Name: functionalization and dispersion of carbon nanomaterials using an environmentally friendly ultrasonicated ozonolysis process
Uploaded: 2017-05-30T12:30:00.000+00:00
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Description: Watch this Scientific Journal Video about Functionalization and Dispersion of Carbon Nanomaterials Using an Environmentally Friendly Ultrasonicated Ozonolysis Process at JoVE.com

这项工作的非薪酬部分由澳大利亚联邦资助。特拉华大学的作者非常感谢美国国家科学基金会（拨款＃1254540，项目总监Mary Toney博士）的支持。作者感谢Mark Fitzgerald先生对电泳沉积测量的帮助。

通过超声波臭氧分解对CNTs和GNP的功能化<ol><li>在装有HEPA过滤器的通风柜内的手套箱中称量纳米材料。将所需数量的纳米材料称重到烧杯中。转移到瓶子中，加入超纯水使浓度达到1g / L。 </li><li>用盖子密封瓶子。超声波在标准超声波浴中（参见材料列表;频率:〜43±2kHz;功率:60W）以分散CNT或GNP。 注意:小心。请参阅上述工作健康和安全通知。 </li><li>小心地将纳米材料悬浮液倒入装有磁力搅拌棒的反应炉中。安装一个反应瓶盖，并提供足够的孔口用于臭氧和超声波喇叭入口和出口。将其放在搅拌板上，通过调节表盘打开磁力搅拌器，以防止CNT沉淀出悬浮液。 </li><li>将超声波喇叭装入超声波电池并检查喇叭提示处于良好状态。参见图1 。 </li></ol><img alt="图1" src="/files/ftp_upload/55614/55614fig1.jpg" /> 图1:超声波臭氧分解系统。该示意图说明了如何连接超声波臭氧分解系统的各种元件。 <a href="http://ecsource.jove.com/files/ftp_upload/55614/55614fig1large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <ol start="5"><li>使用硅胶管连接反应器，超声波电池和蠕动泵。参见图1 。 </li><li>将臭氧起泡器插入反应器并将其连接到臭氧发生器。 注意:小心。请参阅上述工作健康和安全通知。 </li><li> 将循环液体冷却器单元连接到冷却盘管（以冷却反应器）和超声波电池冷却套管。翻转开关打开循环液体冷却液g单元以冷却臭氧反应堆和超声波电池。确保冷却液流经超声波电池和反应器冷却浴。 <ol><li>使用连接到超声波喇叭控制单元的热电偶来测量反应器温度。等待系统冷却至5°C。 </li></ol></li><li> 将反应器烧瓶放置在位置。将臭氧扩散器插入反应器烧瓶的底部，使其完全浸没。确保超声波电池的出口管被浸没在分散体表面以下至少25毫米处。 <ol><li>使用与蠕动泵送操作相同的硅胶管将出口管从反应器连接到臭氧破坏装置。在臭氧破坏装置的出口侧使用水鼓泡器是可选的，但它有助于捕获任何残留的臭氧，并提供臭氧发生器连接并正常工作的指示。 </li></ol></li><li>打开臭氧发生器的氧气供应，并调节阀门，通过臭氧发生器达到0.5升/分钟的流速。 </li><li>通过翻转开关打开臭氧发生器。在开始泵送或超声波处理之前让其运行30-60分钟。 </li><li> 打开蠕动泵，通过将泵转盘转到大约5或6的设置将其调节到0.67 Hz，并确保CNT分散体均匀地流过电池。 <ol><li>打开超声波喇叭，通过在手动操作菜单中将该值输入控制模块，将电源调整到60瓦。 </li><li>初始启动时，缓慢升高振幅设置，达到所需的功率输出为60W。 注意:超声波喇叭的工作频率为20 kHz。幅度设置和功率设置通常是相似的值，但是在初始启动时，幅度设置可能需要缓慢增加才能达到预期d功率输出为60W </li></ol></li><li>观察超音波处理至少30分钟，以确保泵送和超声波喇叭的稳定运行。 </li><li>监测与蠕动泵机构直接接触的柔性管道以进行磨损。至少每2小时调整管子位置，以确保管道保持完整性。更换每个单独的碳纳米材料处理运行的管道。 </li><li> 当所需的USO处理时间过去时，按开关关闭臭氧发生器，超声波发生器和泵。保持搅拌直到碳纳米材料分散液准备好转移到密封容器中，以供以后用于电泳沉积。 <ol><li>在转移分散体之前约等待1小时，以使溶液中的臭氧分解。 </li></ol></li><li>如果在USO处理的24小时内不进行电泳，则再次超声处理纳米材料分散体以使颗粒数量最小化摆脱分散。将声音喇叭插入碳纳米材料分散体瓶中，并在使用前超声波处理30分钟。 </li></ol> 2.电泳<ol><li> 准备3个不锈钢电极，60 mm（L）x 25 mm（W），0.2 mm片材。 <ol><li>用超纯水作为润滑剂的P1000氧化铝砂纸磨损电极。磨损后，将电极放在超声波清洗槽中，并在超纯水中清洗10分钟。 </li></ol></li><li>将用于阳极沉积的电极放置在100℃的干净的烘箱中，并干燥10分钟。将电极移动到干燥器并使其冷却。在四位数分析天平上称重电极。 </li><li>将电极的重量记录为小数点后四位，以克为单位的未涂覆重量。干燥剩余的两个电极并将其储存在干燥器中，用作de的阴极位置。 </li><li>使用合适的夹紧装置（参见图2 ），例如小型的10毫米非导电塑料隔离件，组装电极，外部电极用作阴极，内部电极用作阳极。 </li></ol><img alt="图2" src="/files/ftp_upload/55614/55614fig2.jpg" /> 图2:电泳沉积细胞。该示意图示出了电泳沉积池的结构。 <a href="http://ecsource.jove.com/files/ftp_upload/55614/55614fig2large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <ol start="5"><li>将35 mL碳纳米材料分散液转移到50 mL烧杯中。 </li><li>将不锈钢电极固定装置放置在蒸馏台上，并将电极缓慢下降至烧杯的全深度。将直流电源的正极端子连接到中央不锈钢德。将直流电源的负极连接到外部阴极。使用带鳄鱼夹的导线连接两个外阴极。 </li><li>如果需要精确的电流测量，请连接与电源单元和电极串联的万用表，以便在沉积期间进行监控。 </li><li>将直流电源上的电流设置手动调整为最大电流（标称为2A），然后将电压调整到所需的值，以确保电源输出关闭。准备一个秒表，并在所需的涂层持续时间内打开电源。 </li><li>对于典型的涂层实验，将电压调节至10 V，涂层时间范围为1至15分钟。关闭直流电源，然后缓慢地将电极从分散体中提起，确保胶片不受干扰。 </li><li> 断开端子与电极的连接，并慢慢地将电极反转到水平方向to允许阳极上的膜均匀干燥。水分在室温下从薄膜中蒸发掉后，拆下电极固定装置，将阳极置于烘箱中100℃烘干1小时。 <ol><li>夹住并将阳极悬挂在烤箱中，以确保胶片不会与任何表面直接接触。 </li></ol></li><li>将涂膜阳极放置在干燥器中，使其冷却，然后称重在四位数分析天平上。将重量记录到小数点后四位。减去未涂覆阳极的重量，以确定沉积膜的质量。 </li><li>照照涂层阳极。使用合适的图像处理包来精确测量沉积膜的面积。使用质量和面积记录薄膜的面密度，单位为mg / cm 2 。 </li><li>对每个沉积时间重复涂层和称重步骤，以确定碳纳米材料沉积到不锈钢上所需的速度针对所使用的特定场强。 </li></ol> 3.化学表征 - X射线光电子能谱（XPS） 15 <ol><li> 为了制备用于XPS分析的样品，将CNT分散体从原始1g / L分散液中滴出。 <ol><li>使用移液管，将一滴分散体沉积在不锈钢盘上，并允许在室温下干燥。重复该过程，直到在盘上观察到厚度约为2μm的均匀厚的CNT涂层。使用双面导电胶带将不锈钢磁盘安装到样品柱上。 </li></ol></li><li>将样品插入样品进样室，并将其送至5 x 10 -7 Torr的真空，然后将其转移到主分析室。在定位样品并进行分析之前，请等待主室压力达到5×10 -9乇。 </li><li> 至遵循XPS测量的典型工作条件，使用工作在150 W的单色Al Kα ，1 X射线源照射700μm×300μm的面积。相对于样品表面以90°起飞角检测光电子。 <ol><li>使用Au 4f 7/2光电子峰在83.98 eV的结合能量下校准光谱仪的能量刻度。 注意:在仪器的初始调试期间，仪表控制软件中的能量表被调整。在负责设备的光谱师进行任何维护操作后，经常检查，不应由用户更改。 </li></ol></li><li>通过在C 1s区域上定位30-eV窗口来监视初始采样电荷。通过系统调整电子喷枪参数来进行电荷补偿，以将C 1s峰值定位在284.6 eV，并将峰值宽度最小化为最大峰值强度的一半<html> （FWHM）。 </li><li> 在固定分析仪传输模式下以160 eV通过能量和0.5 eV步长进行测量扫描，停留时间为0.1 s，以识别表面元素物种。以0.05eV步长和0.2s的驻留采集20eV通过能量的区域光谱。使用4到8次扫描，以提高信噪比。 <ol><li>为了量化光谱，使用来自合适元素库16的Shirley背景拟合和灵敏度因子。 </li></ol></li><li> 解卷积C 1s高分辨率X射线光电子光谱，以确定USO处理时间15存在的不同碳氧物种。 <ol><li>为了准确地对C 1s峰进行解卷积，对石墨碳的形状进行初始峰值拟合，以确保由于sp 2结合引起的峰形状和来自低能π型振动卫星的贡献被保持&gt; 17。对于所有峰拟合，分别约束分量结合能和FWHM±0.1eV和±0.2eV，并使用30的高斯/洛伦兹比。 </li><li>使用六个单独的峰适应石墨峰形状。以固定比例保持相对于主要石墨峰的每个峰的面积为284.6eV，以保持由于处理的纳米材料15,9,14中的石墨成分而保持一致的形状。 </li></ol></li></ol> 4.结构表征 - 拉曼光谱18 <ol><li>通过用去离子水稀释原始分散体来制备拉曼光谱表征的纳米材料，以达到0.1g / L浓度。移取0.05 mL分散体到合适的抛光金底物上。允许液滴在室温下蒸发以产生在其上聚焦的薄碳膜我们拉曼激光点。 注意:当使用大的基材时，金基板的尺寸是结果的附带，多个样品可以沉积在单个载玻片上。 </li><li> 使用分散共聚焦显微镜和532 nm激光，用50倍放大的物镜进行拉曼测量。以2厘米-1的分辨率获得3,500和50厘米-1之间的光谱。使用50μm的针孔，激光能量在1到10 mW之间，使用尽可能最大的能量，使得在采集过程中不会发生样品退化。 <ol><li>通过累积10到50次扫描并使用2到5秒之间的曝光时间来进行每次扫描以获得合理的信噪比来收集光谱。 </li></ol></li></ol> 5.薄膜形态 - 扫描电子显微镜（SEM） <ol><li>对于功能化与未官能化的CNT / GNP的SEM分析，稀释每分散体用0.1g / L的去离子水。将其沉积在铝SEM短棒上，并使其在空气中干燥过夜。 </li><li>对于沉积在不锈钢电极上的EPD膜，将电极切割成1厘米×1厘米的正方形，并使用双面导电胶带将其安装到样品短截线上。在样品的顶部表面上涂上一小束银匕（ 即导电粘合剂/涂料），以改善导电路径。将样品在加热灯下干燥至少15分钟。 </li><li> 将安装的样品放在溅射涂布机中，并给出约1.3-1.5nm厚的导电铱涂层19 。 <ol><li>在厚度测量单元上，将材料密度设置为适当的水平，铱为22.56 g / cm 3 。调整目标厚度设置为1.0 nm，以便在考虑涂层p期间的热漂移时给出约1.3-1.5 nm的厚度rocess。 </li><li>设置涂布机单元以允许溅射涂布机操作由厚度测量单元控制。选择所需的功率输出，高分辨率涂层应为80 mA。 </li><li>将厚度控制单元上的涂层厚度计置零，然后按"循环"按钮开始自动化室抽真空，氩气渗/冲洗和涂布顺序。当功率已经达到所需的水平时，将目标屏蔽物移开以允许涂层开始。在涂层期间旋转和倾斜舞台，以便在所有方面均匀涂抹。 </li></ol></li><li>使用带有透镜检测器的场致发射SEM检查纳米材料。使用约3mm的工作距离和3.0kV的加速电压。 </li></ol>

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Electron Spectrosc. 128, 205-213 (2003).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> DXR Raman Instruments: Getting Started. , (2008).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Cressington 208HR High Resolution Sputter Coater for FE-SEM: Operating Manual. , (2003).</li><li>Krishnamoorthy, K., Veerapandian, M., Yun, K., Kim, S. -. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+chemical+and+structural+analysis+of+graphene+oxide+with+different+degrees+of+oxidation.">The chemical and structural analysis of graphene oxide with different degrees of oxidation.</a> Carbon. 53, 38-49 (2013).</li><li>Hamaker, H. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Formation+of+a+Deposit+by+Electrophoresis.">Formation of a Deposit by Electrophoresis.</a> T. Faraday Soc. 35, 279-287 (1940).</li><li>Rider, A. N., An, Q., Brack, N., Thostenson, E. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer+nanocomposite+-+fiber+model+interphases:+Influence+of+processing+and+interface+chemistry+on+mechanical+performance.">Polymer nanocomposite - fiber model interphases: Influence of processing and interface chemistry on mechanical performance.</a> Chem. Eng. J. 269, 121-134 (2015).</li></ol>

作者没有什么可以披露的。

When working with nanoparticles of high hardness, such as CNTs, the potential erosion effect on containers and tubing should not be overlooked. Step 1.14 in the protocol was inserted after the tubing became worn at a bend due to CNTs impinging on the tube side wall, causing a system leak.
Also, note that the CNTs are in suspension, not solution, and that they must be stirred before each use if a homogeneous suspension is desired. For example, this would be necessary to maintain the desired con...

使用碳纳米材料改性聚合物和复合体系已经在过去20年中引起了浓厚的研究兴趣。最近关于使用碳纳米管1 （CNTs）和石墨烯纳米片2 （GNP）的综述提供了广泛的研究。 CNT和GNP的高比刚度和强度以及它们的高固有电导率使得材料理想地适合于结合到聚合体系中以增强纳米复合材料的机械和电性能。 CNT和GNP也被用于通过使用碳纳米材料来改变纤维界面粘合力和基体刚度3,4等级来开发分级复合结构。 碳纳米材料均匀分散在聚合物体系中往往需要处理步骤，其化学改变纳米材料以改善与聚合物基质的化学相容性，去除杂质，并从所接收的材料中减少或去除附聚物。化学修饰碳纳米材料的各种方法是可用的，并且可以包括使用强酸5,6进行湿化学氧化，用表面活性剂改性7 ，电化学嵌入和剥离8或使用基于等离子体的方法的干法化学处理9 。 在CNT的氧化步骤中使用强酸引入氧官能团并除去杂质。然而，它具有显着降低CNT长度，对CNT外壁造成损害并使用危险化学品的缺点，这些危险化学品需要与经处理的材料隔离以进一步处理10 &lt;/ SUP&gt;。使用与超声波结合的表面活性剂提供了较不积极的制备稳定分散体的方法，但是表面活性剂通常难以从经处理的材料中除去，并且可能不与用于制备纳米复合材料材料1,11的聚合物相容。表面活性剂分子与CNT或GNP之间的化学相互作用的强度也可能不足以用于机械应用。在大气条件下进行的干等离子体处理工艺可能适用于存在于纤维或平面表面上的用于制备分层复合材料的CNT阵列的功能化。然而，大气等离子体更难应用于干燥粉末，并且不能解决存在于原始碳纳米材料中的附聚物的问题。 在目前的工作中，我们介绍了超声波的详细描述我们以前曾用于碳纳米材料12,13,14的冰解臭氧分解（USO）方法。 USO工艺用于制备稳定的水分散体，其适用于将CNT和GNP两者电泳沉积（EPD）到碳和玻璃纤维上。将提供使用USO官能化的CNT将不均匀薄膜沉积到不锈钢和碳织物基底上的EPD的实例。还将使用X射线光电子能谱（XPS）和拉曼光谱来提供用于化学表征官能化CNT和GNP的方法和典型结果。将提供与其他功能化技术相比较的表征结果的简要讨论。 工作健康安全通知书暴露于纳米颗粒（如碳纳米管）对人体健康的影响尚不清楚。它建议采取特殊措施，尽量减少CNT粉末的暴露和避免环境污染。建议的危害隔离措施包括在配有HEPA过滤器的通风橱和/或手套箱内工作。职业卫生措施包括穿防护服和两层手套，并使用湿纸巾或带有HEPA过滤器的吸尘器定期清洁表面，以除去杂散CNT粉末。污染物品应装箱危险废物处理。 暴露于臭氧会刺激眼睛，肺部和呼吸系统，而在较高浓度下可能会导致肺部的损伤。建议采取措施尽可能减少对生成的臭氧气体的个人和环境影响。隔离措施包括在通风柜内工作。由于返回空气流将包含未使用的臭氧，因此应在通入臭氧破坏装置之前进入大气领域。已经臭氧气泡通过的分散体将含有一些溶解的臭氧。在臭氧分解操作后，允许分散体静置1小时，然后进行进一步处理，以使臭氧进行自然分解。

<table><tbody><tr><td>Ultrasonic bath</td><td>Soniclean</td><td>80TD</td><td></td></tr><tr><td>Ultrasonic horn</td><td>Misonix</td><td>S-4000-010 with CL5 converter</td><td>Daintree Scientific</td></tr><tr><td>Flocell stainless steel water jacketed</td><td>Misonix</td><td>800BWJ</td><td>Daintree Scientific</td></tr><tr><td>Peristaltic pump</td><td>Masterflex easy-load</td><td>7518-00</td><td></td></tr><tr><td>Controller for peristaltic pump</td><td>Masterflex modular controller</td><td>7553-78</td><td></td></tr><tr><td>Ozone generator</td><td>Ozone Solutions</td><td>TG-20</td><td></td></tr><tr><td>Ozone destruct unit</td><td>Ozone Solutions</td><td>ODS-1</td><td></td></tr><tr><td>Recirculating liquid cooler</td><td>Thermoline</td><td>TRC2-571-T</td><td></td></tr><tr><td>Multi-mode power supply unit</td><td>TTi</td><td>EX752M</td><td></td></tr><tr><td>High resolution computing multimeter</td><td>TTi</td><td>1906</td><td></td></tr><tr><td>X-ray photoelectron spectroscopy</td><td>Kratos Analytical</td><td>Axis Nova</td><td></td></tr><tr><td>XPS analysis software</td><td>Casa Software</td><td>Casa XPS</td><td>www.casaxps.com</td></tr><tr><td>Kratos elemental library for use with Casa XPS</td><td>Casa Software</td><td>Download Kratos Related Files</td><td>http://www.casaxps.com/kratos/</td></tr><tr><td>Raman dispersive confocal microscope</td><td>Thermo</td><td>DXR</td><td></td></tr><tr><td>Field emission scanning electron microscope</td><td>Leo</td><td>1530 VP</td><td></td></tr><tr><td>Sputter coater with iridium target</td><td>Cressington</td><td>208 HR</td><td></td></tr><tr><td>Thickness measurement unit</td><td>Cressington</td><td>mtm 20</td><td></td></tr><tr><td>Magnetic stirrer</td><td>Stuart</td><td>CD162</td><td></td></tr><tr><td>Analytical balance</td><td>Kern</td><td>ALS 220-4N</td><td></td></tr><tr><td>Analytical balance</td><td>Mettler Toledo</td><td>NewClassic MF MS 2045</td><td></td></tr><tr><td>Laboratory balance</td><td>Shimadzu</td><td>ELB 3000</td><td></td></tr><tr><td>Electrodes from 316 stainless steel sheet</td><td>RS Components</td><td>559-199</td><td></td></tr><tr><td>Sanding sheets, P1000 grade</td><td>Norton</td><td>No-Fil A275</td><td></td></tr><tr><td>Multi-walled carbon nanotubes</td><td>Hanwha</td><td>CM-95</td><td>http://hcc.hanwha.co.kr/eng/business/bus_table/nano_02.jsp</td></tr><tr><td>Graphene nanoplatelets</td><td>XG Sciences</td><td>XGNP Grade C</td><td>http://xgsciences.com/products/graphene-nanoplatelets/grade-c/</td></tr></tbody></table>

functionalization and dispersion of carbon nanomaterials using an environmentally friendly ultrasonicated ozonolysis process

碳纳米材料的功能化通常是促进其融入更大材料体系和器件的关键步骤。以收纳的形式，碳纳米管（CNT）或石墨烯纳米片（GNP）等碳纳米材料可能含有大的附聚物。当碳纳米管或GNP纳入聚合物或复合材料体系中时，附聚物和杂质都会降低提供的独特电气和机械性能的优点。虽然存在用于官能化碳纳米材料和产生稳定的分散体的各种方法，但是许多方法使用苛刻的化学品，有机溶剂或表面活性剂，这是环境不友好的，并且当分离纳米材料以供后续使用时可能增加处理负担。目前的研究详细介绍了使用替代的，环保的CNT和GNP功能化技术。它产生不含腐蚀性的稳定的水性分散体ul化学品。 CNT和GNP都可以以高达5 g / L的浓度添加到水中，并可通过高功率超声波电池再循环。同时将臭氧注入到电池中逐渐氧化碳纳米材料，并且组合的超声波分解聚集体并立即暴露新鲜的材料进行官能化。制备的分散体理想地适用于使用电泳沉积（EPD）将薄膜沉积在固体底物上。来自水分散体的CNT和GNP可以容易地用于使用EPD涂覆碳纤维和玻璃增强纤维来制备分级复合材料。

图3显示了经过USO处理的CNT的XPS宽扫描表征。没有经历过USO的CNT几乎没有显示出氧含量。随着USO时间的增加，表面氧含量增加。 图4将氧碳比提高为USO时间的函数。 表1显示了用USO处理的GNP的去卷积碳原子浓度。峰值拟合使用由Gr1至Gr6表示的约束峰的组合来表示由于石墨和相关的能量损失特征17引起的固有峰形。然后?...

Watch this Scientific Journal Video about Functionalization and Dispersion of Carbon Nanomaterials Using an Environmentally Friendly Ultrasonicated Ozonolysis Process at JoVE.com

Functionalization and Dispersion of Carbon Nanomaterials Using an Environmentally Friendly Ultrasonicated Ozonolysis Process

这里描述了用于碳纳米材料在水性环境中的官能化和稳定分散的新方法。将臭氧直接注入碳纳米材料的水分散体中，其通过高功率超声波细胞连续再循环。

碳纳米材料的功能化和分散使用环境友好的超声波臭氧分解过程

Functionalization of carbon nanomaterials is often a critical step that facilitates their integration into larger material systems and devices. In the ...

functionalization-dispersion-carbon-nanomaterials-using-an

Research

JoVE Journal

Environment

10.2K 次观看.  Defence Science and Technology Group. 这里描述了用于碳纳米材料在水性环境中的官能化和稳定分散的新方法。将臭氧直接注入碳纳米材料的水分散体中，其通过高功率超声波细胞连续再循环。 

视频: Functionalization and Dispersion of Carbon Nanomaterials Using an Environmentally Friendly Ultrasonicated Ozonolysis Process

Dry Oxidation and Vacuum Annealing Treatments for Tuning the Wetting Properties of Carbon Nanotube Arrays

In this article, we describe a simple method to reversibly tune the wetting properties of vertically aligned carbon nanotube (CNT) arrays. Here, CNT arrays are defined as densely packed multi-walled carbon nanotubes oriented perpendicular to the growth substrate as a result of a growth process by the standard thermal chemical vapor deposition (CVD) technique.1,2 These CNT arrays are then exposed to vacuum annealing treatment to make them more hydrophobic or to dry oxidation treatment to render them more hydrophilic. The hydrophobic CNT arrays can be turned hydrophilic by exposing them to dry oxidation treatment, while the hydrophilic CNT arrays can be turned hydrophobic by exposing them to vacuum annealing treatment. Using a combination of both treatments, CNT arrays can be repeatedly switched between hydrophilic and hydrophobic.2 Therefore, such combination show a very high potential in many industrial and consumer applications, including drug delivery system and high power density supercapacitors.3-5
The key to vary the wettability of CNT arrays is to control the surface concentration of oxygen adsorbates. Basically oxygen adsorbates can be introduced by exposing the CNT arrays to any oxidation treatment. Here we use dry oxidation treatments, such as oxygen plasma and UV/ozone, to functionalize the surface of CNT with oxygenated functional groups. These oxygenated functional groups allow hydrogen bond between the surface of CNT and water molecules to form, rendering the CNT hydrophilic. To turn them hydrophobic, adsorbed oxygen must be removed from the surface of CNT. Here we employ vacuum annealing treatment to induce oxygen desorption process. CNT arrays with extremely low surface concentration of oxygen adsorbates exhibit a superhydrophobic behavior.

This article describes a simple method to fabricate vertically aligned carbon nanotube arrays by CVD and to subsequently tune their wetting properties by exposing them to vacuum annealing or dry oxidation treatment.

干式氧化及真空退火处理调整的润湿性能的碳纳米管阵列

In this article, we describe a simple method to reversibly  tune the wetting properties of vertically aligned carbon nanotube (CNT) arrays.  Here, CNT ...

科研

工程学

Synthesis and Functionalization of Nitrogen-doped Carbon Nanotube Cups with Gold Nanoparticles as Cork Stoppers

Nitrogen-doped carbon nanotubes consist of many cup-shaped graphitic compartments termed as nitrogen-doped carbon nanotube cups (NCNCs). These as-synthesized graphitic nanocups from chemical vapor deposition (CVD) method were stacked in a head-to-tail fashion held only through noncovalent interactions. Individual NCNCs can be isolated out of their stacking structure through a series of chemical and physical separation processes. First, as-synthesized NCNCs were oxidized in a mixture of strong acids to introduce oxygen-containing defects on the graphitic walls. The oxidized NCNCs were then processed using high-intensity probe-tip sonication which effectively separated the stacked NCNCs into individual graphitic nanocups. Owing to their abundant oxygen and nitrogen surface functionalities, the resulted individual NCNCs are highly hydrophilic and can be effectively functionalized with gold nanoparticles (GNPs), which preferentially fit in the opening of the cups as cork stoppers. These graphitic nanocups corked with GNPs may find promising applications as nanoscale containers and drug carriers.

We discussed the synthesis of individual graphitic nanocups using a series of techniques including chemical vapor deposition, acid oxidation and probe-tip sonication. By citrate reduction of HAuCl4, the graphitic nanocups were effectively corked with gold nanoparticles due to the chemically reactive edges of the cups.

黄金纳米粒子作为软木塞氮掺杂碳纳米管杯的合成与功能构造

Nitrogen-doped carbon  nanotubes consist of many cup-shaped graphitic compartments termed as  nitrogen-doped carbon nanotube cups (NCNCs).  These ...

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

化学

Preparation of Carbon Nanosheets at Room Temperature

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into defined aggregates in aqueous media and at the air-water interface. In the aggregated state, the oligoynes can then be carbonized under mild conditions while preserving the morphology and the embedded chemical functionalization. This novel approach provides direct access to functionalized carbon nanomaterials. In this article, we present a synthetic approach that allows us to prepare hexayne carboxylate amphiphiles as carbon-rich siblings of typical fatty acid esters through a series of repeated bromination and Negishi-type cross-coupling reactions. The obtained compounds are designed to self-assemble into monolayers at the air-water interface, and we show how this can be achieved in a Langmuir trough. Thus, compression of the molecules at the air-water interface triggers the film formation and leads to a densely packed layer of the molecules. The complete carbonization of the films at the air-water interface is then accomplished by cross-linking of the hexayne layer at room temperature, using UV irradiation as a mild external stimulus. The changes in the layer during this process can be monitored with the help of infrared reflection-absorption spectroscopy and Brewster angle microscopy. Moreover, a transfer of the carbonized films onto solid substrates by the Langmuir-Blodgett technique has enabled us to prove that they were carbon nanosheets with lateral dimensions on the order of centimeters.

We present the synthesis of an amphiphilic hexayne and its use in the preparation of carbon nanosheets at the air-water interface from a self-assembled monolayer of these reactive, carbon-rich molecular precursors.

碳纳米片在室温下准备

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into ...

Dispersion of Nanomaterials in Aqueous Media: Towards Protocol Optimization

The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and stability of the suspension. In this study, a systematic step-wise approach is carried out to identify optimal sonication conditions in order to achieve a stable dispersion. This approach has been adopted and shown to be suitable for several nanomaterials (cerium oxide, zinc oxide, and carbon nanotubes) dispersed in deionized (DI) water. However, with any change in either the nanomaterial type or dispersing medium, there needs to be optimization of the basic protocol by adjusting various factors such as sonication time, power, and sonicator type as well as temperature rise during the process. The approach records the dispersion process in detail. This is necessary to identify the time points as well as other above-mentioned conditions during the sonication process in which there may be undesirable changes, such as damage to the particle surface thus affecting surface properties. Our goal is to offer a harmonized approach that can control the quality of the final, produced dispersion. Such a guideline is instrumental in ensuring dispersion quality repeatability in the nanoscience community, particularly in the field of nanotoxicology.

Here, we present a step-wise protocol for the dispersion of nanomaterials in aqueous media with real-time characterization to identify the optimal sonication conditions, intensity, and duration for improved stability and uniformity of nanoparticle dispersions without impacting the sample integrity.

纳米材料在水介质中的分散: 对协议优化的研究

The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and ...

环境科学

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous solution. In a carbon nanotube/PEO105-PPO70-PEO105 (poloxamer 407) aqueous solution, the amphiphilic poloxamer 407 adsorbs onto the carbon nanotube surfaces and self-assembles into continuous layers, driven by intermolecular interactions between constituent molecules. The addition of 5-methylsalicylic acid changes the self-assembled structure from spherical-micellar to a cylindrical morphology. The fabricated poloxamer 407/carbon nanotube hybrid particles exhibit thermo-responsive structural features so that the density and thickness of poloxamer 407 layers are also reversibly controllable by varying temperature. The detailed structural properties of the poloxamer 407/carbon nanotube particles in suspension can be characterized by small-angle neutron scattering experiments and model fit analyses. The distinct curve shapes of the scattering intensities depending on temperature control or addition of aromatic additives are well described by a modified core-shell cylinder model consisting of a carbon nanotube core cylinder, a hydrophobic shell, and a hydrated polymer layer. This method can provide a simple but efficient way for the fabrication and in-situ characterization of carbon nanotube-based nano particles with a structure-tunable encapsulation.

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

单壁碳纳米管与热可逆嵌段共聚物及表征功能化小角度中子散射

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous ...

Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for Cu(II) Through Microwave Pre-Pyrolysis

An environment-friendly technique for synthesizing biomass-based mesoporous activated carbon with high nitrogen-/oxygen-chelating adsorption for Cu(II) is proposed. Bagasse impregnated with phosphoric acid is utilized as the precursor. To pyrolyze the precursor, two separate heating modes are used: microwave pyrolysis and conventional electric-heating pyrolysis. The resulting bagasse-derived carbon samples are modified with nitrification and reduction modification. Nitrogen (N)/oxygen (O) functional groups are simultaneously introduced to the surface of activated carbon, enhancing its adsorption of Cu(II) by complexing and ion-exchange. Characterization and copper adsorption experiments are performed to investigate the physicochemical properties of four prepared carbon samples and determine which heating method favors the subsequent modification for doping of N/O functional groups. In this technique, based on analyzing data of nitrogen adsorption, Fourier transform infrared spectroscopy, and batch adsorption experiments, it is proven that microwave-pyrolyzed carbon has more defect sites and, therefore, time-saving effective microwave pyrolysis contributes more N/O species to the carbon, although it leads to a lower specific surface area. This technique offers a promising route to synthesis adsorbents with higher nitrogen and oxygen content and a higher adsorption capacity of heavy-metal ions in wastewater remediation applications.

Preparation of Biomass-based Mesoporous Carbon with Higher Nitrogen-/Oxygen-chelating Adsorption for CuII Through Microwave Pre-Pyrolysis

Here, we present a protocol to synthesize nitrogen/oxygen dual-doped mesoporous carbon from biomass by chemical activation in different pyrolysis modes followed by modification. We demonstrate that the microwave pyrolysis benefits the subsequent modification process to simultaneously introduce more nitrogen and oxygen functional groups on the carbon.

微波热解法制备了更高氮素/氧螯合吸附的生物物质基介孔碳对 cu (ii) 的研究

An environment-friendly technique for synthesizing biomass-based mesoporous activated carbon with high nitrogen-/oxygen-chelating adsorption for Cu(II) is ...

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.

Here we report the synthesis and characterization of ordered nanoporous carbon (with a 4.6 nm pore size) and SBA-15 (with a 5.3 nm pore size). The work describes the surface and textural properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the materials.

合成纳米碳和二氧化硅矩阵的表面性能

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

Tuning the Acidity of Pt/ CNTs Catalysts for Hydrodeoxygenation of Diphenyl Ether

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid nanosheets, a series of Pt/xHMNO6/CNTs with different solid acid compositions (x = 5, 20 wt%; M = Nb, Ta; N = Mo, W) have been prepared by carbon nanotube pretreatment, protonic exchange, solid acid exfoliation, aggregation and finally Pt particles impregnation. The Pt/xHMNO6/CNTs are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and NH3-temperature programmed desorption. The study revealed that HNbWO6 nanosheets were attached on CNTs, with some edges of the nanosheets being bent in shape. The acid strength of the supported Pt catalysts increases in the following order: Pt/CNTs &#60; Pt/5HNbWO6/CNTs &#60; Pt/20HNbMoO6/CNTs &#60; Pt/20HNbWO6/CNTs &#60; Pt/20HTaWO6/CNTs. In addition, the catalytic hydroconversion of lignin-derived model compound: diphenyl ether using the synthesized Pt/20HNbWO6 catalyst has been investigated.

A protocol for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs is presented.

调整二苯醚氢氧化的Pt/CNT催化剂的酸度

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid ...

Metal Oxide Heterojunction for Photocatalytic Activities

There is a significant global demand for improvements in synthesis techniques and their optimal characteristics, especially for industrial-scale applications. Sol-gel-based solution combustion synthesis (SG-SCS) is a simple method to produce ordered porous materials. In this regard, Pearson&#39;s hard and soft acids and bases theory assists in selecting host-dopant reactivity to form a proper heterojunction.
The formation of a heterojunction also changes the essential properties of the materials, improving photocatalysis via charge transfer or synergistic activities. A calcination temperature of 500 &#176;C is ideal for this process based on the results of the stability assessment via a differential thermogravimetry ratio analysis (DTG).
The nanoscale dimensions of the nanoparticles (NPs) and nanocomposites (NCs) generated were validated using X-ray diffraction and high-resolution transmission electron microscopy (HRTEM). Furthermore, the scanning electron microscopy micrographs and BET analyses confirmed the porosity nature of the materials. HRTEM, X-ray photoelectron spectroscopy, and energy-dispersive X-ray investigations established the materials composition. The study found that NCs degraded the acid orange 8 (AO8) color more efficiently than bare ZnO.

The development of a heterojunction boosts the photocatalytic activities of solution combustion synthesis, which is a time-/energy-efficient process. Advanced analytical characterization techniques were used in this protocol to evaluate the materials&#39; characteristics, and nanocomposites demonstrated improved acid orange-8 dye degradation.