CN108033688B - 一种氧化硅基超疏水涂层及其制备方法 - Google Patents
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Abstract
本发明涉及一种氧化硅基超疏水涂层及其制备方法，包括基体，其特征在于基体上涂覆球形石英粉A、乙醇制成的底膜层、球形石英粉、四乙氧基硅烷、乙醇、稀盐酸制成的中间膜层、氟硅烷溶液喷涂制成的表面膜层。a.球形石英粉A分散于乙醇中，形成悬浮液；b.清洗玻璃片，放入浓硫酸和双氧水混合液中浸泡、干燥得玻璃基片；c.玻璃基片浸入悬浮液，取出干燥得石英粉底膜层；d.将四乙氧基硅烷、乙醇混合搅拌，加入稀盐酸制得二氧化硅溶胶；e.二氧化硅溶胶中加入球形石英粉B，混合制得混合液；f.石英粉底膜层上涂覆混合液，干燥、烧结得中间膜层；g.在中间膜层表面喷涂氟硅烷溶液，固化即可。本发明优点，一种氧化硅基超疏水涂层坚固耐用，化学稳定性好，可用于陶瓷、玻璃等材料表面，发挥防污染、防指纹、防氧化、疏水等特性。
Description
技术领域
本发明属疏水涂层技术领域，涉及一种氧化硅基超疏水涂层，还涉及一种氧化硅基超疏水涂层制备方法。
背景技术
超疏水表面的水接触角大于150°，且具有较低的滚动角（小于10°）。实现超疏水的方法有：垂直阵列纳米管和纳米纤维，溶胶-凝胶法（sol-gel），相分离法，层层自组装（LBL），掠射角沉积等。在这些技术中，溶胶-凝胶法（sol-gel）在沉积超疏水涂层的技术中较其他方法简单高效，同时，它的显著优点在于可大面积涂膜，被沉积物体表面形状不限，涂膜时间短。影响固体表面润湿性的两个主要因素分别为表面化学成分（表面自由能）和表面形貌（粗糙度）。超疏水是特定粗糙结构和低表面能物质综合作用结果。为了实现超疏水，可以首先获得粗糙表面，然后低表面能化，或者同时实现低表面能的粗糙结构。
由于超疏水表面的粗糙结构减少了固液接触面积，同时也使得表面与污染物的接触面积较少，减弱了两者之间的作用力；当液滴滚动时，超疏水表面的污染物很容易被带走，这种独特的自清洁性质使其在工农业生产、国防建设和日常生活中具有广阔应用前景。
发明内容
本发明的目的生产一种具有自清洁性质的涂层，提供一种氧化硅基超疏水涂层及其制备方法。
为了实现上述目的，本发明采用的技术方案如下：
一种氧化硅基超疏水涂层，包括基体，其特征在于基体上依次涂覆由球形石英粉A、乙醇制成的底膜层，由球形石英粉B、四乙氧基硅烷、乙醇、稀盐酸制成的中间膜层，由氟硅烷溶液喷涂制成的表面膜层；其中，底膜层原料为：质量浓度为8%~13%的粒度0.8μm~4μm球形石英粉A的无水乙醇混合液，中间膜层原料配比为：按质量份数计，粒度0.1μm~0.8μm球形石英粉B 2~4、四乙氧基硅烷15~20、无水乙醇28~33、稀盐酸10~14。
一种氧化硅基超疏水涂层制备方法，其特征在于包括以下步骤：
a. 按质量份数比称取上述原料，将粒度0.8μm~4μm（优选2μm~4μm）的球形石英粉A分散于无水乙醇中，控制石英粉A的无水乙醇混合液的质量浓度为8%~13%，充分搅拌、超声振荡，形成均匀的悬浮液；
b.用无水乙醇和去离子水依次超声波清洗玻璃片，然后放入由浓度为98%的浓硫酸和浓度为30%的双氧水按体积比3:1组成的混合液，80℃条件下浸泡1h，干燥后得活化、新鲜的玻璃基片；
c.将步骤b得到的玻璃基片浸入步骤a得到的悬浮液，静置20s取出，在干燥箱中，100℃干燥15~30min，然后置于580℃~600℃马弗炉中使玻璃表面软化，最底层的石英粉由于重力作用嵌入玻璃表面并粘合在一起，保温30min，取出用去离子水冲洗干净，玻璃上得一层石英粉底膜层；
d.按质量份数比称取四乙氧基硅烷15~20份，无水乙醇28~33份混合进行水解，磁力搅拌1h，随后加入0.1mol/L的10~14份的稀盐酸进行缩合反应4h制得二氧化硅溶胶；
e. 向二氧化硅溶胶中加入粒度为0.1μm~0.8μm（优选0.1μm~0.4μm）的球形石英粉B，控制超声波功率300W，频率40KHz，振荡分散30min，得二氧化硅溶胶和石英粉B的混合液；
f.在步骤c得到的石英粉底膜层上涂覆步骤e制备的混合液，120℃干燥30min~60min，350℃~420℃烧结20min~30min，得到超疏水膜的中间膜层；
g.使用喷枪在步骤f得到的中间膜层表面喷涂氟硅烷溶液，在100℃~150℃固化60min~120min后即得一种氧化硅基超疏水涂层。
进一步，一种氧化硅基超疏水涂层制备方法，所述氟硅烷溶液制备方法为：向50mL去离子水中加入49 mL乙二醇纯溶剂中，再缓慢加入1 mL十七氟癸基三甲氧基硅烷，磁力搅拌均匀，添加草酸控制pH值在3.0左右，搅拌1h，静置5h十七氟癸基三甲氧基硅烷充分水解得。
为使表面实现一定的粗糙度和具有较低的表面能，本发明所述涂层由球形石英粉底层、氧化硅溶胶中间层和氟硅烷表层三层组成。
本发明有益效果，一种氧化硅基超疏水涂层坚固耐用，化学稳定性好；可应用于陶瓷、玻璃等材料表面，发挥防污染、防指纹、防氧化、疏水等优良性质。
具体实施方式
一种氧化硅基超疏水涂层及其制备方法，具体实施步骤如下：
实施例1
(1)将10g粒径为2μm~4μm的球形石英粉A分散于100 mL无水乙醇中，充分搅拌后放入超声波清洗机，水浴加热至50℃，超声波功率300W，频率40KHz，振荡时间30min，形成均匀的悬浮液；
(2)用无水乙醇和去离子水依次超声波清洗76mm*25mm*1mm玻璃片15min，然后放入由浓度98%浓硫酸和浓度30%双氧水体积比3:1组成的混合液，80℃条件下浸泡1h后，干燥得活化、新鲜的玻璃基片；
(3)将步骤(2)得到的玻璃基片水平浸入步骤(1)所得悬浮液，静置20s，水平取出并在干燥箱中100℃条件下干燥10min，然后置于580℃马弗炉中保温30min，将样品取出，用去离子水冲洗干净，去除多余的未牢固结合的石英粉，在玻璃表面形成一层单颗粒层的石英粉底膜层；
(4)将41.8 mL无水乙醇与20mL的四乙氧基硅烷混合，室温下磁力搅拌1h，然后滴入0.1mol/L盐酸溶液13 mL，搅拌4h，得无色透明二氧化硅溶胶；
(5)向二氧化硅溶胶中加入2.98g粒径为0.1μm~0.4μm的球形石英粉B，在超声波功率300W，频率40KHz，振荡分散30min，将步骤（3）制成的石英粉底膜层采用浸渍提拉法制备凝胶膜，提拉速率130mm/min，浸渍时间40s，得中间膜层；
(6)在50mL去离子水中加入49mL乙二醇纯溶剂中，再缓慢加入1 mL十七氟癸基三甲氧基硅烷，磁力搅拌均匀，添加草酸控制pH值在3.0左右，搅拌1h氟硅烷分散均匀，静置5h氟硅烷充分水解得氟硅烷溶液，将配制的氟硅烷溶液装入压缩空气喷涂镀膜设备的涂料储罐，涂料喷嘴口径0.8mm，涂料空气压力0.29MPa，空气流量270L/min，涂料喷出量150mL/min，喷嘴距离中间膜层表面20cm，均匀喷涂5s后形成顶层氟硅烷膜层，室温沥去多余氟硅烷溶液，置于烘箱中，120℃干燥1.5h得到一种氧化硅基超疏水涂层。
Claims (2)
1.一种氧化硅基超疏水涂层制备方法，其特征在于包括以下步骤：
a. 按质量份数比称取原料，将粒度0.8μm~4μm的球形石英粉A分散于无水乙醇中，控制石英粉A在分散剂无水乙醇中的质量浓度为8%~13%，充分搅拌、超声振荡，形成均匀的悬浮液；
b.用无水乙醇和去离子水依次超声波清洗玻璃片，然后放入由浓度为98%的浓硫酸和浓度为30%的双氧水按体积比3:1组成的混合液，80℃条件下浸泡1h，干燥后得活化、新鲜的玻璃基片；
c.将步骤b得到的玻璃基片浸入步骤a得到的悬浮液中，静置20s取出，在干燥箱中，100℃干燥15~30min，然后置于580℃~600℃马弗炉中保温30min，取出用去离子水冲洗干净，玻璃上得一层石英粉底膜层；
d.按质量份数比称取四乙氧基硅烷15~20份，无水乙醇28~33份混合进行水解，磁力搅拌1h，随后加入0.1mol/L的10~14份的稀盐酸进行缩合反应4h制得二氧化硅溶胶；
e.向二氧化硅溶胶中加入2-4份粒度为0.1μm~0.8μm的球形石英粉B，控制超声波功率300W，频率40KHz，振荡分散30min，得二氧化硅溶胶和石英粉B的混合液；
f.在步骤c得到的石英粉底层膜上涂覆步骤e制备的混合液，120℃干燥30min~60min，350℃~420℃烧结20min~30min，得到超疏水膜的中间膜层；
g.使用喷枪在步骤f得到的中间膜层表面喷涂氟硅烷溶液，在100℃~150℃固化60 min~120min后即得一种氧化硅基超疏水涂层。
2.根据权利要求1所述一种氧化硅基超疏水涂层制备方法，其特征在于氟硅烷溶液制备方法为：向50 mL去离子水中加入49 mL乙二醇纯溶剂中，再缓慢加入1 mL十七氟癸基三甲氧基硅烷，磁力搅拌均匀，添加草酸控制pH值在3.0左右，搅拌1h，静置5h十七氟癸基三甲氧基硅烷充分水解得。
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