CN101224876A - Method for preparing silicon nitride nano-wire and nano-strip - Google Patents
Method for preparing silicon nitride nano-wire and nano-strip Download PDFInfo
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- CN101224876A CN101224876A CNA2008100639274A CN200810063927A CN101224876A CN 101224876 A CN101224876 A CN 101224876A CN A2008100639274 A CNA2008100639274 A CN A2008100639274A CN 200810063927 A CN200810063927 A CN 200810063927A CN 101224876 A CN101224876 A CN 101224876A
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Abstract
The invention relates to a method for producing silicon nitride nanometer wire and nanometer band, which solves the problems that in the prior art for producing the silicon nitride nanometer wire and the nanometer band, the technique in preparation is complex, the cost is high and the environment can be polluted. The producing method is that: industrial silicon powder is poured into a crucible, then is sintered under the nitrogen atmosphere, and then is cooled to room temperature together with a furnace and the silicon nitride nanometer wire and the silicon nitride nanometer band can be obtained. The production method of silicon nitride nanometer wire and the nanometer band provided by the invention is simple in technique, low in cost and does not generate harmful gas to the environment.
Description
Technical field
The present invention relates to the preparation method of a kind of beta-silicon nitride nanowire and nano belt.
Background technology
Silicon nitride (Si
3N
4) be a kind of stupalith of excellent performance, two kinds of common variants are arranged, i.e. low temperature phase α-Si
3N
4With stable six sides β-Si mutually
3N
4Silicon nitride has under the hot conditions and keeps high strength, low density, and good erosion resistance, wear resistance, thermal shock performance, creep property, and excellent chemical stability etc.Silicon nitride still is a kind of wide bandgap semiconductor, can obtain higher doping content, thereby possesses the potentiality that become good host material, can be applicable to microelectronics and optoelectronic areas, thereby and can adjust its electronics and optical property by mixing.Along with science and technology development, one dimension Nano structure receives increasing the concern and attention with its excellent properties; Monodimension nanometer material comprises nanotube, nanometer rod, metal and semiconductor nanowires, coaxial nano cable, nano belt etc.Studies show that the 1-dimention nano silicon nitride material not only has outstanding mechanical property, also have very big application prospect at electronics and optical component field.
The method for preparing the 1-dimention nano silicon nitride material is a lot, classify according to raw material and preparation technology, mainly can be divided into the crystallization control method of the high-temperature ammonolysis reaction method of (1) carbon nanotube-template growth method, (2) nano-silicon powder or silica powder, nano-metal particle catalytic growth method that (3) utilize solid-liquid-mechanism of qi system, (4) autoclave low-temp reaction method, (5) amorphous nano boron nitride particle; Though the preparation method is different, ubiquity complex process, wayward, deficiencies such as cost is higher, contaminate environment have restricted the research and the application of 1-dimention nano silicon nitride material to a great extent.At present, have with SiCl
4And Na
3N is the feedstock production silicon nitride nanometer rod, but SiCl in the raw material
4Gas is very big to the human injury, causes environmental pollution easily, and the processing condition of preparation require very harsh, and the cost height is unfavorable for control and actual production; Name is called in the patent of " silicon nitride and silicon carbide one dimension Nano structure and preparation method thereof (China Patent No.: ZL03152915.1; the applying date: on 09 02nd, 2003; open day: on 04 28th, 2004) " has introduced metallic element as catalyzer, cause big difficulty to purification, technological process is numerous and diverse, is unfavorable for mass production.
Summary of the invention
The present invention seeks in order to solve higher, the problem of environment pollution caused of complicated process of preparation, cost of beta-silicon nitride nanowire and nano belt in the prior art, and the preparation method of a kind of beta-silicon nitride nanowire and nano belt is provided.
The preparation method of a kind of beta-silicon nitride nanowire and nano belt carries out according to the following steps: put into atmosphere sintering furnace behind the crucible of, industrial silica fume being packed into, vacuumize, make the vacuum tightness of atmosphere sintering furnace be lower than 10Pa; Two, in atmosphere sintering furnace, charge into nitrogen, make furnace gas pressure reach 0.1～2.0MPa; Three, atmosphere sintering furnace is warmed up to 1200～1600 ℃ with the speed of 5～30 ℃/min, and cools to room temperature with the furnace behind heat preservation sintering 5～360min, gets beta-silicon nitride nanowire and nano belt.
Selecting industrial silica fume among the preparation method of beta-silicon nitride nanowire of the present invention and nano belt for use is raw material; be beneficial to and obtain and reduce cost, easy, the easy handling of technology does not produce the obnoxious flavour of any contaminate environment in the reaction process; be beneficial to environmental protection and large-scale production, product is monocrystalline phase α-Si
3N
4The gained beta-silicon nitride nanowire, even thickness, diameter is 30～200nm, wherein based on 80～150nm, length controlled, the longest millimeter magnitude that reaches; Gained silicon nitride nano tape thickness is 40～60nm, and width is 180～220nm.
Description of drawings
Fig. 1 is the electron-microscope scanning figure of prepared beta-silicon nitride nanowire and nano belt in the embodiment seven.
Embodiment
Embodiment one: the preparation method of a kind of beta-silicon nitride nanowire of present embodiment and nano belt carries out according to the following steps: put into atmosphere sintering furnace behind the crucible of, industrial silica fume being packed into, vacuumize, make the vacuum tightness of atmosphere sintering furnace be lower than 10Pa; Two, in atmosphere sintering furnace, charge into nitrogen, make furnace gas pressure reach 0.1～2.0MPa; Three, atmosphere sintering furnace is warmed up to 1200～1600 ℃ with the speed of 5～30 ℃/min, and cools to room temperature with the furnace behind heat preservation sintering 5～360min, gets beta-silicon nitride nanowire and nano belt.
Embodiment two: present embodiment and embodiment one are different is that the diameter of particle of used industrial silica fume in the step 1 is 1～5 μ m.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is that the diameter of particle of used industrial silica fume in the step 1 is 3 μ m.Other step and parameter are identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is that furnace gas pressure reaches 1MPa in the step 2.Other step and parameter are identical with embodiment one.
Embodiment five: present embodiment and embodiment one are different is that atmosphere sintering furnace is warmed up to 1400 ℃ with the speed of 10 ℃/min in the step 3, and heat preservation sintering 100min.Other step and parameter are identical with embodiment one.
Embodiment six: present embodiment and embodiment one are different is that atmosphere sintering furnace is warmed up to 1500 ℃ with the speed of 15 ℃/min in the step 3, and heat preservation sintering 240min.Other step and parameter are identical with embodiment one.
Embodiment seven: the preparation method of a kind of beta-silicon nitride nanowire of present embodiment and nano belt carries out according to the following steps: put into atmosphere sintering furnace behind the crucible of, industrial silica fume being packed into, vacuumize, the vacuum tightness that makes atmosphere sintering furnace is 0.1Pa; Two, in atmosphere sintering furnace, charge into nitrogen, make furnace gas pressure reach 1MPa; Three, atmosphere sintering furnace is warmed up to 1500 ℃ with the speed of 13 ℃/min, and cools to room temperature with the furnace behind the heat preservation sintering 240min, gets beta-silicon nitride nanowire and nano belt.
The beta-silicon nitride nanowire and the nano belt of present embodiment preparation, as seen from Figure 1, the product pattern is nano wire and nano belt; Nanowire diameter is 60～120nm, and length reaches a millimeter magnitude; Nano belt thickness is 40～60nm, and width is 180～220nm.
Claims (6)
1. the preparation method of beta-silicon nitride nanowire and nano belt, the preparation method who it is characterized in that beta-silicon nitride nanowire and nano belt carries out according to the following steps: put into atmosphere sintering furnace behind the crucible of, industrial silica fume being packed into, vacuumize, make the vacuum tightness of atmosphere sintering furnace be lower than 10Pa; Two, in atmosphere sintering furnace, charge into nitrogen, make furnace gas pressure reach 0.1～2.0MPa; Three, atmosphere sintering furnace is warmed up to 1200～1600 ℃ with the speed of 5～30 ℃/min, and cools to room temperature with the furnace behind heat preservation sintering 5～360min, gets beta-silicon nitride nanowire and nano belt.
2. the preparation method of a kind of beta-silicon nitride nanowire according to claim 1 and nano belt, the diameter of particle that it is characterized in that used industrial silica fume in the step 1 is 1～5 μ m.
3. the preparation method of a kind of beta-silicon nitride nanowire according to claim 1 and nano belt, the diameter of particle that it is characterized in that used industrial silica fume in the step 1 is 3 μ m.
4. the preparation method of a kind of beta-silicon nitride nanowire according to claim 1 and nano belt is characterized in that furnace gas pressure reaches 1MPa in the step 2.
5. the preparation method of a kind of beta-silicon nitride nanowire according to claim 1 and nano belt is characterized in that atmosphere sintering furnace in the step 3 is warmed up to 1400 ℃ with the speed of 10 ℃/min, and heat preservation sintering 100min.
6. the preparation method of a kind of beta-silicon nitride nanowire according to claim 1 and nano belt is characterized in that atmosphere sintering furnace in the step 3 is warmed up to 1500 ℃ with the speed of 15 ℃/min, and heat preservation sintering 240min.
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| CN2008100639274A CN101224876B (en) | 2008-01-28 | 2008-01-28 | Method for preparing silicon nitride nano-wire and nano-strip |
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| CN2008100639274A CN101224876B (en) | 2008-01-28 | 2008-01-28 | Method for preparing silicon nitride nano-wire and nano-strip |
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| CN101224876B CN101224876B (en) | 2011-07-06 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807196A (en) * | 2012-08-26 | 2012-12-05 | 西安科技大学 | Method for preparing silicon nitride nano material |
| CN107342403A (en) * | 2017-06-09 | 2017-11-10 | 江永斌 | Nano material containing silicon nitride and its production and use |
| CN110436934A (en) * | 2019-07-09 | 2019-11-12 | 南昌大学 | A kind of preparation method of alpha-phase silicon nitride powder, overlength beta-silicon nitride nanowire |
| CN111620699A (en) * | 2020-06-03 | 2020-09-04 | 北京科技大学 | Ceramic sponge material with resilient nanofiber framework and preparation method thereof |
| 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 |
| CN116768635A (en) * | 2023-07-10 | 2023-09-19 | 兰溪泛翌精细陶瓷有限公司 | Modified silicon nitride composite material and preparation method thereof |
-
2008
- 2008-01-28 CN CN2008100639274A patent/CN101224876B/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807196A (en) * | 2012-08-26 | 2012-12-05 | 西安科技大学 | Method for preparing silicon nitride nano material |
| CN102807196B (en) * | 2012-08-26 | 2013-12-25 | 西安科技大学 | Method for preparing silicon nitride nano material |
| CN107342403A (en) * | 2017-06-09 | 2017-11-10 | 江永斌 | Nano material containing silicon nitride and its production and use |
| CN107342403B (en) * | 2017-06-09 | 2019-11-12 | 江永斌 | Nano material and its preparation method and application containing silicon nitride |
| CN110436934A (en) * | 2019-07-09 | 2019-11-12 | 南昌大学 | A kind of preparation method of alpha-phase silicon nitride powder, overlength beta-silicon nitride nanowire |
| CN110436934B (en) * | 2019-07-09 | 2022-02-11 | 南昌大学 | Preparation method of high alpha-phase silicon nitride powder and ultra-long silicon nitride nanowire |
| CN111620699A (en) * | 2020-06-03 | 2020-09-04 | 北京科技大学 | Ceramic sponge material with resilient nanofiber framework and preparation method thereof |
| CN111620699B (en) * | 2020-06-03 | 2021-08-17 | 北京科技大学 | Ceramic sponge material with resilient nanofiber framework and preparation method thereof |
| 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 |
| CN116768635A (en) * | 2023-07-10 | 2023-09-19 | 兰溪泛翌精细陶瓷有限公司 | Modified silicon nitride composite material and preparation method thereof |
| CN116768635B (en) * | 2023-07-10 | 2023-11-28 | 兰溪泛翌精细陶瓷有限公司 | Modified silicon nitride composite material and preparation method thereof |
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|---|---|
| CN101224876B (en) | 2011-07-06 |
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