CN108117833B - 二氧化钛/聚合物复合介电疏水材料及制备方法 - Google Patents
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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。
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