CN113755229A - 一种C3N4/TiO2纳米复合颗粒电流变液及其制备方法 - Google Patents
一种C3N4/TiO2纳米复合颗粒电流变液及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种C3N4/TiO2纳米复合颗粒电流变液及其制备方法,该电流变液的分散相是C3N4/TiO2纳米复合颗粒,采用两步法制备而成;所得C3N4具备疏松多孔的二维材料特征,负载TiO2纳米颗粒后形成一种C3N4/TiO2纳米复合颗粒;该材料与甲基硅油所配成的电流变液具有一些优异的特性,包括极强的电流变效应、很好的抗沉淀稳定性、电流密度低、化学稳定性好。附图中显示了C3N4/TiO2纳米复合颗粒电流变液在不同电场强度下其剪切应力与剪切速率的关系。
Description
技术领域
本发明涉及一种电流变液及其制备方法,具体涉及一种C3N4/TiO2纳米复合颗粒电流变液及其制备方法。
背景技术
智能材料在人们的科学研究和社会发展中的作用越来越重要,他们可以受各种外加条件激发而做出相应的响应,并且这种响应往往是特殊且罕见的。例如:压力、温度、电场磁场、pH值等。电流变液(ERF)作为一种新颖的智能材料近年来收到越来越广泛的关注,其特点是在外加电场条件下,分散于绝缘介质(硅油、矿物油等)中的具有高极化能力的分散颗粒发生一系列粘度和流变性质变化,并且这一过程往往是可逆的,且响应速度极快(一般情况下是几个毫秒)。电场对分散体系所产生的内部架构以及流变性质产生变化的效应被叫做电流变效应。因此电流变液通常由两部分组成;分散相和绝缘介质,其电流变性质主要取决于前者。
电流变液是一种对电场快速响应的智能材料,通常是由高介电常数的微小颗粒分散在低介电常数的绝缘液体中形成的悬浮体系。这类材料在外加电场的作用下,在两平行电极之间,构造成链状或柱状结构,因此材料的流变性能包括剪切应力,弹性模量,剪切粘度等都会发生从液体到类固体的转变,其粘度和剪切强度会快速提高,具有快速可逆的特点。电流变材料因为能耗低,受控变化的品质使其在减振、机械传动、自控、机电一体化、微驱动等领域具有巨大的应用前景。
分散相材料是指电流变液的固体颗粒,一般分为四种:有机高分子材料;无机材料;复合材料;液体材料。但任一材料通常应满足以下特点:(1)合适的电导率以及较大的介电常数;(2)工作温度范围宽泛且物理化学性质稳定;(3)适当的形貌以及密度。其中有机高分子材料主要分为两类:一类是拥有大Π键的材料,由于大Π键电子云的共轭作用,这类材料在电场的作用下拥有很强的极化能力,且介电常数较大;另一类是含有极性官能团的材料,极性基团超大的极化率导致此类材料在电场作用下往往也具有较大的极化能力。石墨相氮化碳材料 (g-C3N4)作为一种新型共轭二维聚合物,近年来在功能材料领域有着广泛的应用。无机材料主要是指金属氧化物,其中纳米TiO2被认为是一种极具潜力的电流变分散相材料,它拥有着高的介电常数,且制备方法简便多样,原料无毒环保的特点,在电流变材料中占着很大的比重。众所周知,分散相纳米粒子的微观结构与表面形貌对其电流变性质有着重要影响,TiO2粒子之间的紧密程度和相互作用对界面极化有着很大影响。复合材料一般是由导电层和绝缘层组成,核心导电层颗粒保证颗粒的快速极化,因此往往也成为了实验设计与改造的核心部分。外层的绝缘层主要用于保护导电层颗粒,降低其电导率,保护极化电荷不团聚,维持粒子之间稳定的静电作用。因此拥有特殊结构的复合材料往往能大幅提升原有两者的电流变性能。液体材料主要指液晶聚合物,此类材料最大特点是不存在固体材料常有的聚沉问题,但其本征粘度往往较大,且常出现分层现象。
本发明的目的是提供一种g-C3N4/TiO2纳米复合颗粒电流变液,其分散相是 g-C3N4/TiO2纳米复合颗粒,连续相为二甲基硅油。g-C3N4/TiO2纳米复合颗粒具有独特的形貌,扫描电镜和透射电镜结果表明g-C3N4/TiO2纳米复合颗粒为多孔复合结构,TiO2纳米颗粒在g-C3N4层间沉积,分布均匀且粒径细小。制备工艺为改性的溶胶-凝胶法,没有添加任何表面活性剂,属于无模板法,绿色环保。以该材料与甲基硅油所配成的电流变液,由于空心结构颗粒的抗沉降性,赋予该电流变液优异的悬浮稳定性,解决了电流变的一大难题。该工艺还可以通过控制反应时间和比例来调控产物的形貌,尺寸,孔状程度等,可调性强。
本发明的目的还在于提供一种两步法制备g-C3N4/TiO2纳米颗粒的方法,属于改进的两步复合制备法,C3N4/TiO2纳米复合颗粒通过两步法制备而得,先采用煅烧法制得疏松多孔二维材料C3N4,然后以C3N4为模板,再通过溶胶-凝胶法制得C3N4/TiO2纳米复合颗粒;C3N4/TiO2纳米复合颗粒具备独特的形貌,极强的电流变效应,良好的温度效应,适中的电流密度。制备工艺简单,原料易得,以该材料与甲基硅油所配成的电流变液具有一些优异的特性,包括极强的电流变效应、很好的抗沉淀稳定性、电流密度低、化学稳定性好。
本发明的目的可以通过以下技术方案来实现:
本发明所制备电流变液,其分散相是g-C3N4/TiO2纳米颗粒,连续相为二甲基硅油。
上述电流变液的制备工艺包括以下步骤:
(1)在60mL无水乙醇、30mL异丙醇和1.5mL去离子水的混合溶液中加入1.5mL钛酸四丁酯后搅拌30min,然后用无水乙醇洗涤离心得到TiO2纳米颗粒,放入烘箱70℃干燥12h得到固体粉末;将2g双氰胺于马弗炉中550℃煅烧4h,升温速率2.3℃/min,自然冷却至室温收集,然后用去离子水和无水乙醇离心洗涤各3次,于烘箱中70℃干燥6h,得到淡黄色氮化碳粉末。
(2)将0.5g氮化碳粉末分散于50ml无水乙醇中,搅拌30min至均匀乳黄色,然后加入0.1gTiO2纳米颗粒,超声分散2h,加热至70℃蒸干收集,得到C3N4/TiO2纳米复合颗粒。
(3)将该样品与二甲基硅油按固体颗粒与硅油的重量比10wt%配制成电流变液。
附图说明
图1g-C3N4模板的SEM照片
图2g-C3N4/TiO2纳米颗粒SEM照片
图3g-C3N4/TiO2纳米颗粒TEM照片
图4g-C3N4/TiO2纳米颗粒XRD曲线
图5g-C3N4/TiO2纳米颗粒FTIR图谱
图6g-C3N4/TiO2纳米颗粒BET曲线
图7g-C3N4/TiO2纳米颗粒电流变性能图
图8TiO2纳米颗粒SEM照片
图9g-C3N4/TiO2纳米颗粒SEM照片(15mL异丙醇)
图10g-C3N4/TiO2纳米颗粒SEM照片(20mL异丙醇)
具体实施方式
实施例一:(g-C3N4的制备)
g-C3N4通过煅烧法制备而得,具体操作过程如下所述:将2g双氰胺与6g 氯化钠溶解于50mL去离子水中,充分搅拌至均匀。然后于液氮中快速冷冻至固态,置于冷冻干燥机中干燥24h以获得白色细小粉末。将白色粉末于马弗炉中550℃煅烧4h,升温速率2.3℃/min,自然冷却至室温收集,然后用去离子水和无水乙醇离心洗涤各3次,于烘箱中70℃干燥6h,得到淡黄色氮化碳粉末。图1是g-C3N4模板的SEM照片,由图可以看出,g-C3N4模板成纳米片层结构,层厚在5-7nm左右,壁面平滑,层间空隙适中,孔径大小均一。
实施例二:
在60mL无水乙醇、30mL异丙醇和1mL去离子水混合溶液中加入1.5mL 钛酸四丁酯,将溶液搅拌30min后用无水乙醇洗涤离心三次后得到纳米TiO2颗粒,放入烘箱中烘干得到固体粉末;将2g双氰胺与6g氯化钠溶解于50ml去离子水中,充分搅拌至均匀。然后于液氮中快速冷冻至固态,置于冷冻干燥机中干燥24h以获得白色细小粉末。将白色粉末于马弗炉中550℃煅烧4h,升温速率2.3℃/min,自然冷却至室温收集,然后用去离子水和无水乙醇离心洗涤各3 次,于烘箱中70℃干燥6h,得到淡黄色氮化碳粉末;将0.5g氮化碳粉末分散于50ml无水乙醇中,搅拌30min至均匀乳黄色,然后加入0.1gTiO2纳米颗粒,超声分散2h,加热至70℃蒸干收集,得到C3N4/TiO2纳米复合颗粒。将该样品与二甲基硅油按固体颗粒与硅油的重量比10wt%配制成电流变液。
图2和图3分别是g-C3N4/TiO2纳米颗粒的SEM和TEM照片,从图中可以看出复合颗粒的形貌呈纳米片状,TiO2纳米颗粒均匀分布在层间。图4是 g-C3N4/TiO2纳米颗粒的XRD图谱,原始TiO2的XRD谱与锐钛矿TiO2(JCPDS 21-1272)的XRD谱相匹配分别,通过与标准锐钛矿型氧化钛卡片PDF#21-1272 对比可知25.37°对应的晶面指数为(101),37.03°对应的晶面指数为(103),48.12 °对应的晶面指数为(200),55.10°所对应的晶面指数为(211),62.74°对应的晶面指数为(204),表明氧化钛晶型是锐钛矿型,并且峰形尖锐,结晶性良好。根据先前的研究,g-C3N4分别在2θ=12.8°和27.4°处揭示两个特征信息峰,分别对应其(100)和(002)两个晶面指数。复合纳米颗粒的图谱保留了两者的特征峰,证实了两者的共存且晶体结构没有发生改变。图5是g-C3N4/TiO2纳米颗粒的FTIR图,400-1000cm-1对应的是O-Ti-O键的伸缩振动峰,1200-1700cm-1范围对应氮化碳内部N-(C)3或者C-NH-C键的伸缩振动,3000-3500cm-1范围对应其-NH2或=NH基团的振动,复合物的FTIR图谱都包含了两者的特征振动峰,证实了两者的共存以及化学基础结构并没有发生大的变化。图6是g-C3N4/TiO2纳米颗粒的的BET曲线图,从BET曲线可以看出,g-C3N4/TiO2纳米颗粒的平均孔径分布在10.6nm左右,且根据t-plot法计算出其表面积达到了61.7g/m2,其氮气吸附脱附曲线满足Ⅳ型吸附脱附曲线特征,这是典型介孔材料的特点,并且其孔容大小大约在0.2cm3/g左右。图7是g-C3N4/TiO2纳米颗粒基电流变液在不同场强下剪切强度与剪切速率的关系。由图可知,电压加到了3kV,并且其电流密度较小,说明该体系的电流变液的抗击穿性能较好。从图中可以看到,在不加电场的情况下,剪切应力随着剪切速率增加而线性增加,流体呈现牛顿流体行为;加电场后,颗粒在电场中迅速发生极化,偶极之间相互吸引,颗粒排列成链状结构,在电场强度的提高下,剪切应力不断上升,并且在高频区域呈现出平台区,其特征为宾汉流体,电流变效率为345,体现出极强的电流变效应。图8为纳米二氧化钛的SEM照片,可以看出其粒径控制在纳米范围内,大小均一,分布均匀,无明显团聚现象。
实施例三:
在60mL无水乙醇、15mL异丙醇和1mL去离子水混合溶液中加入1.5mL 钛酸四丁酯,将溶液搅拌30min后用无水乙醇洗涤离心三次后得到纳米TiO2颗粒,放入烘箱中烘干得到固体粉末;将2g双氰胺于马弗炉中550℃煅烧4h,升温速率2.3℃/min,自然冷却至室温收集,然后用去离子水和无水乙醇离心洗涤各3次,于烘箱中70℃干燥6h,得到淡黄色氮化碳粉末;将0.5g氮化碳粉末分散于50ml无水乙醇中,搅拌30min至均匀乳黄色,然后加入0.1gTiO2纳米颗粒,超声分散2h,加热至70℃蒸干收集,得到C3N4/TiO2纳米复合颗粒。将该样品与二甲基硅油按固体颗粒与硅油的重量比10wt%配制成电流变液。图9 是g-C3N4/TiO2纳米颗粒SEM照片(15mL异丙醇),相比于30mL异丙醇体系,模板的孔隙结构发生的一定程度的坍塌,考虑是生成了无定形的TiO2使得孔隙发生堵塞所导致。
实施例四:
在60mL无水乙醇、20mL异丙醇和1mL去离子水混合溶液中加入1.5mL 钛酸四丁酯,将溶液搅拌30min后用无水乙醇洗涤离心三次后得到纳米TiO2颗粒,放入烘箱中烘干得到固体粉末;将2g双氰胺于马弗炉中550℃煅烧4h,升温速率2.3℃/min,自然冷却至室温收集,然后用去离子水和无水乙醇离心洗涤各3次,于烘箱中70℃干燥6h,得到淡黄色氮化碳粉末;将0.5g氮化碳粉末分散于50ml无水乙醇中,搅拌30min至均匀乳黄色,然后加入0.1gTiO2纳米颗粒,超声分散2h,加热至70℃蒸干收集,得到C3N4/TiO2纳米复合颗粒。将该样品与二甲基硅油按固体颗粒与硅油的重量比10wt%配制成电流变液。图10 是g-C3N4/TiO2纳米颗粒SEM照片(20mL异丙醇),相比于30mL异丙醇体系,模板发生了坍塌与团聚,使得孔隙结构大幅减少,考虑是不足量的异丙醇使得 TiO2的纳米成核不均匀导致。
Claims (2)
1.一种电流变液,其特征在于该电流变液分散相是C3N4/TiO2纳米复合颗粒,连续相为二甲基硅油;C3N4/TiO2纳米复合颗粒通过两步法制备而得,先采用煅烧法制得疏松多孔二维材料C3N4;然后以C3N4为模板,再通过溶胶-凝胶法制得C3N4/TiO2纳米复合颗粒;C3N4/TiO2纳米复合颗粒具备独特的形貌,极强的电流变效应,良好的温度效应,适中的电流密度。
2.如权利要求1所述的一种电流变液,其特征在于制备工艺包括以下步骤:
(1)将2g双氰胺与6g氯化钠溶解于50mL去离子水中,充分搅拌至均匀;然后于液氮中快速冷冻至固态,置于冷冻干燥机中干燥24h以获得白色细小粉末;将白色粉末于马弗炉中550℃煅烧4h,升温速率2.3℃/min,自然冷却至室温收集,然后用去离子水和无水乙醇离心洗涤各3次,于烘箱中70℃干燥6h,充分碾磨得到淡黄色氮化碳粉末;
(2)在60mL无水乙醇和30mL异丙醇混合溶液中加入1.5mL钛酸四丁酯后搅拌30min,然后用无水乙醇洗涤离心得到TiO2纳米颗粒,放入烘箱70℃干燥12h得到固体粉末;
(3)将0.5g氮化碳粉末分散于50ml无水乙醇中,搅拌30min至均匀乳黄色,然后加入0.1gTiO2纳米颗粒,超声分散2h,加热至70℃蒸干收集,得到C3N4/TiO2纳米复合颗粒;
(4)将该样品与二甲基硅油按固体颗粒与硅油的重量比10wt%配制成电流变液。
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