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Publication numberCN102453465 A
Publication typeApplication
Application numberCN 201010521305
Publication date16 May 2012
Filing date27 Oct 2010
Priority date27 Oct 2010
Also published asCN102453465B
Publication number201010521305.9, CN 102453465 A, CN 102453465A, CN 201010521305, CN-A-102453465, CN102453465 A, CN102453465A, CN201010521305, CN201010521305.9
Inventors徐杰, 王敏, 陈晨, 马继平
Applicant中国科学院大连化学物理研究所
Export CitationBiBTeX, EndNote, RefMan
External Links: SIPO, Espacenet
Adhesive super-hydrophobic material and preparation method thereof
CN 102453465 A
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.
Claims(7)  translated from Chinese
1. 一种粘附型超疏水材料,其特征在于:该材料是一种含有有机基团的二氧化硅纳米颗粒;该材料附着于基体表面,通过控制化学成分来调变粘附力。 An adhesion type super-hydrophobic material, wherein: the material is an organic group comprising silica nanoparticles; the material is attached to the substrate surface, by controlling the chemical composition to modulate adhesion.
2.按照权利要求1所述粘附型超疏水材料,其特征在于:以所述的材料作为构建单元,在基体上进行沉积得到具有二重纳米粗糙度的表面;该材料表面具有超疏水性能,接触角在140〜170之间,而且具有很强的粘附力,水滴在倾斜或者倒置的情况下不会滑落下来。 2. according to claim 1 adherent superhydrophobic materials, characterized in that: in said material as a construction unit, deposited on a substrate having a surface roughness obtained double nm; superhydrophobic surface of the material properties , the contact angle between 140~170 , and has a strong adhesion, water droplets in a tilted or inverted situation will not fall down.
3.按照权利要求1或2所述粘附型超疏水材料,其特征在于:基体是玻璃片、硅片、金属或金属氧化物。 3. according to claim 1 or claim 2 adherent superhydrophobic materials, characterized in that: the substrate is glass, silicon, metal or metal oxide.
4.按照权利要求1所述粘附型超疏水材料,其特征在于:所述含有有机基团的二氧化硅纳米颗粒,有机基团为甲基、乙基、丙基、乙烯基、苯基、十二烷基、十八烷基、三氟丙基、全氟葵基和五氟苯基等有机基团中的一种或者多种,质量含量为0. 1〜60% ;有机修饰的二氧化硅颗粒表面粗糙,粒径为20〜lOOOnm。 According to claim 1 wherein the adhesion-type super-hydrophobic material, wherein: said organic group-containing silica nanoparticles, the organic groups are methyl, ethyl, propyl, vinyl, phenyl , dodecyl, octadecyl, trifluoropropyl, perfluoro decyl and pentafluorophenyl other organic groups of one or more, the quality of the content of 0. 1~60%; organic modified silica particles surface roughness, particle size 20~lOOOnm.
5. 一种权利要求1所述粘附型超疏水材料的制备方法,其特征在于:a)无机沉淀剂在油相中分散及其均勻沉淀:将表面活性剂、有机相、助表面活性剂和沉淀剂氨水按照比例配置成微乳液A ;正硅酸乙酯或者正硅酸甲酯和有机硅烷为硅源,配成溶液B ;室温下,往A微乳液中滴入溶液B,搅拌6〜48h ;加入1-10倍硅源质量的丙酮破乳,离心得到固体,加入5-50倍硅源质量的乙醇回流5〜30min,离心,重复2〜5次洗涤,分散在乙醇中,得二氧化硅乙醇分散液,二氧化硅质量浓度为1〜20wt% ;所得最终混合溶液的质量比为1〜10表面活性剂:0.5〜6氨水:5〜15有机相:0〜6助表面活性剂:1正硅酸乙酯或者正硅酸甲酯:0. 05〜1. 5有机硅烷;氨水浓度为1〜30wt% ;b)超疏水表面的形成:基体先用洗涤剂超声清洗,再用水清洗2〜6次、丙酮清洗2〜 6次,将二氧化硅乙醇分散液在基体表面上沉积,20〜200C下保持1〜48h,得到超疏水表面。 The method for preparing a superhydrophobic adherent material according to claim 5., characterized in that: a) an inorganic precipitating agent in the oil phase and uniformly dispersed precipitation: a surfactant, an organic phase, cosurfactant and precipitating agent is configured according to the proportion of ammonia microemulsion A; TEOS or methyl silicate and organic silane as the silicon source, dubbed solution B; room temperature drops to A microemulsion solution B, stir 6 ~48h; added 1-10 times the mass of the silicon source demulsification acetone, centrifuged to obtain a solid, the silicon source is added 5-50 times the mass of ethanol was refluxed for 5~30min, centrifugation was repeated 2 ~ 5 times washing, dispersing in ethanol to give ethanol dispersion liquid of silica, the silica concentration of 1~20wt%; final mass ratio of the resulting mixed solution of a surfactant for 1~10: 0.5~6 ammonia: 5 ~ 15 organic phase: 0~6 cosurfactant Agent: a TEOS or methyl silicate: 0 05~1 5 organosilane; ammonia concentration 1~30wt%; b) forming a super-hydrophobic surface: matrix first ultrasonic cleaning with detergent, then 2 ~ 6 times washed with water, acetone 2 ~ 6 times, ethanol dispersion of the silica surface of the substrate is deposited, 20~200 C while maintaining 1~48h, to give a superhydrophobic surface.
6.按照权利要求5所述的制备方法,其特征在于:所述表面活性剂为阴离子表面活性剂中的C8-20直链烷基苯磺酸钠或α -烯基磺酸钠,或为非离子表面活性剂中的C8-20长链的有机伯胺、Np系列或吐温系列表面活性剂,或为阳离子表面活性剂中的十六烷基三甲基溴化胺;所述有机相为环己烷、正己烷或甲苯;助表面活性剂为正丁醇、正戊醇、正己醇或正辛醇。 6. The production method according to claim 5, wherein, wherein: the surfactant is an anionic surfactant of C8-20 linear alkylbenzene sulfonate or α - olefin sulfonate, or Non-ionic surfactants in C8-20 long-chain organic primary amine, Np series or Tween series surfactants, or cationic surfactant cetyl trimethyl ammonium bromide; the organic phase cyclohexane, n-hexane or toluene; co-surfactant is n-butanol, n-pentanol, n-hexanol or n-octanol.
7.按照权利要求5所述的制备方法,所述有机硅烷为甲基三甲氧基硅烷、乙基三甲氧基硅烷、丙基三甲氧基硅烷、乙烯基三甲氧基硅烷、氯丙基三甲氧基硅烷、苯基三甲氧基硅烷、十二烷基三甲氧基硅烷、十八烷基基三甲氧基硅烷、三氟丙基三甲氧基硅烷、五氟苯基三甲氧基硅烷及其相对应的乙氧基硅烷中的一种或二种以上。 7. A production method according to claim 5, wherein, the organic silane is methyl trimethoxysilane, ethyl trimethoxysilane, propyl trimethoxysilane, vinyl trimethoxysilane, chloropropyl trimethoxy silane, phenyl trimethoxy silane, dodecyl trimethoxy silane, octadecyl alkyl trimethoxysilane, trifluoropropyl trimethoxysilane, pentafluorophenyl trimethoxysilane and the corresponding ethoxy silane of one or two or more kinds.
Description  translated from Chinese

一种粘附型超疏水材料及其制备方法 An adhesion-type super-hydrophobic material and method

技术领域 FIELD

[0001] 本发明涉及到一种超疏水粘附型材料及其制备方法。 [0001] The present invention relates to a super-hydrophobic adherent material and method. 背景技术 BACKGROUND

[0002] 超疏水是指表面上水的表观接触角超过150的一种特殊表面现象。 [0002] superhydrophobic means apparent contact angle of water on the surface above 150 of a special surface phenomenon. 近年来,超疏水表面引起了人们极大的关注,它在自清洁材料、微流体装置、催化、采油、涂饰、防水、和生物材料等许多领域等领域中有着广泛的应用前景。 In recent years, the superhydrophobic surface has aroused great concern, it has a broad application prospects in the field of self-cleaning materials, microfluidic devices, catalysis, production, finishing, waterproofing, and biological materials, such as in many other fields. 最典型的例子就是自然界中的荷叶表面,水滴在叶面上可以自由滚动,能够将附着在叶面上的灰尘等污染物带走,从而使表面保持清洁。 The most typical example is the nature of the lotus leaf surface, water droplets can roll freely in the leaf surface, can be attached to the leaf surface of dust and other pollutants away, so that the surface clean. 传统超疏水表面的制备一般采用两种方法:一种是在粗糙表面修饰低表面能的物质;另一种是在疏水性表面构建粗糙结构。 Preparation of traditional superhydrophobic surface generally use two methods: one is a roughened surface modification of low surface energy material; the other is constructed in a hydrophobic surface roughness. 关于超疏水粗糙表面的研制方法,主要有相分离法、模板法、溶胶-凝胶法、电纺法、刻蚀法、腐蚀法、自组装、化学气相沉积及其他方法。 On the development of methods rough superhydrophobic surface, mainly phase separation, template, sol - gel, electro-spinning method, etching, etching, self-assembly, chemical vapor deposition, and other methods. 根据液体在表面的滚动效果,超疏水表面又可分为斥水型和粘附型超疏水表面。 According to the liquid on the surface of the rolling effect, super-hydrophobic surface can be divided into water-repellent and adhesion-type super-hydrophobic surfaces. 斥水型超疏水表面与水滴的接触角大于150,但是对水滴粘附力很小,水滴很容易从表面滚落。 Water-repellent superhydrophobic surface contact angle with water droplets of larger than 150 , but small water droplets adhesion, water droplets roll off the surface easily. 自然界大量存在这种超疏水表面,比如荷叶,鸟的羽毛和水虫等都是这种低粘附力的斥水型表面。 Nature, the presence of such a large number of super-hydrophobic surfaces, such as leaves, bird feathers and water insects and other such low adhesion are water-repellent surface. 由于这种超疏水表面自清洁性能,大量的研究都专注这种表面的合成。 Because of this super-hydrophobic surface self-cleaning properties, a large number of studies have focused on the synthesis of such surfaces. 粘附型超疏水表面不但与水滴的接触角大于150,而且对水滴具有很强的粘附力,将表面倾斜或者倒置, 水滴都不会滚动下来。 Adhesive based superhydrophobic surface contact angle with water droplets is not only greater than 150 , but also has a strong adhesion of water droplets, the surface is inclined or upside down, the water droplets will not roll down. 这种超疏水表面虽然不能够自清洁,但是此种对液体高的粘附力,有利于在微米级别上对水滴进行操作,在无损失液体转移,微流控制体系和生物传感器等方面表现出很好的应用前景。 Such super-hydrophobic surface, while not capable of self-cleaning, but such a high adhesion of the liquid, in favor of the droplets in the micron-level operation, without loss of liquid transfer, the control system and aspects of microfluidic biosensors exhibit good application prospects. 相对而言,粘附型超疏水表面研究的较少。 In contrast, less adherent superhydrophobic surface studies. 现有的研究都集中在对表面的结构控制上,利用毛细管力对液体进行粘附。 Existing studies have focused on the structure of the control surface, by capillary force of the liquid adhesion. 发展一种简便合成超疏水粘附型表面的方法具有重要的意义 The development of a simple synthesis of superhydrophobic surface adherent method has important significance

发明内容 SUMMARY

[0003] 本发明提供一种粘附型超疏水材料及其制备方法。 [0003] The present invention provides an adherent superhydrophobic material and method.

[0004] 该材料是一种含有有机基团的二氧化硅纳米颗粒,通过控制表面的化学成分来调控粘附力大小。 [0004] This material is an organic group comprising silica nanoparticles, by controlling the chemical composition of the surface to regulate the adhesion size. 以该材料作为构建单元,在基体上进行沉积得到具有二维纳米粗糙度的表面。 In the material as a construction unit, deposited on the substrate to obtain a surface having a two-dimensional roughness. 基体可以是玻璃片,硅片,金属或金属氧化物。 The substrate may be glass, silicon, metal or metal oxide.

[0005] 传统超疏水表面的制备一般采用两种方法:一种是在粗糙表面修饰低表面能的物质;另一种是在疏水性表面构建粗糙结构。 Preparation of [0005] traditional superhydrophobic surface generally use two methods: one is in a roughened surface modified low surface energy material; the other is constructed in a hydrophobic surface roughness. 与上不同,本发明采用低表面能有机物修饰的二氧化硅纳米颗粒为构建单元在基体上沉积,得到具有二重纳米粗糙度的表面。 And different, the present invention is the use of low surface energy organic-modified silica nanoparticles as construction unit is deposited on the substrate, to obtain a surface roughness having a double nanometer. 低表面能物质和粗糙度在沉积过程中一步实现。 Low surface energy material and roughness step to achieve during the deposition process. 操作更为简单,方便。 Operation more simple and convenient. 传统的粗糙结构只有一重粗糙度,或者一重微米级别粗糙度和一重纳米级别粗糙度。 Only a rough structure of traditional heavy roughness, or a re-micron level roughness and a heavy nanoscale roughness. 本发明制备的表面具有二重纳米粗糙结构。 Surface preparation of the present invention has a double nanorough structure. 二氧化硅纳米颗粒本体组装成一重纳米粗糙度,本发明合成的有机修饰的二氧化硅表面本身非常粗糙,形成第二重纳米粗糙结构,两重粗糙结构都在纳米级别。 Silica nanoparticles assembled into a body weight scale roughness, the present invention is the synthesis of organo-modified silica surface itself is very rough, forming a second re-nanometer roughness, double roughness are nanoscale.

[0006] 与通过控制表面结构来调变粘附力不同,本发明通过控制化学成分来调控粘附力大小,可以获得超疏水粘附型材料,接触角在140-170之间,而且具有很强的粘附力,水滴 [0006] By controlling the surface structure and to adjust the different variants adhesion, by controlling the chemical composition of the present invention is to regulate the size of adhesion, adhesion can be obtained super-hydrophobic materials, the contact angle between 140-170 , and having strong adhesion, water droplets

3在倾斜或者倒置的情况下不回滑落下来。 3 in a tilted or upside down without falling back down.

[0007] 沉淀剂是水溶性的,而硅烷是油溶性的,为了合成粒径均一,高分散的含有有机基团的二氧化硅纳米颗粒,必须使沉淀剂与硅烷充分且均勻接触,本发明采用表面活性剂和助表面活性剂将氨水溶液高分散在油相之中,使得硅烷与沉淀剂充分且均勻接触,均勻沉淀。 [0007] precipitating agent is water soluble, but are oil soluble silane, for the synthesis of uniform particle size, highly dispersed silica nanoparticles containing organic group, the precipitating agent must be sufficiently and uniformly contacted with the silane, the present invention use of surfactant and co-surfactant in a highly dispersed aqueous ammonia solution into the oil phase, so that the silane and sufficiently and uniformly contact the precipitating agent, homogeneous precipitation. 通过简单沉积和老化处理可以在基体上形成一个超疏水表面。 By simple deposition and aging treatment and form a superhydrophobic surface on the substrate.

[0008] 所述粘附型超疏水表面制备步骤,可按如下步骤操作: [0008] The adherent superhydrophobic surface preparation steps, according to the following steps:

[0009] a)无机沉淀剂在油相中的分散及其均勻沉淀:表面活性剂,有机相,助表面活性剂和氨水按照一定比例配置成溶液A。 [0009] a) an inorganic precipitating agent in dispersed oil phase and homogeneous precipitation of: a surfactant, an organic phase, co-surfactant and aqueous ammonia solution is arranged according to a certain proportion of A. 一定量的正硅酸乙酯或者正硅酸甲酯为硅源,配成溶液B。 TEOS or a certain amount of methyl silicate as silica source, dubbed the solution B. 室温下,往A微乳液中加入溶液B,搅拌6〜48h。 At room temperature, was added to the A microemulsion solution B, stir 6~48h.

[0010] 所得最终混合溶液的质量比为1〜10表面活性剂:0. 5〜6氨水:5〜15有机相:0〜6助表面活性剂:1硅烷:0. 05〜1. 5有机硅烷。 [0010] The resulting final mass ratio of the mixed solution is 1~10 surfactant: ammonia 0 5 to 6: 5 ~ 15 organic phase: 0~6 cosurfactant: 1 Silane: 0 05~1 5 Organic silane. 氨水浓度为1〜30Wt%。 Ammonia concentration 1~30Wt%.

[0011] 加入1-10倍硅源质量的丙酮破乳,离心得到固体,加入5-50倍硅源质量的乙醇回流5〜30min,离心,重复2〜5次洗涤,分散在乙醇中,得二氧化硅乙醇分散液二氧化硅质量浓度为1〜20wt% ; [0011] the silicon source added 1-10 times the mass of acetone demulsification, centrifuged to obtain a solid, the silicon source is added 5-50 times the mass of ethanol was refluxed for 5~30min, centrifugation was repeated 2 ~ 5 times washing, dispersing in ethanol to give silica dispersion of the silica concentration of ethanol was 1~20wt%;

[0012] b)超疏水表面的形成:基体先用洗涤剂超声清洗,再用水、丙酮反复清洗2〜6 次,将二氧化硅乙醇分散液在基体表面上沉积,20〜200C下老化1〜48h,得到超疏水表面。 [0012] b) forming a super-hydrophobic surface: first substrate to ultrasonic cleaning with detergent and then with water, repeatedly washed with acetone 2 ~ 6 times, the silica dispersion in ethanol was aged at the deposition surface of the substrate, 20~200 C under 1~48h, get super-hydrophobic surfaces.

[0013] 所述表面活性剂为阴离子表面活性剂中的C8-20直链烷基苯磺酸钠或α -烯基磺酸钠,或为非离子表面活性剂中的C8-20长链的有机伯胺、Np系列或吐温系列表面活性剂, 或为阳离子表面活性剂中的十六烷基三甲基溴化胺。 [0013] The surfactant is an anionic surfactant of C8-20 linear alkylbenzene sulfonate or α - olefin sulfonate, or non-ionic surface active agents C8-20 long chain organic primary amine, Np series or Tween series surfactants, or cationic surfactant cetyl trimethyl ammonium bromide. 所述有机相为环己烷、正己烷或者甲苯;助表面活性剂为正丁醇、正戊醇、正己醇或正辛醇。 The organic phase is cyclohexane, n-hexane or toluene; co-surfactant is n-butanol, n-pentanol, n-hexanol or n-octanol. 有机基团为甲基、乙基、丙基、乙烯基、苯基、十二烷基、十八烷基、三氟丙基、全氟葵基和五氟苯基一种或者几种。 The organic groups are methyl, ethyl, propyl, vinyl, phenyl, dodecyl, octadecyl, trifluoropropyl, perfluoro decyl and pentafluorophenyl one or several. 基体为玻璃片,硅片,金属或金属氧化物。 Substrate is glass, silicon, metal or metal oxide.

[0014] 本发明制备的有机修饰的二氧化硅纳米颗粒,大小可控,粒径在20〜1000nm(见图1)。 Silica nanoparticles [0014] The present invention is prepared in the organic-modified, controlled size, particle size 20~1000nm (see Figure 1). 所制备的表面具有粗糙结构(见图幻。所制备的超疏水粘附型表面接触角为140〜 170,水滴在90或180倾斜不会滚动下来(见图3)。 Adhesive based superhydrophobic surface having a surface roughness of the prepared (see Fig magic. Prepared contact angle 140~ 170 , water droplets in the 90 or 180 inclined not roll down (see Figure 3).

附图说明 Brief Description

[0015] 图1实例1中合成的二氧化硅颗粒A的透射电镜照片。 [0015] an example of Figure 1, the synthesis of silica particles A TEM image.

[0016] 图2实例7中采用二氧化硅A制备的超疏水表面扫描电镜照片。 [0016] Figure 2 in Example 7 using superhydrophobic surfaces silica A scanning electron micrograph prepared.

[0017] 图3实例7中采用二氧化硅A制备的超疏水表面水滴接触角图片。 [0017] FIG. 3 used in Example 7, superhydrophobic surfaces silica A water droplet contact angle pictures prepared.

具体实施方式 DETAILED DESCRIPTION

[0018] 表面活性剂,有机相,助表面活性剂和氨水按照一定比例配置成溶液A。 [0018] surfactants, organic phase, co-surfactant and aqueous ammonia solution is arranged according to a certain proportion of A. 一定量的正硅酸乙酯或正硅酸甲酯和有机硅烷配成溶液B。 TEOS or the amount of methyl orthosilicate and organosilane match the solution B.

[0019] 室温下,往A微乳液中滴入溶液B,搅拌6〜48h。 [0019] at room temperature, was added dropwise to a solution of A microemulsion B, stirred 6~48h. 所得最终混合溶液的质量比为1〜10表面活性剂:0. 5〜6氨水:5〜15有机相:0〜6助表面活性剂:1硅烷:0.05〜1.5有机硅烷。 The resulting final mass ratio of the mixed solution is 1~10 surfactant: ammonia 0 5 to 6: 5 ~ 15 organic phase: 0~6 cosurfactant: 1 Silane: 0.05~1.5 organosilane. 加入1-10倍硅源质量的丙酮破乳,离心得到固体,加入5-50 倍硅源质量的乙醇回流5〜30min,离心,重复2〜5次洗涤,分散在乙醇中,得二氧化硅乙醇分散液,二氧化硅质量浓度为1〜20wt% ;基体先用洗涤剂超声清洗,再反复用水,丙酮清洗2〜6次,将二氧化硅乙醇分散液在基体表面上沉积,20〜200C下保持1〜48h,得到超疏水表面。 The quality of the silicon source added 1-10 times the demulsification of acetone, centrifuged to obtain a solid, the silicon source is added 5-50 times the mass of ethanol was refluxed for 5~30min, centrifugation, washing was repeated 2 ~ 5 times, dispersed in ethanol, to give silica ethanol dispersion, the silica concentration of 1~20wt%; first substrate to ultrasonic cleaning with detergent, and then repeatedly washed with water, acetone 2 ~ 6 times, ethanol dispersion of the silica surface of the substrate is deposited, 20~200 By keeping 1~48h C to obtain superhydrophobic surface.

[0020] 下面通过实施例对本发明提供的方法进行详述,但不以任何形式限制本发明。 [0020] described in detail by the following examples of the method of the present invention provides, but without limiting the invention in any way. [0021 ] 实施例1 二氧化硅A (Ph-SiO2)的制备 Preparation 1 Silica A (Ph-SiO2) of Example [0021]

[0022] 取8. Og Np-12、15. Og环己烷、3. Og正辛醇和5. Og IOwt %,得溶液A ; 1. Og正硅酸乙酯0. 5g苯基基三甲氧基硅烷为溶液C ;在搅拌下将溶液B加入溶液D中,老化他;然后, 加入8g丙酮,搅拌30min,离心得到固体; [0022] Take 8. Og Np-12,15 Og cyclohexane, 3 Og octanol and 5. Og IOwt%, to obtain solution A;.. 1. Og TEOS 0. 5g phenyl trimethoxybenzaldehyde silane in solution C; under stirring solution B was added to solution D, the aging him; Then, 8g of acetone was added and stirred for 30min, centrifuged to obtain a solid;

[0023] 向此固体中加入30g乙醇,加热搅拌lOmin,离心;重复此步骤5次,直至表面活性剂去除干净;所得固体分散在IOg乙醇中。 [0023] This solid was added to 30g of ethanol, heating and stirring lOmin, centrifuged; this procedure was repeated five times, until the surfactants were cleanly removed; IOg resulting solid was dispersed in ethanol. 如图1所示,可以看出有机修饰的二氧化硅纳米颗粒,粒径均勻,粒径在lOOnm,表面非常粗糙。 As shown in Figure 1, it can be seen organically modified silica nanoparticles, uniform particle size, particle diameter lOOnm, the surface is very rough.

[0024] 实施例2 二氧化硅BL的制备 Example 2 Preparation of silica-BL [0024] embodiment

[0025] 材料BL的制备方法同材料A,不同之处在于有机硅烷的种类和加入量上,具体采用的有机硅烷的种类和加入量见表1,所得到的材料列于表1。 Preparation [0025] Materials BL with material A, except that the kind and added amount of the organic silane, the kind and amount of the specific use of the organosilane shown in Table 1, the resulting material are shown in Table 1.

[0026] 表1材料BH制备中采用的有机硅烷的种类和加入量 [0026] The type and amount in Table 1 Materials used in the preparation of BH organosilane

Figure CN102453465AD00051

[0028] 实施例3 二氧化硅I (Me-SiO2)的制备 [0028] Example 3 Preparation of Silica I (Me-SiO2) of

[0029] 取2. Og十二烷基苯磺酸钠、10. Og正己烷、l.Og正丁醇和4. Og 15wt%氨水混合得微乳液A ;1. Og正硅酸甲酯和0. 5g甲基三甲氧基硅烷为溶液B。 [0029] Take 2. Og of sodium dodecylbenzenesulfonate, 10 Og hexane, l.Og n-butanol and 4. Og 15wt% aqueous ammonia was mixed microemulsion A;.. 1 Og is methyl silicate and 0 . 5g methyltrimethoxysilane as solution B. 在搅拌下将溶液B滴入溶液D中,老化15h ;然后加入IOg丙酮,搅拌30min,离心得到固体; Under stirring the solution B was added dropwise a solution of D in aging 15h; IOg acetone was then added, stirred for 30min, centrifuged to obtain a solid;

[0030] 向此固体中加入30g乙醇,加热搅拌lOmin,离心;重复此步骤4次,直至表面活性剂去除干净。 [0030] This solid was added to 30g of ethanol, heating and stirring lOmin, centrifuged; this procedure was repeated 4 times, until the surfactants were cleanly removed. 所得固体分散在IOg乙醇中。 The resulting solid was dispersed in IOg ethanol.

[0031 ] 实施例4 二氧化硅JR的制备[0032] 材料JR的制备方法同材料I,不同之处在于有机硅烷的种类和加入量,具体采用的有机硅烷和加入量种类见表2,所得到的材料列于表2。 Example 4 Preparation of Silica JR [0032] [0031] The preparation of materials of the same material JR I, except that the kind and added amount of the organic silane, organic silane and an amount of the specific types of use are shown in Table 2, the The resulting material is shown in Table 2.

[0033] 表2材料JR制备中采用的有机硅烷的种类和加入量 [0033] Table 2, the kind and amount of the material prepared using JR organosilane

Figure CN102453465AD00061

[0035] 实施例5 二氧化硅S (Do-SiO2)的制备 Preparation Example 5 Silica S (Do-SiO2) in the [0035] embodiment

[0036] 取5. Og十六烷基三甲基溴化胺、12. Og甲苯、2. Og正戊醇和4. 5g 5wt%氨水混合得微乳液液A ;1. Og正硅酸甲酯和0. Ig十二烷基三甲氧基硅烷为溶液B ;在搅拌下将溶液C滴入溶液A中,老化Mh ;然后,加入IOg丙酮,搅拌30min,离心得到固体; [0036] Take 5. Og cetyl trimethyl ammonium bromide, 12 Og toluene, 2 Og amyl alcohol 4. 5g 5wt% ammonia was mixed microemulsion liquid A;... 1 n-methyl silicate Og and 0. Ig dodecyl trimethoxy silane in solution B; C under stirring solution was added dropwise to solution A, aging Mh; then, added IOg acetone, stirred 30min, centrifuged to obtain a solid;

[0037] 向此固体中加入30g乙醇,加热搅拌lOmin,离心;重复此步骤3次,直至表面活性剂去除干净。 [0037] To this solid 30g ethanol, heating and stirring lOmin, centrifugal; Repeat this step three times until the surfactant to remove and clean. 所得固体分散在IOg乙醇中。 The resulting solid was dispersed in IOg ethanol.

[0038] 实施例6 二氧化硅UZ的制备 Example 6 Preparation of silica-UZ [0038] embodiment

[0039] 材料TZ的制备方法同材料S,不同之处在于有机硅烷的种类和加入量,具体采用的有机硅烷和加入量种类见表3,所得到的材料列于表3。 Preparation [0039] Materials with TZ material S, except that the kind and added amount of the organic silane, organic silane and an amount of specific species employed in Table 3, the resulting material are shown in Table 3.

[0040] 表3 二氧化硅TZ制备中采用的有机硅烷的种类和加入量 [0040] Table 3, the type and amount of silica used in the preparation of TZ organosilane

[0041] [0041]

Figure CN102453465AD00071

[0042] 实施例7超疏水表面的制备 Preparation Example 7 superhydrophobic surface [0042] Example

[0043] 玻璃片先用洗涤剂超声清洗,再反复用水清洗3次,丙酮清洗4次,干燥。 [0043] glass sheet first ultrasonic cleaning with detergent, and then repeatedly washed with water 3 times, washed four times with acetone, and dried. 将制备好的AZ 二氧化硅乙醇分散液在基体表面上进行沉积,150温度下,老化Mh。 The prepared AZ silica dispersion in ethanol were deposited in the surface of the substrate, at a temperature of 150 , aging Mh.

[0044] 如图2和3所示,可以看出,所制备的表面具有粗糙结构。 [0044] Figures 2 and 3, it can be seen, has a rough surface structure prepared. 此表面具有超疏水性质, 水滴接触角大于150,且具有很强的粘附性能,水滴在倒置的情况下不会掉下来。 This surface has a super-hydrophobic properties, water contact angle greater than 150 , and has a strong adhesion properties, in the case of inverted water droplets will not fall off.

[0045] 本发明提供的方法制备的超疏水材料可以粘附到不同的基体上,形成一个超疏水表面,具有超疏水高粘附性能,该方法操作简单,原料易得,成本低,在无损失液体转移,液体携带生物材料,微流控制体系,生物微量液体转移,分离材料和生物传感器等方面具有广泛的应用前景。 [0045] The method of superhydrophobic materials provided by the invention can be adhered to the preparation of different substrates, to form a superhydrophobic surface, the superhydrophobic having high adhesive properties, this method is simple, readily available raw materials, low cost, in the absence of loss of liquid transfer, liquid carrying biological materials, micro-flow control system, biological trace liquid transfer, aspects of the separation of materials and biological sensors with a wide range of applications.

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