CN102453465A - Adhesive super-hydrophobic material and preparation method thereof - Google Patents

Adhesive super-hydrophobic material and preparation method thereof Download PDF

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CN102453465A
CN102453465A CN2010105213059A CN201010521305A CN102453465A CN 102453465 A CN102453465 A CN 102453465A CN 2010105213059 A CN2010105213059 A CN 2010105213059A CN 201010521305 A CN201010521305 A CN 201010521305A CN 102453465 A CN102453465 A CN 102453465A
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super hydrophobic
silicon
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matrix
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徐杰
王敏
陈晨
马继平
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Dalian Institute of Chemical Physics of CAS
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Abstract

The invention relates to an adhesive super-hydrophobic material and a preparation method thereof. The material refers to silicon dioxide nanoparticles containing organic groups. A surface with dual nanometer roughness is obtained by taking the material as a constructing unit and depositing on a substrate. The surface has super-hydrophobic performance and very high adhesion, a contact angle is 140-170 degrees, and water drops are prevented from falling off under the condition of inclination or reversion. The method has the advantages of easiness for operating, readily-available raw materials, low cost and wide application prospects on conveying, transfer and separation of water.

Description

A kind of adhesive type super hydrophobic material and preparation method thereof
Technical field
The present invention relates to a kind of super-hydrophobic adhesive type material and preparation method thereof.
Background technology
The super-hydrophobic surface that is meant is gone up the apparent contact angle of water and is surpassed a kind of special surface phenomenon of 150 °.In recent years, super hydrophobic surface has caused that people pay close attention to greatly, and it has a wide range of applications in fields such as many fields such as automatically cleaning material, microfluidic device, catalysis, oil recovery, covering with paint, waterproof and biomaterial.Most typical example is exactly the lotus leaf surface of occurring in nature, and water droplet can freely roll on the blade face, can be with taking away attached to the pollutents such as dust on the blade face, thus the surface is kept clean.Two kinds of methods of the general employing of the preparation of tradition super hydrophobic surface: a kind of is the material of modifying low surface energy at uneven surface; Another kind is to make up coarse structure at water repellent surface.About the method for production of super-hydrophobic uneven surface, mainly contain phase separation method, template, sol-gel method, electricity and spin method, etching method, etch, self-assembly, chemical vapour deposition and other methods.According to the rolling effect of liquid on the surface, super hydrophobic surface can be divided into again scolds water type and adhesive type super hydrophobic surface.The contact angle of scolding water type super hydrophobic surface and water droplet is greater than 150 °, but very little to the water droplet adhesive power, water droplet is easy to tumble from the surface.There is this super hydrophobic surface in a large number in nature, such as lotus leaf, the feather of bird and water worm etc. all be this low adhesive power scold water type surface.Because this super hydrophobic surface self-cleaning performance, a large amount of research all are absorbed in the synthetic of this surface.The adhesive type super hydrophobic surface not only with the contact angle of water droplet greater than 150 °, and water droplet had very strong adhesive power, with surface tilt or be inverted, water droplet can not roll.Though this super hydrophobic surface can not automatically cleaning, the adhesive power that this kind is high to liquid helps on micron level, water droplet being operated, and shifts at free of losses liquid, and aspects such as microfluidic control system and biosensor show good application prospects.Comparatively speaking, the research of adhesive type super hydrophobic surface is less.Existing research all concentrates in the structure control to the surface, utilizes capillary force that liquid is adhered to.The method that develops a kind of easy synthetic super-hydrophobic adhesive type surface has great importance
Summary of the invention
The present invention provides a kind of adhesive type super hydrophobic material and preparation method thereof.
This material is a kind of nano SiO 2 particle that contains organic group, regulates and control the adhesive power size through the chemical ingredients of control surface.As construction unit, on matrix, deposit the surface that obtains having the two-dimensional nano roughness with this material.Matrix can be sheet glass, silicon chip, metal or MOX.
Two kinds of methods of the general employing of the preparation of tradition super hydrophobic surface: a kind of is the material of modifying low surface energy at uneven surface; Another kind is to make up coarse structure at water repellent surface.With last different, the nano SiO 2 particle that the present invention adopts the low surface energy organism to modify is that construction unit deposits on matrix, obtains having the surface of double nanometer roughness.A low surface energy material and roughness step in deposition process realizes.Operate more simple, convenient.Traditional coarse structure has only a heavy roughness, perhaps a bicron rank roughness and a heavy Nano grade roughness.The surface of the present invention's preparation has double nanometer coarse structure.The nano SiO 2 particle body is assembled into a heavy nanometer roughness, and the silica sphere of synthetic organic decoration of the present invention itself is very coarse, forms the second heavy nanometer coarse structure, and double coarse structure is all at Nano grade.
With come the modulation adhesive power different through the control surface structure; The present invention regulates and control the adhesive power size through the control chemical ingredients; Can obtain super-hydrophobic adhesive type material; Contact angle and has very strong adhesive power between 140-170 °, water droplet tilt or inverted situation under do not return under the landing.
Precipitation agent is water miscible; And silane is oil-soluble, for synthetic uniform particle diameter, the nano SiO 2 particle that contains organic group of high dispersive; Must make the abundant and uniform contact of precipitation agent and silane; The present invention adopt tensio-active agent and cosurfactant with the ammonia soln high dispersive among oil phase, make silane and precipitation agent fully and uniform contact, precipitation from homogeneous solution.Can on matrix, form a super hydrophobic surface through simple deposition and burin-in process.
Said adhesive type super hydrophobic surface preparation process, can operate as follows:
A) dispersion and the precipitation from homogeneous solution thereof of inorganic precipitant in oil phase: tensio-active agent, organic phase, cosurfactant and ammoniacal liquor are configured to solution A according to a certain percentage.A certain amount of tetraethoxy or methyl silicate are the silicon source, wiring solution-forming B.Under the room temperature, in the A microemulsion, add solution B, stir 6~48h.
The mass ratio of gained final blending solution is 1~10 tensio-active agent: 0.5~6 ammoniacal liquor: 5~15 organic phases: 0~6 cosurfactant: 1 silane: 0.05~1.5 organosilane.Ammonia concn is 1~30wt%.
The acetone breakdown of emulsion that adds 1-10 times of silicon source quality, the centrifugal solid that obtains, the alcohol reflux 5~30min of 5-50 times of silicon source quality of adding; Centrifugal; Repeat 2~5 washings, be dispersed in the ethanol, getting silicon-dioxide alcohol dispersion liquid silicon-dioxide quality concentration is 1~20wt%;
B) formation of super hydrophobic surface: matrix is used the washing composition ultrasonic cleaning earlier, and water, acetone clean 2~6 times repeatedly again, and the silicon-dioxide alcohol dispersion liquid is deposited on matrix surface, and 20~200 ℃ of down aging 1~48h obtain super hydrophobic surface.
Said tensio-active agent is C8-20 linear alkylbenzene sulphonic acid or the α-sodium olefin sulfonate in the AS; Or be organic primary amine, Np series or the tween series of surfactants of the C8-20 long-chain in the nonionogenic tenside, or be the CTAB in the cats product.Said organic phase is hexanaphthene, normal hexane or toluene; Cosurfactant is propyl carbinol, Pentyl alcohol, n-hexyl alcohol or n-Octanol.Organic group be methyl, ethyl, propyl group, vinyl, phenyl, dodecyl, octadecyl, trifluoro propyl, perfluor certain herbaceous plants with big flowers base and pentafluorophenyl group one or several.Matrix is sheet glass, silicon chip, metal or MOX.
The nano SiO 2 particle of the organic decoration of the present invention's preparation, controlled amount, particle diameter is in 20~1000nm (see figure 1).Prepared surface has the coarse structure (see figure 2).Prepared super-hydrophobic adhesive type surface contact angle is 140~170 °, and water droplet is in 90 ° or the 180 ° of inclinations (see figure 3) down of can not rolling.
Description of drawings
The transmission electron microscope photo of synthetic silica dioxide granule A in Fig. 1 instance 1.
Adopt the super hydrophobic surface stereoscan photograph of silicon-dioxide A preparation in Fig. 2 instance 7.
Adopt the super hydrophobic surface water droplet contact angle picture of silicon-dioxide A preparation in Fig. 3 instance 7.
Embodiment
Tensio-active agent, organic phase, cosurfactant and ammoniacal liquor are configured to solution A according to a certain percentage.A certain amount of tetraethoxy or methyl silicate and organosilane wiring solution-forming B.
Under the room temperature, in the A microemulsion, splash into solution B, stir 6~48h.The mass ratio of gained final blending solution is 1~10 tensio-active agent: 0.5~6 ammoniacal liquor: 5~15 organic phases: 0~6 cosurfactant: 1 silane: 0.05~1.5 organosilane.The acetone breakdown of emulsion that adds 1-10 times of silicon source quality, the centrifugal solid that obtains, the alcohol reflux 5~30min of 5-50 times of silicon source quality of adding; Centrifugal, repeat 2~5 washings, be dispersed in the ethanol; Get the silicon-dioxide alcohol dispersion liquid, silicon-dioxide quality concentration is 1~20wt%; Matrix use earlier the washing composition ultrasonic cleaning, water repeatedly again, and acetone 2~6 times deposits the silicon-dioxide alcohol dispersion liquid on matrix surface, and 20~200 ℃ keep 1~48h down, obtain super hydrophobic surface.
Through embodiment method provided by the invention is detailed below, but do not limit the present invention in any form.
Embodiment 1 silicon-dioxide A (Ph-SiO 2) preparation
Get 8.0g Np-12,15.0g hexanaphthene, 3.0g n-Octanol and 5.0g 10wt%, get solution A; 1.0g tetraethoxy 0.5g phenyl base Trimethoxy silane is a solution C; Under agitation solution B is added in the solution D aging 8h; Then, add 8g acetone, stir 30min, the centrifugal solid that obtains;
In this solid, add 30g ethanol, heated and stirred 10min is centrifugal; Repeat this step 5 time, clean until removal of surfactant; The gained solid dispersed is in 10g ethanol.As shown in Figure 1, can find out the nano SiO 2 particle of organic decoration, particle diameter is even, and particle diameter is at 100nm, and the surface is very coarse.
The preparation of embodiment 2 silicon-dioxide B-L
The same materials A of the preparation method of material B-L, difference are on the kind and add-on of organosilane that the kind and the add-on of the concrete organosilane that adopts are seen table 1, and resulting material is listed in table 1.
The kind and the add-on of the organosilane that adopts in table 1 material B-H preparation
Figure BSA00000320449900031
Embodiment 3 silicon-dioxide I (Me-SiO 2) preparation
Get 2.0g X 2073,10.0g normal hexane, 1.0g propyl carbinol and 4.0g 15wt% ammoniacal liquor mix microemulsion A; 1.0g methyl silicate and 0.5g methyltrimethoxy silane are solution B.Under agitation solution B is splashed in the solution D aging 15h; Add 10g acetone then, stir 30min, the centrifugal solid that obtains;
In this solid, add 30g ethanol, heated and stirred 10min is centrifugal; Repeat this step 4 time, clean until removal of surfactant.The gained solid dispersed is in 10g ethanol.
The preparation of embodiment 4 silicon-dioxide J-R
The preparation method of material J-R is with material I, and difference is the kind and the add-on of organosilane, and concrete organosilane and the add-on kind that adopts seen table 2, and resulting material is listed in table 2.
The kind and the add-on of the organosilane that adopts in the table 2 material J-R preparation
Figure BSA00000320449900041
Embodiment 5 silicon-dioxide S (Do-SiO 2) preparation
Get 5.0g CTAB, 12.0g toluene, 2.0g Pentyl alcohol and 4.5g 5wt% ammoniacal liquor mix microemulsion liquid A; 1.0g methyl silicate and 0.1g dodecyl Trimethoxy silane are solution B; Under agitation solution C is splashed in the solution A aging 24h; Then, add 10g acetone, stir 30min, the centrifugal solid that obtains;
In this solid, add 30g ethanol, heated and stirred 10min is centrifugal; Repeat this step 3 time, clean until removal of surfactant.The gained solid dispersed is in 10g ethanol.
The preparation of embodiment 6 silicon-dioxide U-Z
The preparation method of material T-Z is with material S, and difference is the kind and the add-on of organosilane, and concrete organosilane and the add-on kind that adopts seen table 3, and resulting material is listed in table 3.
The kind and the add-on of the organosilane that adopts in the table 3 silicon-dioxide T-Z preparation
Figure BSA00000320449900051
The preparation of embodiment 7 super hydrophobic surfaces
Sheet glass is used earlier the washing composition ultrasonic cleaning, and water cleans 3 times repeatedly again, acetone 4 times, drying.The A-Z silicon-dioxide alcohol dispersion liquid for preparing is deposited on matrix surface, under 150 ° of temperature, aging 24h.
Shown in Fig. 2 and 3, can find out that prepared surface has coarse structure.This surface has superhydrophobic property, and the water droplet contact angle is greater than 150 °, and has very strong adhesion property, and water droplet can not fall down under inverted situation.
The super hydrophobic material of method preparation provided by the invention can adhere on the different matrixes, forms a super hydrophobic surface, has the ultra-hydrophobic high sticking performance; This method is simple to operate, and raw material is easy to get, and cost is low; Shift at free of losses liquid, liquid carries biomaterial, the microfluidic control system; Biological micro liquid shifts, and aspects such as parting material and biosensor are with a wide range of applications.

Claims (7)

1. adhesive type super hydrophobic material, it is characterized in that: this material is a kind of nano SiO 2 particle that contains organic group; This material is attached to matrix surface, comes the modulation adhesive power through the control chemical ingredients.
2. according to the said adhesive type super hydrophobic material of claim 1, it is characterized in that:
As construction unit, on matrix, deposit the surface that obtains having double nanometer roughness with described material; This material surface has ultra-hydrophobicity, and contact angle and has very strong adhesive power between 140~170 °, water droplet tilt or inverted situation under can landing under.
3. according to claim 1 or 2 said adhesive type super hydrophobic materials, it is characterized in that:
Matrix is sheet glass, silicon chip, metal or MOX.
4. according to the said adhesive type super hydrophobic material of claim 1; It is characterized in that: the said nano SiO 2 particle that contains organic group; Organic group is one or more in the organic groups such as methyl, ethyl, propyl group, vinyl, phenyl, dodecyl, octadecyl, trifluoro propyl, perfluor certain herbaceous plants with big flowers base and pentafluorophenyl group, and mass content is 0.1~60%; The silica particles of organic decoration is coarse, and particle diameter is 20~1000nm.
5. the preparation method of the said adhesive type super hydrophobic material of claim 1 is characterized in that:
A) inorganic precipitant disperses and precipitation from homogeneous solution in oil phase: tensio-active agent, organic phase, cosurfactant and precipitation agent ammoniacal liquor proportionally are configured to microemulsion A; Tetraethoxy or methyl silicate and organosilane are the silicon source, wiring solution-forming B; Under the room temperature, in the A microemulsion, splash into solution B, stir 6~48h;
The acetone breakdown of emulsion that adds 1-10 times of silicon source quality, the centrifugal solid that obtains, the alcohol reflux 5~30min of 5-50 times of silicon source quality of adding; Centrifugal, repeat 2~5 washings, be dispersed in the ethanol; Get the silicon-dioxide alcohol dispersion liquid, silicon-dioxide quality concentration is 1~20wt%;
The mass ratio of gained final blending solution is 1~10 tensio-active agent: 0.5~6 ammoniacal liquor: 5~15 organic phases: 0~6 cosurfactant: 1 tetraethoxy or methyl silicate: 0.05~1.5 organosilane; Ammonia concn is 1~30wt%;
B) formation of super hydrophobic surface: matrix is used earlier the washing composition ultrasonic cleaning, and water cleaning 2~6 times again, acetone 2~6 times deposit the silicon-dioxide alcohol dispersion liquid on matrix surface, and 20~200 ℃ keep 1~48h down, obtain super hydrophobic surface.
6. according to the described preparation method of claim 5; It is characterized in that: said tensio-active agent is C8-20 linear alkylbenzene sulphonic acid or the α-sodium olefin sulfonate in the AS; Or be organic primary amine, Np series or the tween series of surfactants of the C8-20 long-chain in the nonionogenic tenside, or be the CTAB in the cats product; Said organic phase is hexanaphthene, normal hexane or toluene; Cosurfactant is propyl carbinol, Pentyl alcohol, n-hexyl alcohol or n-Octanol.
7. according to the described preparation method of claim 5, said organosilane is a kind of in methyltrimethoxy silane, ethyl trimethoxy silane, propyl trimethoxy silicane, vinyltrimethoxy silane, r-chloropropyl trimethoxyl silane, phenyltrimethoxysila,e, dodecyl Trimethoxy silane, octadecyl base Trimethoxy silane, trifluoro propyl Trimethoxy silane, pentafluorophenyl group Trimethoxy silane and the corresponding Ethoxysilane thereof or more than two kinds.
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CN108264678A (en) * 2018-02-08 2018-07-10 青岛软盛塑业有限公司 Hydrophobic type bubble chamber film and preparation method thereof
CN108264678B (en) * 2018-02-08 2021-01-26 青岛软盛塑业有限公司 Hydrophobic bubble film and preparation method thereof

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