mol ratio of water is 1: 4: 4, and dilute hydrochloric acid concentration is 1～5mol/L.
Among the described step c, be evacuated to 10
2～10
4Pa, applying argon gas to 1～5 * 10
4Pressure is lower than 2MPa in the Pa, preparation process stove.
Described SiC nanowire in hierarchical structure is light green or canescence cotton shape material, grows in dry gel powder surface and crucible inwall, and diameter is 80～250nm, and length is 50～500 μ m.
Described SiC nanowire in hierarchical structure is a beta-SiC nano-wire.
The beneficial effect that the present invention has is:
With gelation SiO
2Be the silicon source, carbon black particle is that the SiC nanowire in hierarchical structure of carbon source preparation has following advantage: SiC nano wire purity height, and output is big; The SiC nanowire length is long, the longest 500 μ m that reach; SiC nano wire preparation technology is simple, raw material is easy to get, pollution-free and can realize effective control to pattern.
Description of drawings
Fig. 1 is the stereoscan photograph of product of the preparation method embodiment 1 of SiC nanowire in hierarchical structure of the present invention.
Fig. 2 is the stereoscan photograph of product of the preparation method embodiment 2 of SiC nanowire in hierarchical structure of the present invention.
Embodiment
Embodiment 1:
It is as follows that present embodiment prepares the SiC nanowire in hierarchical structure step:
A. tetraethoxy is dissolved in the Virahol, add 2mol/L dilute hydrochloric acid to promote teos hydrolysis, satisfy tetraethoxy: Virahol: the water mol ratio is 1: 4: 4, add carbon black particle then, make tetraethoxy: the carbon black particle mol ratio is 1: 1, magnetic agitation preparation mixed gel;
B. gel grinds to form powdery 110 ℃ of dryings;
C. dry gel powder is put into plumbago crucible, place high-temperature atmosphere furnace, be evacuated to 10
4Pa, applying argon gas to 2 * 10
4Pressure is lower than 2MPa in the Pa, preparation process stove;
D. high-temperature atmosphere furnace is warming up to 1550 ℃, heat preservation sintering 5h with the speed of 7 ℃/min;
E. naturally cool to room temperature with stove, promptly get SiC nanowire in hierarchical structure.
Fig. 1 is the stereoscan photograph of the product of embodiment 1.
Embodiment 2:
Present embodiment and embodiment 1 be different to be tetraethoxy among the step a: the carbon black particle mol ratio is 1: 2.Other steps are identical with embodiment 1.Fig. 2 is the stereoscan photograph of the product of embodiment 2.
Embodiment 3:
Present embodiment and embodiment 1 are different to be to add among the step a 1mol/L dilute hydrochloric acid to promote teos hydrolysis, and tetraethoxy: the carbon black particle mol ratio is 1: 0.2; Be evacuated to 10 among the step c
2Pa, applying argon gas to 10
4Pa; Speed with 3 ℃/min in the steps d is warmed up to 1400 ℃.Other steps are identical with embodiment 1.
Embodiment 4:
Present embodiment and embodiment 1 be different to be tetraethoxy among the step a: the carbon black particle mol ratio is 1: 5; Be evacuated to 10 among the step c
4Pa, applying argon gas to 5 * 10
4Pa; Speed with 15 ℃/min in the steps d is warmed up to 1600 ℃.Other steps are identical with embodiment 1.
Embodiment 5:
Present embodiment and embodiment 1 are different to be to add among the step a 5mol/L dilute hydrochloric acid to promote teos hydrolysis; Be evacuated to 10 among the step c
3Pa, applying argon gas to 3 * 10
4Pa; Speed with 10 ℃/min in the steps d is warmed up to 1500 ℃.Other steps are identical with embodiment 1.
Claims (5)
1. the preparation method of a SiC nanowire in hierarchical structure is characterized in that, SiC nanowire in hierarchical structure is the preparation method may further comprise the steps:
A, tetraethoxy are dissolved in the Virahol, add dilute hydrochloric acid to quicken teos hydrolysis, add carbon black particle then, magnetic agitation preparation mixed gel;
B, gel grind to form powdery 80～120 ℃ of dryings;
C, dry gel powder is put into plumbago crucible, place in the high-temperature atmosphere furnace, vacuumize and charge into argon gas as protection gas;
D, high-temperature atmosphere furnace are warmed up to 1400～1600 ℃, heat preservation sintering 1～9h with the speed of 3～15 ℃/min;
E, naturally cool to room temperature, promptly get SiC nanowire in hierarchical structure with stove.
2. the preparation method of a kind of SiC nanowire in hierarchical structure according to claim 1, it is characterized in that: among the described step a, tetraethoxy: the mol ratio of carbon black particle is 1: 0.2～5, tetraethoxy: Virahol: the mol ratio of water is 1: 4: 4, and dilute hydrochloric acid concentration is 1～5mol/L.
3. the preparation method of a kind of SiC nanowire in hierarchical structure according to claim 1 is characterized in that: among the described step c, be evacuated to 10
2～10
4Pa, applying argon gas to 1～5 * 10
4Pressure is lower than 2MPa in the Pa, preparation process stove.
4. the preparation method of a kind of SiC nanowire in hierarchical structure according to claim 1, it is characterized in that: described SiC nanowire in hierarchical structure is light green or canescence cotton shape material, grow in dry gel powder surface and crucible inwall, diameter is 80～250nm, and length is 50～500 μ m.
5. the preparation method of a kind of SiC nanowire in hierarchical structure according to claim 1, it is characterized in that: described SiC nanowire in hierarchical structure is the monocrystalline beta-SiC nano-wire.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718217A (en) * | 2012-05-18 | 2012-10-10 | 湖北大学 | High purity linear silicon carbide powder and preparation method |
| CN102730687A (en) * | 2012-07-05 | 2012-10-17 | 浙江理工大学 | Preparation method of SiC nanowire with expandable graphite as carbon source |
| CN103739002A (en) * | 2013-07-29 | 2014-04-23 | 南昌大学 | Preparation method of one-dimensional nanostructured material |
| CN104988658A (en) * | 2015-07-13 | 2015-10-21 | 浙江理工大学 | SiC nanometer fiber non-woven material preparation method |
| CN108394859A (en) * | 2018-02-01 | 2018-08-14 | 南京大学 | A kind of silicon substrate wide spectrum absorbs optical-thermal conversion material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008100863A (en) * | 2006-10-18 | 2008-05-01 | National Institute For Materials Science | Silicon carbide nanostructure and its producing method |
| CN101306816A (en) * | 2008-06-24 | 2008-11-19 | 陕西科技大学 | Method for synthesizing beta-SiC nano-wire |
-
2010
- 2010-06-04 CN CN 201010193691 patent/CN101870470A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008100863A (en) * | 2006-10-18 | 2008-05-01 | National Institute For Materials Science | Silicon carbide nanostructure and its producing method |
| CN101306816A (en) * | 2008-06-24 | 2008-11-19 | 陕西科技大学 | Method for synthesizing beta-SiC nano-wire |
Non-Patent Citations (2)
| Title |
|---|
| 《Journal of Crystal Growth》 20001231 G.W. Meng et al. Growth and characterization of nanostructured beta-SiC via carbothermal reduction of SiO2 xerogels containing carbon nanoparticles 801-806 1-5 第209卷, 2 * |
| 《纳米材料与技术应用进展--第四届全国纳米材料会议论文集》 20051201 魏剑 等 六棱柱状SiC纳米线的制备与表征 577-582 1-4 , 2 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718217A (en) * | 2012-05-18 | 2012-10-10 | 湖北大学 | High purity linear silicon carbide powder and preparation method |
| CN102718217B (en) * | 2012-05-18 | 2014-01-15 | 湖北大学 | High purity linear silicon carbide powder and preparation method |
| CN102730687A (en) * | 2012-07-05 | 2012-10-17 | 浙江理工大学 | Preparation method of SiC nanowire with expandable graphite as carbon source |
| CN102730687B (en) * | 2012-07-05 | 2014-04-16 | 浙江理工大学 | Preparation method of SiC nanowire with expandable graphite as carbon source |
| CN103739002A (en) * | 2013-07-29 | 2014-04-23 | 南昌大学 | Preparation method of one-dimensional nanostructured material |
| CN104988658A (en) * | 2015-07-13 | 2015-10-21 | 浙江理工大学 | SiC nanometer fiber non-woven material preparation method |
| CN104988658B (en) * | 2015-07-13 | 2017-10-20 | 浙江理工大学 | A kind of preparation method of SiC micro/nano-fibre non-woven materials |
| CN108394859A (en) * | 2018-02-01 | 2018-08-14 | 南京大学 | A kind of silicon substrate wide spectrum absorbs optical-thermal conversion material and preparation method thereof |
| CN108394859B (en) * | 2018-02-01 | 2021-09-10 | 南京大学 | Silicon-based wide-spectrum absorption photothermal conversion material and preparation method thereof |
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