CN104064287A - 一种同轴两层CNTs/TiO2纳米电缆结构的制备方法 - Google Patents
一种同轴两层CNTs/TiO2纳米电缆结构的制备方法 Download PDFInfo
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Abstract
本发明公开了一种同轴两层CNTs/TiO2纳米电缆结构的制备方法，属于纳米材料制备领域。本发明利用孔道垂直于表面且上下通孔的多孔阳极氧化铝膜作为模板制备同轴两层CNTs/TiO2纳米电缆结构，制备过程为：以乙炔和氩气为气氛，采用化学气相沉积法在模板孔道中均匀沉积一层碳纳米管；然后在超声振荡条件下将沉积过碳纳米管的阳极氧化铝模板浸入一定温度的异丙醇钛溶液中，均匀沉积一层二氧化钛前驱体；将样品取出进行清洗、烘干后，在200-600℃温度下保温1-6h后制备出同轴两层CNTs/TiO2纳米电缆结构。本发明制备的纳米复合材料，可重复性强，便于规模生产，并且具有较好的催化效率。应用于10mg/L甲基橙溶液的光催化反应，3-5h之后处理效率达到60%-90%。
Description
技术领域：
本发明涉及一种同轴两层CNTs/TiO2纳米电缆结构的制备方法。更具体的说，利用多孔阳极氧化铝膜为模板依次在阳极氧化铝模板孔道中沉积碳纳米管和二氧化钛纳米管制备同轴两层纳米电缆结构的方法，属于纳米材料制备领域。
背景技术：
TiO2以其无毒、稳定性好、催化活性高、氧化能力强、易得等特点而被大家广泛关注，成为了最为理想的光催化材料之一。但由于其光生电子与空穴复合率高，吸收光谱范围限于紫外光，粉末状TiO2难回收等种种不足限制了其实际应用。而碳纳米管除了拥有大比表面积、高化学稳定性、较好吸附能力等传统碳材料的诸多性能外，还因其特有的内在结构(一维管腔、长径比等)而表现出独特的金属或半导体导电性。将TiO2与碳纳米管复合可实现两种材料在特点及优点上的相互协同(利用CNTs提供的大比表面积和电荷传输能力)显著改善TiO2的光催化性能。
TiO2与碳纳米管在复合结构的构型上主要有简单混合、表面分散、同轴型等。制备方法主要有：(1)混合法，直接将碳纳米管与TiO2混合后使用，碳纳米管与TiO2的界面接触为随机接触，存在组分不易分散均匀，易团聚，不利于协同作用的发挥等缺点。(2)化学气相沉积法，采用两步化学气相沉积法制备TiO2/CNTs异质结阵列，第一步以Ti片为基底，二茂铁为催化剂，二甲苯为碳源首先合成碳纳米管阵列，第二步采用化学气相沉积方法在碳纳米管阵列上沉积TiO2，优点是沉积速率高，可形成连续均匀的膜，膜厚易于控制，TiO2与碳纳米管结合强度高，缺点是工艺复杂，技术难度大。(3)静电纺丝法，如将聚丙烯腈(PAN)/CNTs/TiO2复合体系电纺，得到含TiO2及CNTs的复合纤维，该法工艺相对简单，但制备过程参数可控性较差，需后续高温处理以实现TiO2的晶型转换。(4)水热/溶剂热法，将CNTs及异丙醇钛在乙醇溶液中分散后，于反应釜中加热，通过控制异丙醇钛与CNTs的混合比，可得到不同形貌及TiO2含量的TiO2/CNTs。该法析晶及晶型转化一步完成，不需后续高温处理，但形成的产物比表面积相对较小，TiO2多为颗粒而非膜状负载，反应过程需严格控制水热温度、反应时间和压强等。(5)溶胶-凝胶法，溶胶-凝胶工艺具有组分材料定量准确、方便的优点，但存在CNTs在TiO2前驱体的溶剂体系中分散差，表面分布不均和后续焙烧处理过程中的表面团聚等缺点。
阳极氧化铝膜具有均匀分布的垂直于表面且相互平行的纳米孔道，且其孔径、孔间距、膜厚可以通过工艺手段加以控制，在纳米材料的合成中广泛应用。本发明以多孔阳极氧化铝膜为模板，采用层层组装技术，制备同轴两层CNTs/TiO2纳米电缆结构。该法工艺简单，条件温和，制备样品结构有序度高。
发明内容：
本发明的目的是提供一种利用模板合成同轴两层CNTs/TiO2纳米电缆结构的制备方法，提高二氧化钛光催化效率，以克服现有技术上的不足。利用阳极氧化铝模板制备一种同轴两层CNTs/TiO2纳米电缆结构的制备方法，其具体步骤为：
(1)首先选用孔道垂直于表面且上下通孔的多孔氧化铝膜作为模板，其中多孔氧化铝膜为上下通孔，孔径为100-250nm，膜厚度为20-60μm；
(2)在沿孔道方向始终通入氩气的前提下，将马弗炉升温到400～800℃温度，然后以乙炔和氩气为气氛，氩气的流速为20～100sccm,乙炔的流速为总流速的10%～60%。采用化学气相沉积法在模板孔道中均匀沉积一层碳纳米管，沉积时间为5min～60min,随炉冷却至室温，得到含有阳极氧化铝模板在内的碳纳米管阵列；
(3)在超声振荡条件下将沉积过碳纳米管的阳极氧化铝模板放入到30℃～80℃的异丙醇钛溶液中，质量分数大于等于97%，保持振荡时间2min～20min；
(4)将从异丙醇钛溶液中取出的含有碳纳米管和二氧化钛前驱体的阳极氧化铝模板在200～600℃进行热处理保温1～6h，然后随炉冷却至室温，制备完成，得到同轴两层CNTs/TiO2纳米电缆结构。
本发明的有益效果是：
(1)本实验采用层层组装技术制备同轴两层CNTs/TiO2纳米电缆结构。设备简单，操作容易，可以大量制备；
(2)制备的两层CNTs/TiO2纳米电缆结构以多孔阳极氧化铝模板为载体，解决纳米催化剂的负载问题，可循环使用，且属于环境友好型高性能材料。与粉末状(纳米管、纳米颗粒)催化剂的无规则分散状态相比，催化剂以阵列形式存在，易于从处理污水中回收，避免造成二次污染；
(3)二氧化钛均匀的分布在碳纳米管的管壁上，在紫外灯照射300min之后，CNTs/TiO2复合纳米材料催化降解有机污染物如甲基橙效率达到85%～90%，相比于纯TiO2与碳纳米管的40%～45%与10%～15%，催化性能有很大程度的提高。优异的光催化性能及简单的制备工艺，使得同轴两层CNTs/TiO2纳米电缆结构在污水处理领域有广泛的应用前景。
附图说明：
图1为同轴两层CNTs/TiO2纳米电缆结构的SEM图片。
图2为同轴两层CNTs/TiO2纳米电缆结构的EDS图片。
图3为单根同轴两层CNTs/TiO2纳米电缆结构的TEM图片。
图4为(a)AAO模板，(b)碳纳米管，(c)TiO2纳米管，和(d)同轴两层CNTs/TiO2纳米电缆结构对甲基橙光催化降解的影响。
具体实施方式：
实施实例1：
(1)选用孔径约为200nm,厚50μm的多孔阳极氧化铝膜作为模板。
(2)将模板放在管式马弗炉中沿模板孔道方向通入氩气(40sccm),待马弗炉加热到650℃。然后通入乙炔和氩气的混合气氛(20%的乙炔和80%的氩气)，流速为50sccm,保持14min。随后随炉冷却至室温，整个过程一直通入氩气，且氩气的流速不变。
(3)将异丙醇钛溶液，质量分数为97%，室温搅拌30min，然后缓慢升温至55℃。然后将沉积过碳的阳极氧化铝模板浸入异丙醇钛溶液中超声振荡处理9min。
(4)将从异丙醇钛溶液中取出的含有碳纳米管和二氧化钛前驱体的阳极氧化铝模板在225℃进行热处理保温2h，然后随炉冷却至室温，制备完成，得到同轴两层CNTs/TiO2纳米电缆结构。同轴两层CNTs/TiO2纳米电缆结构的复合管直径为200nm左右，管壁厚约为40nm,碳纳米管和二氧化钛纳米管厚度分别为20nm和20nm左右。相关样品的扫描电镜图片(SEM)见图1，EDS图片见图2，透射电镜图片(TEM)见图3。
实施实例2：
用甲基橙溶液的降解速率来测定产品的催化性能。
(1)在一个石英反应器中加入10mL甲基橙溶液，甲基橙溶液的浓度为10mg/L，并用H2SO4调节pH至3待用。
(2)将一块直径为13mm的含有多孔阳极氧化铝模板的同轴两层CNTs/TiO2纳米电缆结构产品放入溶液中，实验开始之前，先将装有试样和甲基橙溶液的石英反应器置于黑暗环境中2h，使甲基橙在催化剂的表面达到吸附/脱附平衡。
(3)在光化学反应仪中，选用功率为300W、主波长为254nm的Hg灯照射，进行光催化降解，每隔30min取样，光催化反应300min。
(4)在分光光度计以水为参照在波长为506nm处测定其吸光度，进而计算光催化降解效率。由图4可知，在紫外灯照射300min之后，CNTs/TiO2复合纳米材料催化降解有机污染物如甲基橙效率达到85%～90%，相比于纯TiO2纳米管与碳纳米管的40%～45%与10%～15%，催化性能有很大程度的提高。
以上实例对本发明进行了详细的阐述，本领域内的技术人员应该理解，在不超出本发明的精神和实质的范围内，对本发明做出一定的修改或变形，比如采用不同厚度和孔径的阳极氧化铝模板或采用不同的气相沉积温度、时间和溶液浸渍温度、时间等不同工艺参数，仍能实现本发明所述之结果，然而不脱离本发明的保护范围。
Claims (2)
1.一种同轴两层CNTs/TiO2纳米电缆结构的制备方法，其特征在于，以多孔阳极氧化铝膜作为模板，其中多孔氧化铝膜为上下通孔，孔径为100-250nm，膜厚度为20-60μm。
2.一种如权利要求1所述的同轴两层CNTs/TiO2纳米电缆结构的制备方法，其特征在于：包括以下步骤：
(1)首先选用孔道垂直于表面且上下通孔的多孔氧化铝膜作为模板；
(2)在沿孔道方向始终通入氩气的前提下，将马弗炉升温到400～800℃温度，然后以乙炔和氩气为气氛，氩气的流速为20～100sccm,乙炔的流速为总流速的10%～60%；采用化学气相沉积法在模板孔道中均匀沉积一层碳纳米管，沉积时间为5min～60min,随炉冷却至室温，得到含有阳极氧化铝模板在内的碳纳米管阵列；
(3)在超声振荡条件下将沉积过碳纳米管的阳极氧化铝模板放入到30℃～80℃的异丙醇钛溶液中，质量分数大于等于97%，保持振荡时间2min～20min；
(4)将从异丙醇钛溶液中取出的含有碳纳米管和二氧化钛前驱体的阳极氧化铝模板在200～600℃进行热处理保温1～6h，然后随炉冷却至室温，制备完成，得到同轴两层CNTs/TiO2纳米电缆结构。
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| CN106928613B (zh) * | 2017-04-12 | 2019-03-26 | 中国科学院化学研究所 | 多组分电缆型纳米纤维阵列及其制备方法 |
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