CN101049931A - Method for synthesizing Nano fiber of ultra hydrophobic SiC - Google Patents
Method for synthesizing Nano fiber of ultra hydrophobic SiC Download PDFInfo
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- CN101049931A CN101049931A CN 200710040470 CN200710040470A CN101049931A CN 101049931 A CN101049931 A CN 101049931A CN 200710040470 CN200710040470 CN 200710040470 CN 200710040470 A CN200710040470 A CN 200710040470A CN 101049931 A CN101049931 A CN 101049931A
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Abstract
This invention discloses a method for synthesizing superhydrophobic SiC nanofibers. The method utilizes silicon wafer as the substrate and silicon source, solid carbon material as the precursor, Ar as the protective gas and carrier gas, and ZnS powder as the selective adjuvant, and grows SiC nanofibers on the silicon wafer. Then a layer of perfluorosilane is vapor-deposited onto the synthesized SiC nanofibers to obtain superhydrophobic SiC nanofibers with waer contact angle above 150 deg. The method has such advantages as simple process, no environmental pollution and no flammable raw materials. The obtained superhydrophobic SiC nanofibers can be used in self-cleaning environment.
Description
Technical field
The present invention relates to a kind of method of technical field of nano material, specifically is a kind of synthetic method of Nano fiber of ultra hydrophobic SiC.
Background technology
The ultra-hydrophobicity surface is meant the surface that has self-cleaning function as lotus leaf, thereby has important application in a lot of fields, such as various materials that need moisture-proof function such as various glass, radar, antennas.Application with superhydrophobic surface material can be saved cleaning cost and time for the mankind, can be by the automatic clean surface of the effect of rainwater, particularly in the cleaning of some high-risk occasions such as skyscraper glass.People have carried out various hydrophobic performance researchs for materials such as various organism at present.Possessing contact angle generally needs two primary conditions greater than 150 super-hydrophobicities of spending, and the one, material surface has certain roughness, and the 2nd, surface free energy is lower.Monodimension nanometer material is because its special geometric construction, and the surface possesses certain roughness, thereby has satisfied hydrophobic requirement, thereby comprises that monodimension nanometer materials such as CNT (carbon nano-tube), silicon nanowire have been studied and be used for ultra-hydrophobicity.SiC nanofiber as the broad stopband width, because its high physical strength, high heat conductivity, under severe environment such as high temperature, high frequency, demonstrate good application potential, particularly aspect superhard material toughener and field emission performance, generally believed it is a kind of nano material that has potentiality.Therefore, the research of one dimension SiC nanofiber in every field is extensively launched.But people, also do not begin one's study aspect the ultra-hydrophobicity for the SiC nanofiber.Simultaneously, for having the organic fluorocompound that reduces the surface free energy effect, be used to multiple super-hydrophobicity material surface, and, also be not employed research on one dimension SiC nanofiber surface.
Find that through literature search not finding has the investigator that the SiC nanofiber is carried out super-hydrophobicity research, just some other monodimension nanometer material has been carried out hydrophobicity research to prior art." Preparation of superhydrophobic silicon oxide nanowire surfaces " (the preparation super-hydrophobicity SiO that delivered on the phase 1608-1671 page or leaf in 2007 the 23rd at " Langmuir " (" Langmuir ") such as Y.Coffinier etc.
2The nanofiber surface), propose at SiO in this article
2Nanofiber surface plating one deck organic fluorocompound, thus the hydrophobic surface that contact angle is 150 degree obtained.Its deficiency is: the preparation procedure complexity, cost is higher, and hydrophobic performance is not very high.
Summary of the invention
The object of the invention is at the deficiencies in the prior art, a kind of synthetic method of Nano fiber of ultra hydrophobic SiC is provided, make it synthesize Nano fiber of ultra hydrophobic SiC, extensive synthetic contact angle on silicon base that can be simple is greater than the Nano fiber of ultra hydrophobic SiC of 150 degree.
The present invention is achieved by the following technical solutions; the present invention adopts silicon chip as reaction substrate and silicon source; with the solid carbon material is presoma; with the rare gas element argon gas is shielding gas and carrier gas; with the ZnS powder is the selectivity auxiliary, grows into the SiC nanofiber on silicon chip, again the SiC nanofiber surface evaporation one deck perfluor silane that is synthesizing; thereby make the SiC nanofiber possess the good hydrophobic performance, obtain the ultra-hydrophobicity SiC nanofiber sample that contact angle is higher than 150 degree.
It is as follows to the present invention includes concrete steps:
The first step is put into quartz tube furnace central authorities with silicon chip (bottom comprises or do not contain the ZnS powder), and carbon solid carbon material is fixed on silica tube one side;
Second step was elevated to 1100 ℃ with furnace body temperature, when temperature reaches 250 ℃, fed the rare gas element argon gas;
The 3rd step, under 1100 ℃ of temperature of reaction, gas flow in the holding chamber, reaction continues to carry out, and after having reacted reaction product is taken out, and obtains a large amount of SiC nanofibers at silicon chip surface;
The 4th step, stainless steel device jar is put in the SiC nanofiber and the sealing of perfluor silane that obtain in the lump, carry out the evaporation reaction, obtain having the SiC nanofiber sample of ultra-hydrophobicity.
In the first step, be reflected in the horizontal quartz tube furnace and carry out, by being sintered to fix a side that feeds in silica tube gas,, then can obtain unordered macro nanometer SiC fiber to carbon solid carbon material if do not add the ZnS powder in the silicon chip bottom; If add the ZnS powder in the silicon chip bottom, then can obtain orderly small size SiC nanofibrous structures.
In second step, described furnace body temperature is elevated to 1100 ℃, temperature rise rate is 15 ℃/min.
In second step, described feeding rare gas element argon gas, gas flow is 15l/h.
In the 3rd step, described reaction continues to carry out, and the time length is 2-4 hour.
In the 4th step, described perfluor silane volume is 0.05-0.2ml, and the evaporation temperature of reaction is 150 degree, 3.0 hours reaction times.
The present invention controls the structure that forms the SiC nano-fiber material by adjusting whether add the ZnS powder.The nucleation that adds ZnS and be for SiC provides more multimachine meeting, can impel the formation of oldered array; Do not add ZnS and then can cause unordered nano SiC fiber, and sample diameter is bigger, degree of crystallinity is relatively poor.The purpose that adds the inert protective gas argon gas mainly is that CO gas is taken to silicon chip surface and reaction with it.Evaporation one deck perfluor silane organism is in order to reduce surface free energy, thereby hydrophobic performance is improved, and contact angle is greater than 150 degree, and general object does not have super-hydrophobicity, and contact angle has only tens degree.
The present invention is simple for process, and raw material adopts cheap and widely used silicon chip, carbon material and ZnS powder, and uses the perfluor silane of considerably less content, can synthesize the SiC nanofiber surface of high hydrophobicity easily by simple tubular type stove and baking oven.
Compared with prior art, the present invention adopts silicon chip as reaction substrate and silicon source, with the solid carbon material is presoma, with the ZnS powder is selective additives, with the rare gas element argon gas is shielding gas, is the surface modification organism with perfluor silane, and preparation technology is simple, with low cost, environmentally safe; Adopt protection of inert gas, do not have obvious inflammable dangerous raw material, gas price is cheap; Apparatus and process is simple, and the prepared sample hydrophobic performance height that goes out, contact angle can reach 156 degree.
Description of drawings
Fig. 1 goes out scanning electron microscope (SEM) photo of unordered SiC nanofiber for employing the present invention is prepared
Fig. 2 is the Nano fiber of ultra hydrophobic SiC optical microscope photograph of 156 degree for contact angle
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
Following examples adopt silicon chip as reaction substrate and silicon source, are presoma with the solid carbon material, and the ZnS powder is the selectivity auxiliary, is shielding gas with the rare gas element argon gas, react, thereby form the SiC nanofibrous structures.The existence of ZnS can make the S that decomposites and silicon react to generate SiS, and SiS can distillation under comparatively high temps and decomposited Si and SiS
2, the Si that decomposites generates oxide compound with oxygen reaction again, thereby for the nucleation of SiC provides more multimachine meeting, can impel the formation of oldered array.There is not ZnS then can generate unordered SiC nanofiber.Stainless steel device jar is put in the sealing of SiC nanofiber and perfluor silane carried out the evaporation reaction, obtain having the SiC nanofiber sample of ultra-hydrophobicity.
Embodiment 1
The ceramic boat that 3 clean silicon chips are housed is placed horizontal quartz tube furnace central authorities, the solid carbon material by being sintered to fix a side that feeds in silica tube gas.Speed with 15 ℃/min is warmed up to 1100 ℃ of temperature of reaction.When temperature reached 250 ℃, feeding gas flow was the argon gas of 15l/h; Under 1100 ℃ of temperature of reaction, gas flow in the holding chamber, reaction continued to carry out 2 hours, after having reacted reaction product is taken out, obtain a large amount of larger-diameter unordered SiC nanofiber samples at silicon chip surface, see Fig. 1, as can be seen, produced the SiC nanofiber of a large amount of lack of alignment at silicon chip surface among the figure.Stainless steel device jar is put in SiC nanofiber that will synthesize and the sealing of the perfluor silane of 0.05ml in the lump, carries out evaporation reaction 3.0 hours under 150 degree, obtains having the SiC nanofiber sample of ultra-hydrophobicity.
Embodiment 2
The ceramic boat that 3 clean silicon chips and 3g ZnS powder are housed is placed horizontal quartz tube furnace central authorities, the solid carbon material by being sintered to fix a side that feeds in silica tube gas.Speed with 15 ℃/min is warmed up to 1100 ℃ of temperature of reaction.When temperature reached 250 ℃, feeding gas flow was the argon gas of 15l/h; Under 1100 ℃ of temperature of reaction, gas flow in the holding chamber, reaction continued to carry out 3 hours, after having reacted reaction product was taken out, and obtained a large amount of orderly SiC nanofiber samples than minor diameter at silicon chip surface.Stainless steel device jar is put in SiC nanofiber that will synthesize and the sealing of the perfluor silane of 0.1ml in the lump, under 150 degree, carry out evaporation reaction 3.0 hours, obtaining contact angle is the SiC nanofiber sample with ultra-hydrophobicity of 156 degree, see Fig. 2, among the figure as can be seen, the good hydrophobic performance that SiC nanofiber sample has demonstrated.
Embodiment 3
The ceramic boat that 3 clean silicon chips and 3g ZnS powder are housed is placed horizontal quartz tube furnace central authorities, the solid carbon material by being sintered to fix a side that feeds in silica tube gas.Speed with 15 ℃/min is warmed up to 1100 ℃ of temperature of reaction.When temperature reached 250 ℃, feeding gas flow was the argon gas of 15l/h; Under 1100 ℃ of temperature of reaction, gas flow in the holding chamber, reaction continued to carry out 4 hours, after having reacted reaction product was taken out, and obtained a large amount of orderly SiC nanofiber samples than minor diameter at silicon chip surface.Stainless steel device jar is put in SiC nanofiber that will synthesize and the sealing of the perfluor silane of 0.2ml in the lump, carries out evaporation reaction 3.0 hours under 150 degree, obtains the SiC nanofiber sample with ultra-hydrophobicity that contact angle is higher than 150 degree.
Claims (9)
1, a kind of synthetic method of Nano fiber of ultra hydrophobic SiC; it is characterized in that; adopt silicon chip as reaction substrate and silicon source; with the solid carbon material is presoma; with the rare gas element argon gas is shielding gas and carrier gas, is the selectivity auxiliary with the ZnS powder, grows into the SiC nanofiber on silicon chip; at the SiC nanofiber surface evaporation one deck perfluor silane that synthesizes, be higher than the 150 ultra-hydrophobicity SiC nanofiber samples of spending again thereby obtain contact angle.
2, the synthetic method of Nano fiber of ultra hydrophobic SiC according to claim 1 is characterized in that, comprises that step is as follows:
The first step is put into quartz tube furnace central authorities with the silicon chip of silicon chip or bottom interpolation ZnS powder, and carbon solid carbon material is fixed on silica tube one side;
Second step was elevated to 1100 ℃ with furnace body temperature, when temperature reaches 250 ℃, fed the rare gas element argon gas;
The 3rd step, under 1100 ℃ of temperature of reaction, gas flow in the holding chamber, reaction continues to carry out, and after having reacted reaction product is taken out, and obtains a large amount of SiC nanofibers at silicon chip surface;
The 4th step, stainless steel device jar is put in the SiC nanofiber and the sealing of perfluor silane that obtain in the lump, carry out evaporation, obtain having the SiC nanofiber sample of ultra-hydrophobicity.
3, the synthetic method of Nano fiber of ultra hydrophobic SiC according to claim 2 is characterized in that, in the first step, is reflected in the horizontal quartz tube furnace and carries out, and carbon solid carbon material is by being sintered to fix a side that feeds in silica tube gas.
4, the synthetic method of Nano fiber of ultra hydrophobic SiC according to claim 2 is characterized in that, in second step, described furnace body temperature is elevated to 1100 ℃, and temperature rise rate is 15 ℃/min.
5, the synthetic method of Nano fiber of ultra hydrophobic SiC according to claim 2 is characterized in that, in second step, and described feeding rare gas element argon gas, gas flow is 15l/h.
6, the synthetic method of Nano fiber of ultra hydrophobic SiC according to claim 2 is characterized in that, in the 3rd step, described reaction continues to carry out, and the time length is 2-4 hour.
7, the synthetic method of Nano fiber of ultra hydrophobic SiC according to claim 2 is characterized in that, in the 4th step, described perfluor silane volume is 0.05-0.2ml.
8, the synthetic method of Nano fiber of ultra hydrophobic SiC according to claim 2 is characterized in that, in the 4th step, described evaporation temperature of reaction is 150 degree.
According to the synthetic method of claim 2 or 8 described Nano fiber of ultra hydrophobic SiC, it is characterized in that 9, in the 4th step, the described evaporation reaction times is 3.0 hours.
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| CNB2007100404700A CN100515941C (en) | 2007-05-10 | 2007-05-10 | Method for synthesizing Nano fiber of ultra hydrophobic SiC |
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| CN101049931A true CN101049931A (en) | 2007-10-10 |
| CN100515941C CN100515941C (en) | 2009-07-22 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103748272A (en) * | 2011-03-09 | 2014-04-23 | 得克萨斯大学体系董事会 | Apparatuses and methods for the production of fibers |
| CN108159779A (en) * | 2018-02-10 | 2018-06-15 | 北京清正泰科技术有限公司 | A kind of filtering material and the air filter unit based on the filtering material |
-
2007
- 2007-05-10 CN CNB2007100404700A patent/CN100515941C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103748272A (en) * | 2011-03-09 | 2014-04-23 | 得克萨斯大学体系董事会 | Apparatuses and methods for the production of fibers |
| CN103748272B (en) * | 2011-03-09 | 2019-11-19 | 得克萨斯大学体系董事会 | Manufacture the device and method of fiber |
| CN108159779A (en) * | 2018-02-10 | 2018-06-15 | 北京清正泰科技术有限公司 | A kind of filtering material and the air filter unit based on the filtering material |
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| Publication number | Publication date |
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| CN100515941C (en) | 2009-07-22 |
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