CN108117833B - 二氧化钛/聚合物复合介电疏水材料及制备方法 - Google Patents
二氧化钛/聚合物复合介电疏水材料及制备方法 Download PDFInfo
- Publication number
- CN108117833B CN108117833B CN201711452890.XA CN201711452890A CN108117833B CN 108117833 B CN108117833 B CN 108117833B CN 201711452890 A CN201711452890 A CN 201711452890A CN 108117833 B CN108117833 B CN 108117833B
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- hydrophobic material
- nano thread
- dielectric
- dioxide nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000000463 material Substances 0.000 title claims abstract description 37
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 34
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 229920000642 polymer Polymers 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 13
- 229920005573 silicon-containing polymer Polymers 0.000 claims abstract description 13
- 238000012856 packing Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000004528 spin coating Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- 239000011521 glass Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910003705 H2Ti3O7 Inorganic materials 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- -1 Radical siloxane Chemical class 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 239000002070 nanowire Substances 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 239000011256 inorganic filler Substances 0.000 abstract description 2
- 229910003475 inorganic filler Inorganic materials 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 230000010287 polarization Effects 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Polymers C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
- C03C2217/445—Organic continuous phases
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/465—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase having a specific shape
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
- C03C2217/475—Inorganic materials
- C03C2217/477—Titanium oxide
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Wood Science & Technology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
本发明涉及纳米复合材料技术,旨在提供一种二氧化钛/聚合物复合介电疏水材料及制备方法。该介电疏水材料是以聚二甲基硅氧烷为聚合物基体,以二氧化钛纳米线为填充材料,通过共混和旋涂工艺制得;所述填充材料占介电疏水材料总质量的5~30wt%。本发明通过水热法制备得到的二氧化钛纳米线,其直径在100纳米左右,长度在8微米左右。将本发明的二氧化钛纳米线用于溶液共混‑旋涂工艺,能够制备得到二氧化钛均匀分散的复合薄膜。高长径比的二氧化钛纳米线可增加无机填料/聚合物界面相互作用区域,实现界面极化效应增强,提高复合材料的介电常数,保持较低的介电损耗和优良的表面疏水性能。本发明制备工艺简单,方法的可操作性和可重复性高。
Description
技术领域
本发明涉及一种二氧化钛/聚合物复合介电疏水材料及制备方法,属于纳米复合材料技术领域。
背景技术
电润湿作为一种新型的利用电压来调控导电液滴的致动技术,调控范围广、响应灵敏且可以重复利用等,在各类微流控芯片、显示元器件以及可变焦液体透镜中具有广泛应用。介电润湿器件一般由4个部分组成——基底、电极、介电层、导电液滴。其中介电层对所需施加的驱动电压以及制作工艺都有着很大的影响,它可以大幅消除电解现象的发生,同时增加电压对导电液滴的调控范围,极大地促进了电润湿在各个领域的应用。通常,电润湿器件驱动电压与介电层的介电常数成反比关系。因此,制备具有较好疏水性能和高介电常数的介电层对提高电润湿性能有着十分重要的意义。然而,目前大多数疏水聚合物材料的介电常数较低,导致驱动电压高,影响介电润湿器件的稳定性。
聚二甲基硅氧烷(Polydimethylsiloxane,PDMS)是一种热固性橡胶,具有优良疏水性、透光性、弹性和可塑性,并且玻璃化转化温度低、成膜工艺简单,通过简单旋涂可制得厚度为微米级的薄膜。但纯PDMS材料的介电常数较低(小于3),限制了其在介电润湿器件、微流控芯片等领域的应用。
发明内容
本发明要解决的问题是,克服现有技术中的不足,提供一种二氧化钛/聚合物复合介电疏水材料及制备方法。
为解决技术问题,本发明所采用的技术方案是:
提供一种二氧化钛/聚合物复合介电疏水材料,该介电疏水材料是以聚二甲基硅氧烷为聚合物基体,以二氧化钛纳米线为填充材料,通过共混和旋涂工艺制得;所述填充材料占介电疏水材料总质量的5~30wt%。
本发明中,所述填充材料通过下述方法制备获得:
(1)将2.5克二氧化钛、12.5毫升无水乙醇、12.5毫升无水乙二醇、100毫升浓度为10摩尔/升的氢氧化钠溶液置于200毫升水热反应釜中,搅拌10分钟后,超声处理10分钟,再搅拌10分钟;然后将反应釜移至鼓风干燥箱中,在180℃条件下恒温反应48小时;
(2)反应结束后取出沉淀物,用37wt%的浓盐酸浸泡6小时;将浸泡后的沉淀物用去离子水洗涤多次后,移至60℃烘箱干燥,得到前驱体H2Ti3O7;
(3)将前驱体H2Ti3O7在空气中灼烧2小时,灼烧温度为600℃,最终获得用作填充材料的二氧化钛纳米线。
本发明还提供了前述二氧化钛/聚合物复合介电疏水材料的制备方法,包括以下步骤:
(1)按质量比1∶4将聚二甲基硅氧烷溶于环己烷中,磁力搅拌0.5小时;然后加入二氧化钛纳米线,超声分散0.5小时;再按聚二甲基硅氧烷与固化剂的质量比为1:10加入Sygard 184固化剂,在50℃水浴锅中搅拌0.5小时后改为室温下搅拌5小时,得到混合均匀的悬浊液;
(2)将悬浊液抽真空1小时以除去气泡后,旋涂于洗净的ITO玻璃上;移至烘箱中在120℃恒温2小时,得到固化的二氧化钛纳米线/聚二甲基硅氧烷复合介电疏水材料。
本发明中,先对ITO玻璃进行清洗:将ITO玻璃放置于烧杯中,用丙酮超声清洗5分钟,再用无水乙醇超声清洗5分钟,移入鼓风烘箱中烘干。
与现有技术相比,本发明的有益效果在于:
1、本发明通过水热法制备得到的二氧化钛纳米线,其直径在100纳米左右,长度在8微米左右。将本发明的二氧化钛纳米线用于溶液共混-旋涂工艺,能够制备得到二氧化钛均匀分散的复合薄膜。高长径比的二氧化钛纳米线可增加无机填料/聚合物界面相互作用区域,实现界面极化效应增强,提高复合材料的介电常数,保持较低的介电损耗和优良的表面疏水性能。
2、本发明制备工艺简单,方法的可操作性和可重复性高。通过调节二氧化钛纳米线的添加含量,能实现复合材料的介电、疏水等性能调控,同时其玻璃化转变温度非常低,可应用于电润湿显示、微流控芯片等器件的制造,具有广阔的发展应用前景。
附图说明
图1为二氧化钛纳米线的电镜照片。
图2为二氧化钛纳米线图谱和二氧化钛纳米线/聚二甲基硅氧烷的XRD图。
具体实施方式
下面结合实施例和对比例对本发明作进一步描述,实施例可以使本专业的专业技术人员更全面地理解本发明,但不以任何方式限制本发明。
实施例1-6
(1)将2.5克二氧化钛,12.5毫升无水乙醇,12.5毫升无水乙二醇,100毫升浓度为10摩尔/升氢氧化钠置于200毫升水热反应釜中,搅拌10分钟,超声处理10分钟,再搅拌10分钟。然后将反应釜放入鼓风干燥箱中在180℃条件下恒温反应48小时;
(2)反应结束后,取出沉淀物,用37wt%的浓盐酸浸泡6小时,将浸泡后的沉淀物用去离子水洗涤多次,移至60℃烘箱干燥,得到前驱体H2Ti3O7;
(3)将前驱体H2Ti3O7在空气中灼烧2小时,灼烧温度为600℃,升温速率5℃/min,获得白色的较为蓬松的二氧化钛粉末(其微观结构为线状,如图1)。
(4)按质量比1∶4将聚二甲基硅氧烷溶于环己烷中,磁力搅拌0.5小时;然后将二氧化钛纳米线填充材料分散在溶液中,超声处理0.5小时;再加入Sygard 184固化剂(聚二甲基硅氧烷与固化剂的质量比为1:10);在50℃水浴锅中搅拌0.5小时,之后在室温下搅拌5小时,得到混合均匀的悬浊液;
(5)将所述悬浊液在真空环境下抽真空1小时以除去气泡,之后将悬浊液旋涂于洗净的ITO玻璃的导电面上,在鼓风烘箱中120℃恒温2小时,得到固化的二氧化钛纳米线/聚二甲基硅氧烷复合介电疏水材料;
(6)通过真空镀膜机在复合膜表面镀上厚度为50nm,直径为1mm纯金作为电极,进行后续电学性能测试。
在步骤(4)中,控制填充材料的添加量,使其占成型后介电疏水材料总质量的5~30wt%;
在步骤(5)中,ITO玻璃应先进行清洗,具体方法如下:先将ITO玻璃放置于烧杯中用丙酮超声清洗5分钟,之后再用无水乙醇超声清洗5分钟,移入鼓风烘箱中烘干即可。
对比例(实施例7)
(1)按质量比1∶4将聚二甲基硅氧烷溶于环己烷中,磁力搅拌0.5小时;再加入Sygard 184固化剂(聚二甲基硅氧烷与固化剂的质量比为1:10);在50℃水浴锅中搅拌0.5小时,之后在室温下搅拌5小时,得到混合均匀的澄清液;
(5)将澄清液在真空环境下抽真空1小时以除去气泡,之后将澄清液旋涂于洗净的ITO玻璃的导电面上,在鼓风烘箱中120℃恒温2小时,得到固化的聚二甲基硅氧烷介电疏水材料;
(6)通过真空镀膜机在复合膜表面镀上厚度为50nm,直径为1mm纯金作为电极,进行后续电学性能测试。
实施效果验证
图1为本发明制备的TiO2的SEM图,可看出制备出的TiO2呈线状,尺寸均一,直径约为100nm,长度在8微米左右。图2为二氧化钛纳米线图谱和二氧化钛纳米线/聚二甲基硅氧烷的XRD图,从图中可以看出制备的TiO2晶型为锐钛矿(PDF#21-1272)。表1给出了实施例制备得到的复合薄膜的测试性能。从表中可以看出,复合薄膜的介电常数在无机物填充量为20wt%时达到最大,为7.01(100Hz),保持较低的介质损耗(100Hz,介电损耗0.059)。同时,在该填充量下样品接触角达到116.10。相对于纯聚二甲基硅氧烷材料的介电性能(100Hz介电常数=2.33,介电损耗0.141),本发明制备获得的介电疏水材料介电常数显著提高,介电损耗较低,满足电润湿显示器件应用的要求。
表1
需要说明的是,上述实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
Claims (3)
1.一种二氧化钛/聚合物复合介电疏水材料,其特征在于,该介电疏水材料是以聚二甲基硅氧烷为聚合物基体,以二氧化钛纳米线为填充材料,通过共混和旋涂工艺制得;所述填充材料占介电疏水材料总质量的5~30 wt%;
所述填充材料通过下述方法制备获得:
(1)将2.5克二氧化钛、12.5毫升无水乙醇、12.5毫升无水乙二醇、100毫升浓度为10摩尔/升的氢氧化钠溶液置于200毫升水热反应釜中,搅拌10分钟后,超声处理10分钟,再搅拌10分钟;然后将反应釜移至鼓风干燥箱中,在180℃条件下恒温反应48小时;
(2)反应结束后取出沉淀物,用37wt%的浓盐酸浸泡6小时;将浸泡后的沉淀物用去离子水洗涤多次后,移至60℃烘箱干燥,得到前驱体H2Ti3O7;
(3)将前驱体H2Ti3O7在空气中灼烧2小时,灼烧温度为600℃,最终获得用作填充材料的二氧化钛纳米线。
2.权利要求1所述二氧化钛/聚合物复合介电疏水材料的制备方法,其特征在于,包括以下步骤:
(1)按质量比1∶4将聚二甲基硅氧烷溶于环己烷中,磁力搅拌0.5小时;然后加入二氧化钛纳米线,超声分散0.5小时;再按聚二甲基硅氧烷与固化剂的质量比为1:10加入Sygard184固化剂,在50℃水浴锅中搅拌0.5小时后改为室温下搅拌5小时,得到混合均匀的悬浊液;
(2)将悬浊液抽真空1小时以除去气泡后,旋涂于洗净的ITO玻璃上;移至烘箱中在120℃恒温2小时,得到固化的二氧化钛纳米线/聚二甲基硅氧烷复合介电疏水材料。
3.根据权利要求2所述的方法,其特征在于,先对ITO玻璃进行清洗:将ITO玻璃放置于烧杯中,用丙酮超声清洗5分钟,再用无水乙醇超声清洗5分钟,移入鼓风烘箱中烘干。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711452890.XA CN108117833B (zh) | 2017-12-28 | 2017-12-28 | 二氧化钛/聚合物复合介电疏水材料及制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711452890.XA CN108117833B (zh) | 2017-12-28 | 2017-12-28 | 二氧化钛/聚合物复合介电疏水材料及制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108117833A CN108117833A (zh) | 2018-06-05 |
CN108117833B true CN108117833B (zh) | 2019-08-23 |
Family
ID=62232004
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201711452890.XA Active CN108117833B (zh) | 2017-12-28 | 2017-12-28 | 二氧化钛/聚合物复合介电疏水材料及制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108117833B (zh) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110563347B (zh) * | 2019-10-11 | 2022-04-19 | 湖北大学 | 一种基于花状二氧化钛纳米颗粒的耐高温液体和沸水的超滑涂层制备方法 |
CN113372589A (zh) * | 2021-04-28 | 2021-09-10 | 王登鑫 | 一种含有纳米粒子的pdms薄膜的制备方法 |
CN114773959B (zh) * | 2022-05-31 | 2023-03-03 | 复旦大学 | 一种高性能透明防腐涂层材料及其制备方法 |
CN117979673A (zh) * | 2024-03-29 | 2024-05-03 | 西北工业大学 | 一种防腐透明电磁屏蔽薄膜及其制备方法和应用 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103318956B (zh) * | 2013-07-11 | 2015-09-23 | 苏州大学 | 一种制备二氧化钛纳米线的方法 |
CN104479437B (zh) * | 2015-01-06 | 2017-01-25 | 东华大学 | 一种超疏水自发光涂层的制备方法 |
CN105540654B (zh) * | 2015-12-10 | 2017-09-29 | 西安电子科技大学 | 一种多层次TiO2纳米结构阵列材料的制备方法 |
-
2017
- 2017-12-28 CN CN201711452890.XA patent/CN108117833B/zh active Active
Also Published As
Publication number | Publication date |
---|---|
CN108117833A (zh) | 2018-06-05 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108117833B (zh) | 二氧化钛/聚合物复合介电疏水材料及制备方法 | |
Hooshyari et al. | Nanocomposite proton exchange membranes based on Nafion containing Fe2TiO5 nanoparticles in water and alcohol environments for PEMFC | |
JP6565923B2 (ja) | 表面修飾金属酸化物粒子分散液及びその製造方法、表面修飾金属酸化物粒子−シリコーン樹脂複合組成物、表面修飾金属酸化物粒子−シリコーン樹脂複合体、光学部材、及び発光装置 | |
WO2015060289A1 (ja) | 蛍光体組成物、蛍光体シート、蛍光体シート積層体ならびにそれらを用いたledチップ、ledパッケージおよびその製造方法 | |
JP5463099B2 (ja) | 中空シリカ粉末、その製造方法及び用途 | |
CN104098860A (zh) | 聚偏氟乙烯/聚多巴胺包覆石墨烯纳米复合材料的制备方法 | |
CN104558664B (zh) | 利用氧化石墨烯和纳米二氧化硅制备强亲水pet膜的方法 | |
CN103820945A (zh) | 一种有机无机杂化纳米超疏水纤维膜的制备方法 | |
Guo et al. | Effect of silicone coupling agent on dielectric properties of barium titanate/silicone elastomer composites | |
JP2015048297A (ja) | 表面修飾メソポーラスシリカナノ粒子の製造方法 | |
WO2021000551A1 (zh) | 一种接枝改性氧化铝及其制备方法、环氧复合材料及其应用 | |
CN103570251B (zh) | 一种绝缘超疏水涂层的制备方法 | |
CN109694537A (zh) | 含有量子点的储能复合薄膜材料及制备方法 | |
CN105355320A (zh) | 一种纳米级导电钛白粉的生产工艺 | |
CN103633270A (zh) | 无机/有机穿插型复合质子交换膜及其制备方法 | |
KR20210146334A (ko) | 분산액, 조성물, 밀봉 부재, 발광 장치, 조명 기구, 표시 장치 및 분산액의 제조 방법 | |
CN110903653B (zh) | 硅橡胶组合物、硅橡胶及其制备方法 | |
CN108641039B (zh) | 一种包覆型核壳结构复合颗粒及其制备方法和应用 | |
CN103979962B (zh) | 一种锆钛酸钡钙无铅梯度厚膜的制备方法 | |
CN107611252B (zh) | 一种ZnO/BaTiO3复合材料制备方法、ZnO/BaTiO3复合材料及应用 | |
CN116082847B (zh) | 一种用于超疏水改性的硅橡胶微球及其制备方法 | |
CN111087899A (zh) | 一种介电润湿复合材料的制备方法 | |
JP2015059161A (ja) | フィラー分散有機樹脂複合体 | |
CN114854061B (zh) | 一种施主掺杂二氧化硅/聚酰亚胺基复合薄膜的制备方法及应用 | |
WO2019073012A1 (en) | COMPOSITION COMPRISING SILVER NANOWIRES AND AT LEAST ONE FLUORINATED POLYMER |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |