CN109647366A - 一种溶胶-凝胶法制备光电催化氧化钛电极的方法 - Google Patents
一种溶胶-凝胶法制备光电催化氧化钛电极的方法 Download PDFInfo
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Abstract
本发明公开了一种溶胶‑凝胶法制备光电催化氧化钛电极的方法，该溶胶‑凝胶法制备光电催化氧化钛电极的方法所制得的氧化钛电极的晶粒尺寸均匀、细小，晶化程度很高，膜层质量好，膜层厚度均匀，且能适合大面积的涂膜；整体工艺方法简单，所需设备少，效率高。
Description
技术领域
本发明涉及氧化钛薄膜电极工艺的技术领域，尤其涉及一种溶胶-凝胶法制备光电催化氧化钛电极的方法。
背景技术
溶胶通常是指固体分散在液体中形成的胶体溶液。凝胶是在溶胶聚沉过程中的特定条件下，形成的一种介于固态和液态间的冻状物质，是由胶粒组成的三维空间网状结构，网络了全部或者部分介质，是一种相当稠厚的物质。溶胶-凝胶(Sol-gel)法是制备负载膜的一种重要方法。其基本原理是：将金属醇盐或无机盐经水解直接形成溶胶或经解凝形成稳定的溶胶，然后采用浸渍涂层、旋转涂层或者喷涂法把溶胶溶液涂覆在基材上，使其自然干燥成为凝聚膜，凝胶膜经过一定温度烧结生成具有一定孔径分布和性能的无机膜。
溶胶-凝胶法包括以下几个过程：(1)溶胶的制备。有两种方法制备溶胶:一是先将部分或全部组分用适当沉淀剂先沉淀出来经解凝，使原来团聚的沉淀颗粒分散成原始颗粒。因这种原始颗粒的大小一般在溶胶体系中胶核的大小范围，因而可制得溶胶。另一种方法是从同样的盐溶液出发，通过对沉淀过程的仔细控制，使首先形成的颗粒不致团聚为大颗粒而沉淀，从而直接得到胶体溶胶。(2)溶胶-凝胶转化:溶胶中含大量的水，凝胶化过程中，使体系失去流动性，形成一种网状的骨架结构。实现胶凝作用的途径有两个:一是化学法，通过控制溶胶中的电解质浓度:二是物理法，迫使胶粒间相互靠近，克服斥力，实现胶凝化。(3)凝胶干燥:在一定条件下(如加热)使溶剂蒸发。干燥过程中凝胶结构变化很大。
溶胶-凝胶工艺具有如下优点：(1)可以通过简单廉价的设备和简单的工艺在大的、形貌复杂的衬底表面形成涂层；(2)可以获得高度均匀的多组分氧化物涂层和特定的组份不均匀涂层；(3)热处理过程所需的温度低；(4)可制备其他方法可能不适合的特殊材料，如有机-无机复合涂层等；(5)化学计量比准确，可大范围内调节成份；(6)可以获狭窄粒径分布、纳米级粒子尺寸的涂层；(7)很容易引入微量元素，掺杂改性；(8)可通过多种方法改变薄膜的表面结构和性能。
但是也存在着一些缺点，如无机膜膜层质量比较差，存在开裂和褶皱现象。目前，大多数商业具有光催化性质的氧化钛薄膜一般是采用溶胶-凝胶法制备的。
而现有技术的溶胶-凝胶制得的氧化钛薄膜通常是以金属有机醇盐为原料，通过水解与缩聚反应而制得溶胶，并进一步缩聚而得到凝胶。水解反应与缩聚反应谁能占主导地位取决于水解和缩聚反应速率的相对大小及水解反应进行的程度。该水解反应是一个放热反应，且反应温度升高，将会使颗粒粒径增大，因此反应温度不宜过高。现有的方法虽然有其它方法不可相比的优点，而且具有良好的光催化活性，但是它缺乏机械耐久力，还有大面积镀膜时，很难保证薄膜厚度的均一性，且限制了大面积基片镀膜的产生。
发明内容
本发明的目的是为了克服上述现有技术的缺点，提供一种溶胶-凝胶法制备光电催化氧化钛电极的方法，该溶胶-凝胶法制备光电催化氧化钛电极的方法所制得的氧化钛电极的晶粒尺寸均匀、细小，晶化程度很高，膜层质量好，膜层厚度均匀，且能适合大面积的涂膜；整体工艺方法简单，所需设备少，效率高。
本发明解决其技术问题所采用的技术方案是：一种溶胶-凝胶法制备光电催化氧化钛电极的方法，包括如下步骤：
(1)将钛网钛网切割成7.5cm×2.8cm，用砂纸打磨后再用去污粉清洗表面，用蒸馏水漂洗并烘干，将钛网依次放入丙酮中作超声波清洗20min和放入无水乙醇中超声清洗20min，再一次用蒸馏水清洗，将清洗好的钛网吹干备用；
(2)将Ti(OBu)4和冰醋酸溶于乙醇溶剂中，均匀混合搅拌配制成A溶液；将蒸馏水、盐酸溶于乙醇溶剂中配制成B溶液；
(3)将B溶液滴入或倒入A溶液中，置于40-60℃水浴中充分搅拌，形成性能稳定的透明溶胶，然后透明溶胶在室温下静置陈化24h后，得到TiO2溶胶；
(4)将处理好的钛网缓慢垂直浸入TiO2溶胶中1h，然后以2mm/s的速率均匀稳定地将钛网提出液面，钛网表面挂上一薄层厚度均匀的湿凝胶膜，然后立即放入80℃的恒温干燥箱中干燥10mins，取出自然冷却；
(5)重复步骤(4)数次，形成对钛网涂膜数次，然后送入马福炉锻烧，升温至500℃恒温退火2h，升温速率保持2℃/min，最后马福炉中自然冷却至室温，得到氧化钛电极。
进一步的，所述的步骤(5)中重复步骤(4)的次数为5次。涂膜次数为5次时，薄膜的催化性能达到最高。
进一步的，所制得的氧化钛电极的晶粒为15nm。
因钛醇盐极易与水反应，可在瞬间生成沉淀。为此，采用冰醋酸为鳌合剂以缓解钛醇盐的剧烈水解，抑制沉淀的生成。盐酸在钛酸四丁酯的水解缩聚反应过程中起到催化反应和稳定溶胶的作用。溶胶是由于静电的相互作用而形成的，向水解缩聚体系中加入胶溶剂时，H+吸附在水解缩聚产物的表面，反应离子在液相中重新分布从而在粒子表面形成双电层，双电层的存在使粒子间产生相互排斥作用。当排斥力大于粒子间的吸引力时，聚集的粒子分散成小粒子形成溶胶。
综上所述，本发明的溶胶-凝胶法制备光电催化氧化钛电极的方法所制得的氧化钛电极的晶粒尺寸均匀、细小，晶化程度很高，膜层质量好，膜层厚度均匀，且能适合大面积的涂膜；整体工艺方法简单，所需设备少，效率高。
附图说明
图1为溶胶-凝胶法在500℃退火温度制备TiO2薄膜的XRD图谱。
具体实施方式
实施例1
本实施例1所描述的一种溶胶-凝胶法制备光电催化氧化钛电极的方法，包括如下步骤：
(1)将钛网钛网切割成7.5cm×2.8cm，用砂纸打磨后再用去污粉清洗表面，用蒸馏水漂洗并烘干，将钛网依次放入丙酮中作超声波清洗20min和放入无水乙醇中超声清洗20min，再一次用蒸馏水清洗，将清洗好的钛网吹干备用；
(2)将Ti(OBu)4和冰醋酸溶于乙醇溶剂中，均匀混合搅拌配制成A溶液；将蒸馏水、盐酸溶于乙醇溶剂中配制成B溶液；
(3)将B溶液滴入或倒入A溶液中，置于40-60℃水浴中充分搅拌，形成性能稳定的透明溶胶，然后透明溶胶在室温下静置陈化24h后，得到TiO2溶胶；
(4)将处理好的钛网缓慢垂直浸入TiO2溶胶中1h，然后以2mm/s的速率均匀稳定地将钛网提出液面，钛网表面挂上一薄层厚度均匀的湿凝胶膜，然后立即放入80℃的恒温干燥箱中干燥10mins，取出自然冷却；
(5)重复步骤(4)5次，形成对钛网涂膜5次，因为涂膜次数为5次时，薄膜的催化性能达到最高。然后送入马福炉锻烧，升温至500℃恒温退火2h，升温速率保持2℃/min，最后马福炉中自然冷却至室温，得到氧化钛电极。
在本实施例中，所制得的氧化钛电极的晶粒为15nm。
因钛醇盐极易与水反应，可在瞬间生成沉淀。为此，采用冰醋酸为鳌合剂以缓解钛醇盐的剧烈水解，抑制沉淀的生成。盐酸在钛酸四丁酯的水解缩聚反应过程中起到催化反应和稳定溶胶的作用。溶胶是由于静电的相互作用而形成的，向水解缩聚体系中加入胶溶剂时，H+吸附在水解缩聚产物的表面，反应离子在液相中重新分布从而在粒子表面形成双电层，双电层的存在使粒子间产生相互排斥作用。当排斥力大于粒子间的吸引力时，聚集的粒子分散成小粒子形成溶胶。
如图1所示，可以发现出它与标准的锐钛矿相的衍射图谱完全一致，在2θ为25.3°、39°、48°、53.8°、55°、63°、75°等位置，均有清晰而且尖锐的衍射峰，且衍射峰比较宽，而这些衍射角处的峰正好是锐钛矿型TiO2的特征衍射峰。说明溶胶-凝胶法制备的经过500℃恒温退火后的TiO2薄膜晶面结构为锐钛矿结构，而且晶粒尺寸比较细小。
氧化钛电极薄膜的平均粒径d可由最强衍射峰(101)面的半高宽,运用Scherrer公式d＝kλ/(βcosθ)求得平均晶粒尺寸约为15nm。
以上所述，仅是本发明的较佳实施例而已，并非对本发明的技术方案作任何形式上的限制。凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明的技术方案的范围内。
Claims (3)
1.一种溶胶-凝胶法制备光电催化氧化钛电极的方法，其特征在于，包括如下步骤：
(1)将钛网钛网切割成7.5cm×2.8cm，用砂纸打磨后再用去污粉清洗表面，用蒸馏水漂洗并烘干，将钛网依次放入丙酮中作超声波清洗20min和放入无水乙醇中超声清洗20min，再一次用蒸馏水清洗，将清洗好的钛网吹干备用；
(2)将Ti(OBu)4和冰醋酸溶于乙醇溶剂中，均匀混合搅拌配制成A溶液；将蒸馏水、盐酸溶于乙醇溶剂中配制成B溶液；
(3)将B溶液滴入或倒入A溶液中，置于40-60℃水浴中充分搅拌，形成性能稳定的透明溶胶，然后透明溶胶在室温下静置陈化24h后，得到TiO2溶胶；
(4)将处理好的钛网缓慢垂直浸入TiO2溶胶中1h，然后以2mm/s的速率均匀稳定地将钛网提出液面，钛网表面挂上一薄层厚度均匀的湿凝胶膜，然后立即放入80℃的恒温干燥箱中干燥10mins，取出自然冷却；
(5)重复步骤(4)数次，形成对钛网涂膜数次，然后送入马福炉锻烧，升温至500℃恒温退火2h，升温速率保持2℃/min，最后马福炉中自然冷却至室温，得到氧化钛电极。
2.根据权利要求1所述的一种溶胶-凝胶法制备光电催化氧化钛电极的方法，其特征在于，所述的步骤(5)中重复步骤(4)的次数为5次。
3.根据权利要求2所述的一种溶胶-凝胶法制备光电催化氧化钛电极的方法，其特征在于，所制得的氧化钛电极的晶粒为15nm。
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