CN101186297A - Method for preparing silicon carbide nano-wire with periodical twin crystal structure - Google Patents
Method for preparing silicon carbide nano-wire with periodical twin crystal structure Download PDFInfo
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- CN101186297A CN101186297A CNA2007101854678A CN200710185467A CN101186297A CN 101186297 A CN101186297 A CN 101186297A CN A2007101854678 A CNA2007101854678 A CN A2007101854678A CN 200710185467 A CN200710185467 A CN 200710185467A CN 101186297 A CN101186297 A CN 101186297A
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Abstract
The invention relates to a preparation method of silicon carbide nano-wire having periodic twin structure. Biphenyl is dissolved in acetone; nitrate is added and dissolved, tetraethyl orthosilicate is added into the solution and well mixed to be hydrolyzed to form sol; hexamethylene tetramine is added in the sol to form gel and the obtained gel is dried for 5-30h at the temperature of 80-110 DEG C to obtain dry gel; the dry gel is heated to 1200-1400 DEG C to be constantly reacted for 3-20h under the condition of argon, naturally cooled to room temperature, oxidized for 1-6h at the temperature of 600-800 DEG C, pickled by hydrochloride and hydrofluoric acid, then is cleaned by water and dried, and at last the silicon carbide nano-wire having periodic twin structure is obtained. The invention has the advantages of low production cost, low reaction temperature and simple and straightforward technique.
Description
Technical field
The present invention relates to a kind of preparation of nanomaterials, relate to a kind of preparation method specifically with silicon carbide nanometer line of periodical twin crystal structure.
Background technology
The wire nano material all has extremely important application at aspects such as electronics, photoelectron, machineries, and physics that it is excellent and chemical property have caused showing great attention to of scientific worker.As a kind of important semi-conductor and stupalith, silicon carbide nanometer line becomes one of research focus because of its special physics and chemical property, they have high physics, chemical stability, high conductivity, specific inductivity is low, energy gap is big, characteristics such as corrosion-resistant and anti-oxidant, make it have broad application prospects aspect semiconducter device of high temperature, high frequency, anti-irradiation; Mechanical propertys such as excellent elasticity, hardness, toughness make it can be used as the toughener that matrixes such as pottery, metal and polymkeric substance meet material.In addition, silicon carbide nanometer line has also shown special optics and electrology characteristic, makes it that important application prospect arranged aspect microelectronics and the photoelectron technology.
The character of silicon carbide nanometer line is relevant with its microscopic appearance, and in order to obtain the nanometer silicon carbide structured material of various patterns, people have developed multiple nanometer silicon carbide structured material technology of preparing.For example: Chinese patent (publication number CN1834309A) discloses a kind of method of silicon carbide nanometer line of synthetic two kinds of different-shapes.This method places in the alumina crucible as starting material with Si powder and multi-walled carbon nano-tubes, crucible is placed in the vacuum high-temperature sintering stove under the Ar gas atmosphere, be warming up to 1410-1600 ℃, constant temperature 3-9 hour, promptly obtain straight, diameter Distribution uniformly and do not have the silicon carbide nanometer line of defectives such as fault and have cucurbit shape nanometer silicon carbide.Chinese patent (publication number CN1762801A) has proposed a kind of preparation method of synthetic pearl silicon carbide nanometer line.This method is with carbon source, silicon source and the rare earth metal salt carbon silicon binary gel that has been feedstock production, and the gained xerogel is warming up to 1250-1400 ℃ under argon gas atmosphere, and isothermal reaction 3-20 hour, the gained sample was through de-carbon, and pickling obtains the pearl silicon carbide nanometer line at last.Chinese patent (publication number CN 1962433A) discloses the method that a kind of preparation contains the silicon carbide nanometer line of non-crystalline state ball-like structure in half a lifetime.This method is 2 according to carbon silicon ratio: the ratio preparation sucrose of 1-5 and the vitreosol of silicon sol, in temperature is under 60-95 ℃ it to be carried out gelation to handle, the gained gel places in the sintering oven under the argon gas atmosphere, temperature rise rate with 5-30 ℃ heats, at 1350-1700 ℃ of sintering temperature 0.5-4 hour, cool to room temperature promptly obtained containing the silicon carbide nanometer line of non-crystalline state ball-like structure in half a lifetime.In addition, DangqingZhang etc. (Nano.Letter.2003 3 983-987) has reported a kind of method for preparing the nanometer silicon carbide spring with plasma reinforced chemical vapour deposition.Yet the preparation method with silicon carbide nanometer line of periodical twin crystal structure does not appear in the newspapers.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with silicon carbide nanometer line of periodical twin crystal structure.
Periodical twin crystal structure has significant effects to optics, electronics, machinery and the chemical property of material, and particularly the twin crystal boundary energy produces a kind of favourable energy, to the electronics and the mechanical property generation great effect of material.Study on Mechanical Properties shows that in copper nano material twin crystal boundary goes to stop the generation of deformational behavior usually as the obstacle of tomography.Periodic twin structure may be given optical property, electrical properties and the mechanical property of silicon carbide nanometer line uniqueness, therefore this material nano-device, matrix material strengthen and optoelectronic areas in potential application foreground is arranged.
The present invention realizes by following method:
(1), 1-4 weight part biphenyl is dissolved in the acetone of 2-11 weight part, the nitrate that adds the 0.03-0.2 weight part, stirring makes it dissolving, under agitation condition, the tetraethoxy of 3-7 weight part is added in the above-mentioned solution, mix, the oxalic acid that adds the 0.01-0.2 weight part promotes teos hydrolysis, at room temperature hydrolysis 6-72 hour, form colloidal sol;
(2), in colloidal sol, add the hexamethylenetetramine of 0.1-0.4 weight part, form gel, gained gel under 80-110 ℃ of condition dry 5-30 hour obtains xerogel;
(3), with xerogel under the argon gas condition, be warming up to 1200-1400 ℃, isothermal reaction 3-20 hour, naturally cooled to after the room temperature in 600-800 ℃ of air oxidation 1-6 hour, remove unreacted carbon, use the mixing pickling of hydrochloric acid and hydrofluoric acid again,, obtain having the silicon carbide nanometer line of periodical twin crystal structure after washing, oven dry.
Aforesaid nitrate is iron nitrate, Xiao Suangu, nickelous nitrate etc.
The volume ratio of the mixing acid of aforesaid hydrochloric acid and hydrofluoric acid is 1: between the 2-5.
The silicon carbide nanometer line with periodical twin crystal structure of the present invention's preparation, its diameter is between the 50-300 nanometer, and length is between the 10-100 micron.
Characteristics of the present invention are to adopt a kind of simple collosol and gel and carbothermic reduction technology, prepare the silicon carbide nanometer line (typical structure is seen accompanying drawing 1-4) with periodical twin crystal structure.In this technology, biphenyl is as carbon source, and tetraethoxy is the silicon source, and nitrate is as growth auxiliary agent and morphology control agent.Equipment is simple, production cost is low, temperature of reaction is lower.
Description of drawings
Fig. 1 is the SEM figure of gained silicon carbide nanometer line.
Fig. 2 is the HRTEM figure of gained silicon carbide nanometer line.
Fig. 3 is the HRTEM figure of gained silicon carbide nanometer line.
Fig. 4 is the fourier transform of Fig. 3.
As shown in the figure: nano wire has periodic structure among Fig. 1,2, and its diameter is between the 50-300 nanometer, and length is between the 10-100 micron.
Fig. 3, Fig. 4 show that the gained nano wire has typical twin structure.
Embodiment
Embodiment 1
1, takes by weighing 15 gram biphenyl and be dissolved in 50 milliliters of acetone, add 0.5 gram iron nitrate, stir and make it dissolving.
2, under continuous stirring condition, 50 milliliters tetraethoxys are joined in the above-mentioned solution, after mixing, add 0.2 gram oxalic acid, hydrolysis is 24 hours under the room temperature, forms colloidal sol.
3,2 gram hexamethylenetetramines are joined in the colloidal sol, form gel, the gained gel was 80 ℃ of dryings 24 hours.
4, xerogel is put into tube type high-temperature furnace, feed argon gas, be warming up to 1200 ℃, isothermal reaction naturally cooled to room temperature after 10 hours under argon gas atmosphere.
5, gained reaction product oxidation 3 hours in 700 ℃ of air, use HCl again: the HF volume ratio is 1: 2 mixing acid pickling, after washing, oven dry, can obtain having Fig. 1-silicon carbide nanometer line of periodical twin crystal structure shown in Figure 4.
Embodiment 2
1, takes by weighing 20 gram biphenyl and be dissolved in 70 milliliters of acetone, add 1 gram Xiao Suangu, stir and make it dissolving.
2, under continuous stirring condition, 70 milliliters tetraethoxys are joined in the above-mentioned solution, after mixing, add 0.4 gram oxalic acid, hydrolysis is 24 hours under the room temperature, forms colloidal sol.
3,4 gram hexamethylenetetramines are joined in the colloidal sol, form gel, the gained gel was 100 ℃ of dryings 12 hours.
4, xerogel is put into tube type high-temperature furnace, feed argon gas, be warming up to 1300 ℃, isothermal reaction naturally cooled to room temperature after 7 hours under argon gas atmosphere.
5, gained reaction product oxidation 4 hours in 600 ℃ of air, use HCl again: the HF volume ratio is 1: 3 mixing acid pickling, after washing, oven dry, can obtain having Fig. 1-silicon carbide nanometer line of periodical twin crystal structure shown in Figure 4.
Embodiment 3
1, takes by weighing 25 gram biphenyl and be dissolved in 80 milliliters of acetone, add 1 gram nickelous nitrate, stir and make it dissolving.
2, under continuous stirring condition, 70 milliliters tetraethoxys are joined in the above-mentioned solution, after mixing, add 0.3 gram oxalic acid, hydrolysis is 24 hours under the room temperature, forms colloidal sol.
3,3 gram hexamethylenetetramines are joined in the colloidal sol, form gel, the gained gel was 110 ℃ of dryings 24 hours.
4, xerogel is put into tube type high-temperature furnace, feed argon gas, be warming up to 1350 ℃, isothermal reaction naturally cooled to room temperature after 6 hours under argon gas atmosphere.
5, gained reaction product oxidation 5 hours in 700 ℃ of air, use HCl again: the HF volume ratio is 1: 4 mixing acid pickling, after washing, oven dry, can obtain having Fig. 1-silicon carbide nanometer line of periodical twin crystal structure shown in Figure 4.
Embodiment 4
1, takes by weighing 30 gram biphenyl and be dissolved in 90 milliliters of acetone, add 1.5 gram iron nitrates, stir and make it dissolving.
2, under continuous stirring condition, 80 milliliters tetraethoxys are joined in the above-mentioned solution, after mixing, add 0.5 gram oxalic acid, hydrolysis is 24 hours under the room temperature, forms colloidal sol.
3,4.5 gram hexamethylenetetramines are joined in the colloidal sol, form gel, the gained gel was 100 ℃ of dryings 30 hours.
4, xerogel is put into tube type high-temperature furnace, feed argon gas, be warming up to 1300 ℃, isothermal reaction naturally cooled to room temperature after 10 hours under argon gas atmosphere.
5, gained reaction product oxidation 5 hours in 700 ℃ of air, use HCl again: the HF volume ratio is 1: 5 mixing acid pickling, after washing, oven dry, can obtain having Fig. 1-silicon carbide nanometer line of periodical twin crystal structure shown in Figure 4.
Claims (3)
1. the preparation method with silicon carbide nanometer line of periodical twin crystal structure is characterized in that comprising the steps:
(1), 1-4 weight part biphenyl is dissolved in the acetone of 2-11 weight part, the nitrate that adds the 0.03-0.2 weight part, stirring makes it dissolving, under agitation condition, the tetraethoxy of 3-7 weight part is added in the above-mentioned solution, mix, the oxalic acid that adds the 0.01-0.2 weight part promotes teos hydrolysis, at room temperature hydrolysis 6-72 hour, form colloidal sol;
(2), in colloidal sol, add the hexamethylenetetramine of 0.1-0.4 weight part, form gel, gained gel under 80-110 ℃ of condition dry 5-30 hour obtains xerogel;
(3), with xerogel under the argon gas condition, be warming up to 1200-1400 ℃, isothermal reaction 3-20 hour, naturally cooled to after the room temperature in 600-800 ℃ of air oxidation 1-6 hour, remove unreacted carbon, use the mixing pickling of hydrochloric acid and hydrofluoric acid again,, obtain having the silicon carbide nanometer line of periodical twin crystal structure after washing, oven dry.
2. a kind of preparation method with silicon carbide nanometer line of periodical twin crystal structure as claimed in claim 1 is characterized in that described nitrate is iron nitrate, Xiao Suangu or nickelous nitrate.
3. a kind of preparation method with silicon carbide nanometer line of periodical twin crystal structure as claimed in claim 1, the mixing acid that it is characterized in that described hydrochloric acid and hydrofluoric acid is that volume ratio is 1: between the 2-5.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730685A (en) * | 2012-07-03 | 2012-10-17 | 西北工业大学 | Method for preparing one-dimensional hafnium carbide nanometer material |
| CN103145129A (en) * | 2013-03-28 | 2013-06-12 | 北京科技大学 | Method for preparing silicon carbide nano-fibre |
| CN106629734A (en) * | 2016-12-22 | 2017-05-10 | 北京光华纺织集团有限公司 | Preparation method of silicon carbide nano material |
| CN106629733A (en) * | 2016-12-22 | 2017-05-10 | 北京光华纺织集团有限公司 | Preparation method of silicon carbide nanomaterial |
| CN106744966A (en) * | 2016-12-22 | 2017-05-31 | 北京光华纺织集团有限公司 | A kind of preparation method of silicon carbide nano material |
| CN111484019A (en) * | 2020-04-27 | 2020-08-04 | 山西烁科晶体有限公司 | Preparation method of high-purity silicon carbide powder for single crystal growth |
-
2007
- 2007-12-21 CN CNA2007101854678A patent/CN101186297A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730685A (en) * | 2012-07-03 | 2012-10-17 | 西北工业大学 | Method for preparing one-dimensional hafnium carbide nanometer material |
| CN102730685B (en) * | 2012-07-03 | 2014-04-02 | 西北工业大学 | Method for preparing one-dimensional hafnium carbide nanometer material |
| CN103145129A (en) * | 2013-03-28 | 2013-06-12 | 北京科技大学 | Method for preparing silicon carbide nano-fibre |
| CN103145129B (en) * | 2013-03-28 | 2015-04-01 | 北京科技大学 | Method for preparing silicon carbide nano-fibre |
| CN106629734A (en) * | 2016-12-22 | 2017-05-10 | 北京光华纺织集团有限公司 | Preparation method of silicon carbide nano material |
| CN106629733A (en) * | 2016-12-22 | 2017-05-10 | 北京光华纺织集团有限公司 | Preparation method of silicon carbide nanomaterial |
| CN106744966A (en) * | 2016-12-22 | 2017-05-31 | 北京光华纺织集团有限公司 | A kind of preparation method of silicon carbide nano material |
| CN111484019A (en) * | 2020-04-27 | 2020-08-04 | 山西烁科晶体有限公司 | Preparation method of high-purity silicon carbide powder for single crystal growth |
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Open date: 20080528 |