CN100494477C - Method for synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet - Google Patents
Method for synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet Download PDFInfo
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- CN100494477C CN100494477C CNB2007100419693A CN200710041969A CN100494477C CN 100494477 C CN100494477 C CN 100494477C CN B2007100419693 A CNB2007100419693 A CN B2007100419693A CN 200710041969 A CN200710041969 A CN 200710041969A CN 100494477 C CN100494477 C CN 100494477C
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Abstract
The invention provides a method of synthesis the hydrophobicity silicon dioxide nanometer fiber with the heat evaporation gold-plating silicon chip, which belongs to nanometer material domain. This invention uses the silicon chip as the response substrate and the silicon source, uses aurum as respond accelerant, and uses argon which is the inert gas as the protective gas. The silicon separates out the coring growth from the silicon chip under the catalytic action of argon and is oxidized into the silicon dioxide nanometer fiber. After coating by vaporization a slice of fluorine silane in the surface of the silicon dioxide nanometer fiber, thus it can obtain superhydrophobicity silicon dioxide nanometer fiber whose contact angle is more than 150 deg. This invention is easy to operation, doesn't have the pollution to the environment, and doesn't have obvious flammable dangerous raw material. Since it's superhydrophobicity is high, it can apply in many clean situation.
Description
Technical field
The present invention relates to a kind of method of technical field of nano material, specifically is a kind of method of synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet.
Background technology
Thereby hydrophobic material has important application in a lot of fields owing to have self-cleaning function, such as various fields that need moisture-proof function such as various windshields, radar, antennas.People have carried out various hydrophobic performance researchs for materials such as various organism at present.Possessing the bigger hydrophobicity of contact angle generally needs two primary conditions, 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 material such as CNT (carbon nano-tube) has been studied and be used for hydrophobic performance.But people are at the early-stage to evaporating the silica nano fibrous hydrophobicity research ability of carrying out of gold-plated silicon chip generation.Simultaneously,, be used to the various hydrophobic material surface for having the organic fluorocompound that reduces the surface free energy effect, and the gold-plated silicon chip of evaporation generate silica nano fibrous aspect, seldom be employed research.
Through the literature search of prior art is found, find that little investigator silica nano fibrously carries out hydrophobicity research to what evaporate that gold-plated silicon chip generates, some other monodimension nanometer material has been carried out hydrophobicity research." Preparation of superhydrophobic silicon oxide nanowiresurfaces " (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 hydrophobic surface obtained.Its deficiency is: the preparation procedure complexity, cost is higher, and contact angle is not high.
Summary of the invention
The object of the invention is at the deficiencies in the prior art, a kind of method of synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet is provided, make it synthesize the hydrophobic silica nanofiber, extensive synthetic contact angle on silicon base that can be simple is greater than the super-hydrophobic silica nanofiber of 150 degree.
The present invention is achieved by the following technical solutions; the present invention adopts gold-plated silicon chip as reaction substrate and silicon source; with the gold in the gold-plated silicon chip is catalysts; with the rare gas element argon gas is shielding gas; growthing silica nanofiber on silicon chip; the silica nano fibrous surperficial evaporation one deck perfluor silane that is synthesizing again; thereby make silica nano fibrous reduction surface energy; possess the good hydrophobic performance, obtain contact angle be higher than 150 the degree ultra-hydrophobicities silica nano fibrous.
The present invention includes following steps:
The first step will be put into quartz tube furnace central authorities by the gold-plated silicon chip that magnetron sputtering obtains;
Described magnetron sputtering, its time is 5-15 minute.
Described quartz tube furnace is horizontal quartz tube furnace.
Described gold-plated silicon chip, its size is 1cm X 1cm.
Second step was elevated to temperature of reaction with furnace body temperature, when beginning to heat up, fed the rare gas element argon gas;
Described temperature of reaction is 1200-1400 ℃.
Described intensification, its speed are 10 ℃/min.
Described feeding rare gas element argon gas, gas flow is 50-400ml/min.
The 3rd step, under 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 silica nano fibrous in a large number at silicon chip surface;
Described reaction continues to carry out, and the time length is 3-6 hour.
The 4th step, stainless steel device jar is put in the silica nano fibrous and perfluor silane sealing that obtains in the lump, carry out the evaporation reaction, obtain having the silica nano fibrous of ultra-hydrophobicity.
Described perfluor silane, its volume are 0.05-0.2ml.
Described evaporation reaction, its temperature are 150 degree.
Described evaporation reaction, 3.0 hours its time.
The present invention is by the gold-plated silicon chip of thermal evaporation under the high temperature, thereby makes silicon nucleation and growth under VLS mechanism, generates behind the nano wire oxidizedly, generates at silicon chip surface at last and has the silica nano fibrous structure of certain roughness in a large number.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.
The present invention is simple for process, raw material adopts cheap and widely used gold-plated silicon chip and general argon gas, and use the perfluor silane of considerably less content, can synthesize the silica nano fibrous 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 gold is catalysts, with the rare gas element argon gas is shielding gas, growthing silica nanofiber on silicon chip 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 155 degree.
Description of drawings
Fig. 1 goes out silica nano fibrous scanning electron microscope (SEM) photo for employing the present invention is prepared
Fig. 2 is the super-hydrophobic silica nanofiber optical microscope photograph of 155 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 catalysts with the gold, are shielding gas with the rare gas element argon gas, under 1200 ℃ on silicon chip the growthing silica nanofiber.Under hot conditions, silicon can be separated out nucleating growth and be oxidized to silica nano fibrous under the katalysis of Au according to VLS mechanism from silicon chip.Stainless steel device jar is put in the silica nano fibrous and perfluor silane sealing that generates carried out the evaporation reaction, obtain having the silica nano fibrous of ultra-hydrophobicity.
Embodiment 1
2 ceramic boat that obtained gold-plated silicon chip (1cm X 1cm) in 5 minutes by magnetron sputtering will be housed put into quartz tube furnace central authorities, be warmed up to 1350 ℃ of temperature of reaction with the speed of 10 ℃/min.When beginning to heat up, feeding gas flow is the argon gas of 50ml/min; Under 1350 ℃ of temperature of reaction, gas flow in the holding chamber, reaction continued to carry out 3 hours, after having reacted reaction product is taken out, obtain a large amount of unordered silica nano fibrous at silicon chip surface, see Fig. 1, as can be seen, produced the silica nano fibrous of a large amount of lack of alignment among the figure at silicon chip surface.Stainless steel device jar is put in the perfluor silane sealing of the silica nano fibrous and 0.05ml that will synthesize in the lump, carries out evaporation reaction 3.0 hours under 150 degree, obtains contact angle and has the silica nano fibrous of ultra-hydrophobicity greater than 150 degree.
Embodiment 2
2 ceramic boat that obtained gold-plated silicon chip (1cm X 1cm) in 10 minutes by magnetron sputtering will be housed put into quartz tube furnace central authorities, be warmed up to 1400 ℃ of temperature of reaction with the speed of 10 ℃/min.When beginning to heat up, feeding gas flow is the argon gas of 200ml/min; Under 1350 ℃ of temperature of reaction, gas flow in the holding chamber, reaction continued to carry out 5 hours, with the reaction product taking-up, obtained unordered in a large number silica nano fibrous at silicon chip surface after react.Stainless steel device jar is put in the perfluor silane sealing of the silica nano fibrous and 0.1ml that will synthesize in the lump, under 150 degree, carry out evaporation reaction 3.0 hours, what obtain contact angle and be 155 degree has the silica nano fibrous of ultra-hydrophobicity, see Fig. 2, among the figure as can be seen, the silica nano fibrous good hydrophobic performance that has demonstrated.
Embodiment 3
2 ceramic boat that obtained gold-plated silicon chip (1cm X 1cm) in 15 minutes by magnetron sputtering will be housed put into quartz tube furnace central authorities, be warmed up to 1350 ℃ of temperature of reaction with the speed of 10 ℃/min.When beginning to heat up, feeding gas flow is the argon gas of 400ml/min; Under 1350 ℃ of temperature of reaction, gas flow in the holding chamber, reaction continued to carry out 6 hours, with the reaction product taking-up, obtained unordered in a large number silica nano fibrous at silicon chip surface after react.Stainless steel device jar is put in the perfluor silane sealing of the silica nano fibrous and 0.2ml that will synthesize in the lump, carries out evaporation reaction 3.0 hours under 150 degree, obtains contact angle and has the silica nano fibrous of ultra-hydrophobicity greater than 150 degree.
By above embodiment as can be seen, technology of the present invention is simple, and is with low cost, environmentally safe, obtain contact angle be higher than 150 the degree ultra-hydrophobicities silica nano fibrous.
Claims (10)
1, a kind of method of synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet; it is characterized in that; adopt gold-plated silicon chip as reaction substrate and silicon source; with the gold in the gold-plated silicon chip is catalysts; with the rare gas element argon gas is shielding gas; growthing silica nanofiber on silicon chip, again at the silica nano fibrous surperficial evaporation one deck perfluor silane that synthesizes, obtain contact angle be higher than 150 the degree ultra-hydrophobicities silica nano fibrous.
2, the method for synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet according to claim 1 is characterized in that, comprises that step is as follows:
The first step will be put into quartz tube furnace central authorities by the gold-plated silicon chip that magnetron sputtering obtains;
Second step was elevated to 1200 ℃-1400 ℃ of temperature of reaction with furnace body temperature, when beginning to heat up, fed the rare gas element argon gas;
The 3rd step, under 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 silica nano fibrous in a large number at silicon chip surface;
The 4th step, stainless steel device jar is put in the silica nano fibrous and perfluor silane sealing that obtains in the lump, carry out the evaporation reaction, obtain having the silica nano fibrous of ultra-hydrophobicity.
3, the method for synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet according to claim 2 is characterized in that, in the first step, and described magnetron sputtering, its time is 5-15 minute.
According to the method for claim 2 or 3 described synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet, it is characterized in that 4, in the first step, described quartz tube furnace is horizontal quartz tube furnace.
5, according to the method for claim 2 or 3 described synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet, it is characterized in that, in the first step, described gold-plated silicon chip, its size is 1cmX1cm.
6, the method for synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet according to claim 2 is characterized in that, in second step, and described intensification, its speed is 10 ℃/min.
7, according to the method for claim 2 or 6 described synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet, it is characterized in that, in second step, described feeding rare gas element argon gas, gas flow is 50-400ml/min.
8, the method for employing synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet according to claim 2 is characterized in that, in the 3rd step, described reaction continues to carry out, and the time length is 3-6 hour.
9, the method for employing synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet according to claim 2 is characterized in that, in the 4th step, described perfluor silane, its volume are 0.05-0.2ml.
10, according to the method for claim 2 or 9 described employing synthesizing hydrophobic silicon dioxide nano fiber by heat evaporation of gold-plate silicon sheet, it is characterized in that, in the 4th step, described evaporation reaction, its temperature is 150 degree, 3.0 hours time.
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| CN101844741A (en) * | 2010-05-05 | 2010-09-29 | 北京邮电大学 | One-dimensional porous (Zn, cd) S/SiO2tubular nanocomposite and its prepn |
| JP6042355B2 (en) * | 2011-03-09 | 2016-12-14 | ボード・オブ・リージエンツ，ザ・ユニバーシテイ・オブ・テキサス・システム | Apparatus and method for the production of fibers |
| CN104108719B (en) * | 2014-07-24 | 2016-06-08 | 黑龙江科技大学 | A kind of method preparing amorphous silica nanotube |
| CN105908128B (en) * | 2016-04-21 | 2018-11-06 | 厦门建霖健康家居股份有限公司 | A kind of photoinduction prepares the surface treatment method of bionical hydrophobic layer |
| CN106346017B (en) * | 2016-09-09 | 2018-11-09 | 昆明理工大学 | A kind of preparation method of silver/silicon dioxide nanowire composite |
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