CN105200528A - Method for corrosively preparing silicon-base super-hydrophobic surface by utilizing pine structural porous silver as catalyst - Google Patents
Method for corrosively preparing silicon-base super-hydrophobic surface by utilizing pine structural porous silver as catalyst Download PDFInfo
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- CN105200528A CN105200528A CN201510657170.1A CN201510657170A CN105200528A CN 105200528 A CN105200528 A CN 105200528A CN 201510657170 A CN201510657170 A CN 201510657170A CN 105200528 A CN105200528 A CN 105200528A
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Abstract
The invention discloses a method for corrosively preparing a silicon-base super-hydrophobic surface by utilizing pine structural porous silver as a catalyst. The method comprises the following steps: sintering pine which is used as a raw material in a non-oxidation atmosphere to obtain porous carbon having the pine structure, soaking the porous coal by virtue of a silver nitrate solution, and sintering in an oxygen-free atmosphere to obtain porous silver having the pine structure; immersing monocrystalline silicon by adopting a mixed solution of hydrofluoric acid, hydrogen peroxide and water as a corrosion agent, pressing the porous silver onto a silicon plane so as to realize a catalytic effect, facilitating the corrosion reaction, and forming a silicon surface which is fluctuated oppositely to the porous silver structure; immersing the porous silver structure in a mixed solution of fluorinated silane and isopropanol to obtain the silicon-base super-hydrophobic surface. The prepared silicon surface can copy a micro structure of the pine, the nature is highly imitated, and the superhydrophobicity is excellent.
Description
Technical field
The invention belongs to a kind of a kind of silver-colored method done catalyzer etch silicon plane and prepare silica-based super hydrophobic surface of porous that method preparing silica-based super hydrophobic surface, particularly utilization have pine structure.
Background technology
Wettability, as a kind of important performance of material, is determined jointly by surface topography and chemical constitution.The preparation of super hydrophobic surface in recent years receives the extensive concern of people.Super hydrophobic surface has very high using value in protection against corrosion, waterproof, automatically cleaning, Drag Reduction, harmless fluid transport, the side such as anti-oxidant, becomes the important topic in Surface Engineering field gradually.The method preparing super hydrophobic surface has two kinds: one to be in coarse solids finishing low-surface energy substance usually, and another kind builds coarse structure at hydrophobic surface.The silicon materials role that performer is important in modern microelectronic, photoelectron, sensor and MEMS (micro electro mechanical system).And make silica-base material have super hydrophobic surface; the range of application of silicon materials can be expanded undoubtedly; such as; in silicon materials are the electron device of master and solar photovoltaic device is applied; the short circuit that the super hydrophobic surface of silicon materials can effectively avoid device to cause because of rainwater and corrosion, thus provide effective protection to device.The approach of the silica-based super hydrophobic surface of current preparation is mainly and utilizes low-surface energy substance to modify the silica-base material with coarse microstructural surfaces, and the surface roughness of silica-base material obtains usually through etching method and chemical Vapor deposition process, as prepared micron order cylindrical-array coarse structure on silica-base material surface with the method for photoengraving or Mechanical lithography.
In the process of material and structure design thereof, natural biology gives people and much enlightens.Nature is in the evolution of long-term evolution and differentiation, vegetable material in biosystem defines a kind of natural three-dimensional contiguous network structure construction, have multi-level, multi-component order tissue topography feature, this structure is difficult to be obtained by artificial means.If by the structure reference of plant uniqueness in the design preparation of type material, this will break through the designing axiom of traditional material, and the development for materialogy provides a kind of new theory.At present, investigation of materials person is just exploring and is utilizing natural phant structure, preparation has the controlled type material of distinct plant structure feature, unique microstructure weave construction, and expect that this unique texture can give the performance of material excellence, as investigator utilizes the plant structure such as timber, wood materials, cotton, coconut husk, rice husk, by technology controlling and process and compound, SiC, Si/SiC/C, SiOC/C, Al of maintaining natural plant constitutional features are prepared
2o
3, TiO
2, ZrO
2, SnO
2deng stupalith.Research shows that the natural structure of plant has excellent performance to some new ceramics and plays an important role, and is expected to be used widely in molecular sieve, strainer, support of the catalyst, thermal insulation material, gas sensitive, electromagnetic shielding material, far-infrared radiation material etc.
Summary of the invention
The object of the present invention is to provide the method for the silica-based super hydrophobic surface of preparation of a kind of high level reference nature, finished product excellent property.
The technical solution realizing the object of the invention is: a kind of method preparing silica-based super hydrophobic surface with pine structural porous silver as catalytic erosion, and step is as follows:
(1) take pine as raw material, pine is placed in non-oxidizing atmosphere sintering oven and sinters, sintering temperature is not less than 500 DEG C, and temperature rise rate, not higher than 3 DEG C/min, obtains the porous carbon with pine structure;
(2) flooded in silver nitrate solution by porous carbon, strength of solution is 0.1mol/L, and dipping time is 1 ~ 2 hour, is taken out by porous carbon dry after dipping;
(3) be placed in oxygen-free atmosphere process furnace by dried porous carbon and sinter, sintering temperature is 450 ~ 550 DEG C, obtains the porous silver with pine structure;
(4) etching reagent is made with the mixed solution of hydrofluoric acid, hydrogen peroxide and water, and with etching reagent submergence silicon single crystal;
(5) be pressed in silicon single crystal plane by the porous silver with pine structure, make it abundant contact, duration of contact is 19 ~ 21 minutes, and under the catalysis of silver, etching reagent corrodes silicon single crystal rapidly, and forms the silicon face contrary with porous silver structure convex-concave;
(6) monocrystalline silicon surface after corrosion is immersed immersion in silicon fluoride and Virahol mixed solution and be greater than 4 days, silicon fluoride and Virahol volume ratio are 1:4 ~ 1:8, take out drying subsequently, just obtained silica-based super hydrophobic surface.
In step 1, described pine is the Pinaceae timber of broad sense, and preferred kahikatea is wooden, metasequoia is wooden; Described non-oxidizing atmosphere sintering oven is Wood carbonization stove, vacuumizes process furnace, Ar-sintering stove or nitrogen protective sintering stove continuously; Described sintering temperature preferably 500 ~ 800 DEG C; Described temperature rise rate is 1 ~ 2 DEG C/min preferably.
In step 3, described oxygen-free atmosphere process furnace is for vacuumize process furnace, argon shield process furnace or nitrogen protection process furnace continuously.
In step 4, in mixed solution, the volume ratio of hydrofluoric acid, hydrogen peroxide, water is 6:2:2.
In step 6, described silicon fluoride and the preferred 1:6 of Virahol volume ratio; Described soak time preferably 4 ~ 15 days.
Compared with prior art, its remarkable advantage is in the present invention: prepared silicon face topology pine microtexture, the reference nature of high level, has excellent ultra-hydrophobicity.
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the microtexture figure with kahikatea timber structure porous silver obtained in the embodiment of the present invention 1.
Fig. 2 be in the embodiment of the present invention 1 obtained have kahikatea timber structure porous silver XRD figure spectrum.
Fig. 3 utilizes kahikatea timber structure porous silver to make the obtained silicon face microtexture figure of catalytic erosion in the embodiment of the present invention 1.
Fig. 4 is the contact angle figure of the silicon face utilizing kahikatea timber structure porous silver to obtain as catalytic erosion in the embodiment of the present invention 1.
Embodiment
Principle of the present invention is: the present invention utilizes pine for template, it is sintered in non-oxidizing atmosphere.Organism during sintering in pine decomposes, oxygen, hydrogen, nitrogen and part carbon change gaseous volatilization into, most carbons wherein then remain, and the original vesicular structure of timber is also remained by complete in sintering process, thus form the porous carbon with Wood microstructure.This porous carbon, after silver nitrate solution dipping, taking-up drying, can form Silver Nitrate tectum in porous carbon surface and aperture.When being sintered, Silver Nitrate decomposes, and generate silver, nitrogen, oxygen and nitrogen peroxide, gas is discharged in tube furnace, and silver then under porous carbon surface precipitation, thus forms the porous silver/carbon with pine structure.Obtained porous silver is covered the surface being pressed in silicon single crystal, adds etching reagent HF, H
2o
2with the mixed solution of deionized water.Wherein porous silver serves as catalyzer, and following reaction occurs silicon single crystal:
H
2O
2+2H
+→2h
++2H
2O6HF+4h
+→H
2SiF
6+4H
+
Due to porous silver existing a large amount of said minuscule hole, just corrosion reaction can occur with the silicon of silver-colored close contact and produce depression, and the silicon below hole can not react, the columnar arrays silicon face contrary with porous silver structure convex-concave can be formed like this.Silicon single crystal is taken out after corrosion certain hour.Then soaked in silicon fluoride solution by this silicon face, silicon fluoride forms very thin tectum by hydrolysis and polycondensation at silicon face.When above the globule drops on, the air in the protruding gap of column can be locked, and forms the gas cloud that one deck is very thin between the globule and silicon single crystal, and such water only forms point cantact with columnar projections, and decrease contact area, surface adhesion reactive force is very weak.Therefore water can congeal into the globule under surface tension effects, and arbitrarily can roll on monocrystalline silicon surface, thus realizes super-hydrophobicity.
Prepare the method for silica-based super hydrophobic surface as catalytic erosion with pine structural porous silver, its step is as follows:
(1) kahikatea wood, metasequoia are woodenly placed in Wood carbonization stove, vacuumize process furnace, Ar-sintering stove or nitrogen protective sintering stove continuously and sinter, sintering temperature 500 ~ 800 DEG C, temperature rise rate is 1 ~ 2 DEG C/min preferably, the obtained porous carbon with pine structure;
(2) flooded in silver nitrate solution by porous carbon, strength of solution is 0.1mol/L, and dipping time is 1 ~ 2 hour, is taken out by porous carbon dry after dipping;
(3) be placed on by dried porous carbon to vacuumize continuously in process furnace, argon shield process furnace or nitrogen protection process furnace and sinter, sintering temperature is 500 DEG C, obtains the porous silver with pine structure;
(4) make etching reagent with the mixed solution of hydrofluoric acid, hydrogen peroxide, water, the volume ratio of hydrofluoric acid, hydrogen peroxide, water is 6:2:2, and with etching reagent submergence silicon single crystal;
(5) be pressed in silicon plane by porous silver, make it abundant contact, to play katalysis, corrosion reaction is occurred, duration of contact is 20 minutes;
(6) soak in the silicon face immersion silicon fluoride after corrosion and Virahol mixed solution 4 ~ 15 days, silicon fluoride and Virahol volume ratio are 1:6, take out drying subsequently, just obtained silica-based super hydrophobic surface.
Embodiment 1
Kahikatea wood is placed in Wood carbonization stove and is heated to 500 DEG C with the temperature rise rate of 2 DEG C/min, the obtained porous carbon with kahikatea timber structure; Be flood 2 hours in the silver nitrate solution of 0.1mol/L again in concentration by this porous carbon, after dipping, take out drying; Dried porous carbon is sintered to 500 DEG C in argon shield process furnace, obtains the porous silver with kahikatea timber structure; Figure 1 shows that the stereoscan photograph of obtained porous silver microtexture, this porous silver has left over the microtexture of kahikatea wood well as seen.Figure 2 shows that the X diffracting spectrum of obtained porous silver, is silver from diffraction peak this material known.The mixed solution etching reagent of preparation hydrofluoric acid, hydrogen peroxide, water, the volume ratio of hydrofluoric acid, hydrogen peroxide, water is 6:2:2, and with etching reagent submergence silicon single crystal, now corrosion-free reaction generation; Be pressed in silicon plane by porous silver, make it abundant contact, to play katalysis, corrosion reaction is occurred, duration of contact is 20 minutes, and under the catalysis of silver, etching reagent corrodes silicon rapidly.Figure 3 shows that the silicon face microtexture stereoscan photograph after corrosion, silicon face defines the columnar protrusions contrary with porous silver structure convex-concave.Immersed in silicon fluoride and Virahol mixed solution by silicon face after corrosion and soak 8 days, silicon fluoride and Virahol volume ratio are 1:6, take out drying subsequently, i.e. obtained silica-based super hydrophobic surface.Figure 4 shows that obtained silica-based super hydrophobic surface and the contact angle of water, θ
contact angle=155 °, reach super-hydrophobicity.
Embodiment 2
Kahikatea wood is placed in Wood carbonization stove and is heated to 800 DEG C with the temperature rise rate of 1 DEG C/min, the obtained porous carbon with kahikatea timber structure; Be flood 1 hour in the silver nitrate solution of 0.1mol/L again in concentration by this porous carbon, after dipping, take out drying; Dried porous carbon is sintered to 500 DEG C in argon shield process furnace, obtains the porous silver with kahikatea timber structure.The mixed solution etching reagent of preparation hydrofluoric acid, hydrogen peroxide, water, the volume ratio of hydrofluoric acid, hydrogen peroxide, water is 6:2:2, and with etching reagent submergence silicon single crystal.Be pressed in silicon plane by porous silver, make it abundant contact, to play katalysis, corrosion reaction is occurred, duration of contact is 20 minutes.Immersed in silicon fluoride and Virahol mixed solution by silicon face after corrosion and soak 15 days, silicon fluoride and Virahol volume ratio are 1:6, take out drying subsequently, i.e. obtained silica-based super hydrophobic surface.
Embodiment 3
Metasequoia wood is placed in Wood carbonization stove and is heated to 500 DEG C with the temperature rise rate of 2 DEG C/min, the obtained porous carbon with metasequoia timber structure; Be flood 2 hours in the silver nitrate solution of 0.1mol/L again in concentration by this porous carbon, after dipping, take out drying; Dried porous carbon is sintered to 500 DEG C in argon shield process furnace, obtains the porous silver with metasequoia timber structure.The mixed solution etching reagent of preparation hydrofluoric acid, hydrogen peroxide, water, the volume ratio of hydrofluoric acid, hydrogen peroxide, water is 6:2:2, and with etching reagent submergence silicon single crystal.Be pressed in silicon plane by porous silver, make it abundant contact, to play katalysis, corrosion reaction is occurred, duration of contact is 20 minutes.Immersed in silicon fluoride and Virahol mixed solution by silicon face after corrosion and soak 4 days, silicon fluoride and Virahol volume ratio are 1:6, take out drying subsequently, i.e. obtained silica-based super hydrophobic surface.
Claims (5)
1. prepare a method for silica-based super hydrophobic surface as catalytic erosion with pine structural porous silver, it is characterized in that, step is as follows:
(1) take pine as raw material, pine is placed in non-oxidizing atmosphere sintering oven and sinters, sintering temperature is not less than 500 DEG C, and temperature rise rate, not higher than 3 DEG C/min, obtains the porous carbon with pine structure;
(2) flooded in silver nitrate solution by porous carbon, strength of solution is 0.1mol/L, and dipping time is 1 ~ 2 hour, is taken out by porous carbon dry after dipping;
(3) be placed in oxygen-free atmosphere process furnace by dried porous carbon and sinter, sintering temperature is 450 ~ 550 DEG C, obtains the porous silver with pine structure;
(4) etching reagent is made with the mixed solution of hydrofluoric acid, hydrogen peroxide and water, and with etching reagent submergence silicon single crystal;
(5) be pressed in silicon single crystal plane by the porous silver with pine structure, make it abundant contact, duration of contact is 19 ~ 21 minutes;
(6) monocrystalline silicon surface after corrosion is immersed immersion in silicon fluoride and Virahol mixed solution and be greater than 4 days, silicon fluoride and Virahol volume ratio are 1:4 ~ 1:8, take out drying subsequently, just obtained silica-based super hydrophobic surface.
2. prepare the method for silica-based super hydrophobic surface as claimed in claim 1 with pine structural porous silver as catalytic erosion, it is characterized in that, in step 1, described pine is that kahikatea wood or metasequoia are wooden; Described non-oxidizing atmosphere sintering oven is Wood carbonization stove, vacuumizes process furnace, Ar-sintering stove or nitrogen protective sintering stove continuously; Described sintering temperature is 500 ~ 800 DEG C; Described temperature rise rate is 1 ~ 2 DEG C/min.
3. prepare the method for silica-based super hydrophobic surface as claimed in claim 1 as catalytic erosion with pine structural porous silver; it is characterized in that; in step 3, described oxygen-free atmosphere process furnace is for vacuumize process furnace, argon shield process furnace or nitrogen protection process furnace continuously.
4. prepare the method for silica-based super hydrophobic surface as claimed in claim 1 as catalytic erosion with pine structural porous silver, it is characterized in that, in step 4, in mixed solution, the volume ratio of hydrofluoric acid, hydrogen peroxide, water is 6:2:2.
5. prepare the method for silica-based super hydrophobic surface as claimed in claim 1 as catalytic erosion with pine structural porous silver, it is characterized in that, in step 6, described silicon fluoride and Virahol volume ratio are 1:6; Described soak time is 4 ~ 15 days.
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Cited By (5)
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| CN106498502A (en) * | 2016-12-06 | 2017-03-15 | 南京理工大学 | A kind of method that utilization metal auxiliary etch has timber reverse geometry silicon face |
| CN109680312A (en) * | 2019-01-24 | 2019-04-26 | 南京理工大学 | The method for plating the preparation super-hydrophobic Zinc material of sheet as template electric using natural timber |
| CN111935965A (en) * | 2020-07-14 | 2020-11-13 | 西安工程大学 | Preparation method of silver/biomass porous carbon electromagnetic wave absorption composite material |
| CN112125706A (en) * | 2020-09-26 | 2020-12-25 | 河北银瓷天成文化传播有限公司 | Preparation method of silver porcelain tea caddy |
| CN116332170A (en) * | 2023-03-30 | 2023-06-27 | 华中师范大学 | Pine substrate, three-dimensional graphite alkyne and preparation method of pine substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109680312A (en) * | 2019-01-24 | 2019-04-26 | 南京理工大学 | The method for plating the preparation super-hydrophobic Zinc material of sheet as template electric using natural timber |
| CN111935965A (en) * | 2020-07-14 | 2020-11-13 | 西安工程大学 | Preparation method of silver/biomass porous carbon electromagnetic wave absorption composite material |
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| CN116332170A (en) * | 2023-03-30 | 2023-06-27 | 华中师范大学 | Pine substrate, three-dimensional graphite alkyne and preparation method of pine substrate |
| CN116332170B (en) * | 2023-03-30 | 2024-04-19 | 华中师范大学 | Pine substrate, three-dimensional graphite alkyne and preparation method of pine substrate |
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