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 border="0" cellpadding="0" cellspacing="0" width="588">
	
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Ultrasonic bath</td>
			<td style="width:87px;">Soniclean</td>
			<td style="width:119px;">80TD</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Ultrasonic horn</td>
			<td style="width:87px;">Misonix</td>
			<td style="width:119px;">S-4000-010 with CL5 converter</td>
			<td>Daintree Scientific</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Flocell stainless steel water jacketed</td>
			<td style="width:87px;">Misonix</td>
			<td style="width:119px;">800BWJ</td>
			<td>Daintree Scientific</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Peristaltic pump</td>
			<td style="width:87px;">Masterflex easy-load</td>
			<td style="width:119px;">7518-00</td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">Controller for peristaltic pump</td>
			<td style="width:87px;">Masterflex modular controller</td>
			<td style="width:119px;">7553-78</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Ozone generator</td>
			<td style="width:87px;">Ozone Solutions</td>
			<td style="width:119px;">TG-20</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Ozone destruct unit</td>
			<td style="width:87px;">Ozone Solutions</td>
			<td style="width:119px;">ODS-1</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Recirculating liquid cooler</td>
			<td style="width:87px;">Thermoline</td>
			<td style="width:119px;">TRC2-571-T</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Multi-mode power supply unit</td>
			<td style="width:87px;">TTi&#160;</td>
			<td style="width:119px;">EX752M</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">High resolution computing multimeter</td>
			<td style="width:87px;">TTi&#160;</td>
			<td style="width:119px;">1906</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">X-ray photoelectron spectroscopy</td>
			<td style="width:87px;">Kratos Analytical</td>
			<td style="width:119px;">Axis Nova</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">XPS analysis software</td>
			<td style="width:87px;">Casa Software</td>
			<td style="width:119px;">Casa XPS</td>
			<td>www.casaxps.com</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Kratos elemental library for use with Casa XPS</td>
			<td style="width:87px;">Casa Software</td>
			<td style="width:119px;">Download Kratos Related Files</td>
			<td>http://www.casaxps.com/kratos/</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Raman dispersive confocal microscope</td>
			<td style="width:87px;">Thermo</td>
			<td style="width:119px;">DXR</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Field emission scanning electron microscope</td>
			<td style="width:87px;">Leo</td>
			<td style="width:119px;">1530 VP</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Sputter coater with iridium target</td>
			<td style="width:87px;">Cressington</td>
			<td style="width:119px;">208 HR</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Thickness measurement unit</td>
			<td style="width:87px;">Cressington</td>
			<td style="width:119px;">mtm 20</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Magnetic stirrer</td>
			<td style="width:87px;">Stuart</td>
			<td style="width:119px;">CD162</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Analytical balance</td>
			<td style="width:87px;">Kern</td>
			<td style="width:119px;">ALS 220-4N</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Analytical balance</td>
			<td style="width:87px;">Mettler Toledo</td>
			<td style="width:119px;">NewClassic MF MS 2045</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Laboratory balance</td>
			<td style="width:87px;">Shimadzu</td>
			<td style="width:119px;">ELB 3000</td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">Electrodes from 316 stainless steel sheet</td>
			<td style="width:87px;">RS Components</td>
			<td style="width:119px;">559-199</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Sanding sheets, P1000 grade</td>
			<td style="width:87px;">Norton</td>
			<td style="width:119px;">No-Fil A275</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Multi-walled carbon nanotubes</td>
			<td style="width:87px;">Hanwha</td>
			<td style="width:119px;">CM-95</td>
			<td>http://hcc.hanwha.co.kr/eng/business/bus_table/nano_02.jsp</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Graphene nanoplatelets</td>
			<td style="width:87px;">XG Sciences</td>
			<td style="width:119px;">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

Universidad de Cartagena UDEC

Research

JoVE Journal

Environment

10.1K 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

The Use of an Automated System (GreenFeed) to Monitor Enteric Methane and Carbon Dioxide Emissions from Ruminant Animals

Ruminant animals (domesticated or wild) emit methane (CH4) through enteric fermentation in their digestive tract and from decomposition of manure during storage. These processes are the major sources of greenhouse gas (GHG) emissions from animal production systems. Techniques for measuring enteric CH4 vary from direct measurements (respiration chambers, which are highly accurate, but with limited applicability) to various indirect methods (sniffers, laser technology, which are practical, but with variable accuracy). The sulfur hexafluoride (SF6)&#160;tracer gas method is commonly used to measure enteric CH4 production by animal scientists and more recently, application of an Automated Head-Chamber System (AHCS) (GreenFeed, C-Lock, Inc., Rapid City, SD), which is the focus of this experiment, has been growing. AHCS is an automated system to monitor CH4 and carbon dioxide (CO2) mass fluxes from the breath of ruminant animals. In a typical AHCS operation, small quantities of baiting feed are dispensed to individual animals to lure them to AHCS multiple times daily. As the animal visits AHCS, a fan system pulls air past the animal&#8217;s muzzle into an intake manifold, and through an air collection pipe where continuous airflow rates are measured. A sub-sample of air is pumped out of the pipe into non-dispersive infra-red sensors for continuous measurement of CH4 and CO2 concentrations. Field comparisons of AHCS to respiration chambers or SF6 have demonstrated that AHCS produces repeatable and accurate CH4 emission results, provided that animal visits to AHCS are sufficient so emission estimates are representative of the diurnal rhythm of rumen gas production. Here, we demonstrate the use of AHCS to measure CO2 and CH4 fluxes from dairy cows given a control diet or a diet supplemented with technical-grade cashew nut shell liquid.

The Use of an Automated System GreenFeed to Monitor Enteric Methane and Carbon Dioxide Emissions from Ruminant Animals

Accuracy and precision of the techniques used to measure methane emissions from ruminant animals are critically important for the success of greenhouse gas mitigation efforts. This manuscript describes the principles and operation of an automated system to monitor methane and carbon dioxide mass fluxes from the breath of ruminant animals.

自动系统（绿色饲料）的用于监视肠道的甲烷和二氧化碳从反刍动物排放

Ruminant animals (domesticated or wild) emit methane (CH4) through enteric fermentation in their digestive tract and from decomposition of manure during ...

科研

环境科学

Measuring Carbon-based Contaminant Mineralization Using Combined CO2 Flux and Radiocarbon Analyses

A method is described which uses the absence of radiocarbon in industrial chemicals and fuels made from petroleum feedstocks which frequently contaminate the environment. This radiocarbon signal &#8212; or rather the absence of signal &#8212; is evenly distributed throughout a contaminant source pool (unlike an added tracer) and is not impacted by biological, chemical or physical processes (e.g., the 14C radioactive decay rate is immutable). If the fossil-derived contaminant is fully degraded to CO2, a harmless end-product, that CO2 will contain no radiocarbon. CO2 derived from natural organic matter (NOM) degradation will reflect the NOM radiocarbon content (usually &#60;30,000 years old). Given a known radiocarbon content for NOM (a site background), a two end-member mixing model can be used to determine the CO2 derived from a fossil source in a given soil gas or groundwater sample. Coupling the percent CO2 derived from the contaminant with the CO2 respiration rate provides an estimate for the total amount of contaminant degraded per unit time. Finally, determining a zone of influence (ZOI) representing the volume from which site CO2 is collected allows determining the contaminant degradation per unit time and volume. Along with estimates for total contaminant mass, this can ultimately be used to calculate time-to-remediate or otherwise used by site managers for decision-making.

Measuring Carbon-based Contaminant Mineralization Using Combined CO2 Flux and Radiocarbon Analyses

A protocol is described wherein CO2 mineralized from organic contaminant (derived from petroleum feedstocks) biodegradation is trapped, quantified, and analyzed for 14C content. A model is developed to determine CO2 capture zone's spatial extent. Spatial and temporal measurements allow integrating contaminant mineralization rates for predicting remediation extent and time.

测量碳为基础的污染物矿化结合使用CO<sub&gt; 2</sub&gt;助焊剂和放射性碳分析

A method is described which uses the absence of radiocarbon in industrial chemicals and fuels made from petroleum feedstocks which frequently contaminate ...

Spotting Cheetahs: Identifying Individuals by Their Footprints

The cheetah (Acinonyx jubatus) is Africa's most endangered large felid and listed as Vulnerable with a declining population trend by the IUCN1. It ranges widely over sub-Saharan Africa and in parts of the Middle East. Cheetah conservationists face two major challenges, conflict with landowners over the killing of domestic livestock, and concern over range contraction. Understanding of the latter remains particularly poor2. Namibia is believed to support the largest number of cheetahs of any range country, around 30%, but estimates range from 2,9053 to 13,5204. The disparity is likely a result of the different techniques used in monitoring.
Current techniques, including invasive tagging with VHF or satellite/GPS collars, can be costly and unreliable. The footprint identification technique5 is a new tool accessible to both field scientists and also citizens with smartphones, who could potentially augment data collection. The footprint identification technique analyzes digital images of footprints captured according to a standardized protocol. Images are optimized and measured in data visualization software. Measurements of distances, angles, and areas of the footprint images are analyzed using a robust cross-validated pairwise discriminant analysis based on a customized model. The final output is in the form of a Ward's cluster dendrogram. A user-friendly graphic user interface (GUI) allows the user immediate access and clear interpretation of classification results.
The footprint identification technique algorithms are species specific because each species has a unique anatomy. The technique runs in a data visualization software, using its own scripting language (jsl) that can be customized for the footprint anatomy of any species. An initial classification algorithm is built from a training database of footprints from that species, collected from individuals of known identity. An algorithm derived from a cheetah of known identity is then able to classify free-ranging cheetahs of unknown identity. The footprint identification technique predicts individual cheetah identity with an accuracy of &gt;90%.

The cheetah (Acinonyx jubatus) is an iconic, endangered species, but conservation efforts are challenged by habitat shrinkage and conflict with commercial farmers. The footprint identification technique, a robust, accurate and cost-effective image classification system, is a new approach to monitoring cheetahs.

通过他们的足迹识别个体:合模猎豹

The cheetah (Acinonyx jubatus) is Africa's most endangered large felid and listed as Vulnerable with a declining population trend by the IUCN1. It ranges ...

Assessment of Labile Organic Carbon in Soil Using Sequential Fumigation Incubation Procedures

Management practices and environmental changes can alter soil nutrient and carbon cycling. Soil labile organic carbon, a readily decomposable C pool, is highly sensitive to disturbance. It is also the primary substrate for soil microorganisms, which is fundamental to nutrient cycling. Due to these attributes, labile organic carbon (LOC) has been identified as an indicator parameter for soil health. Quantifying the turnover rate of LOC also aids in understanding changes in soil nutrient cycling processes. A sequential fumigation incubation method has been developed to estimate soil LOC and potential C turnover rate. The method requires fumigating soil samples and quantifying CO2-C respired during a 10 day incubation period over a series of fumigation-incubation cycles. Labile organic C and potential C turnover rate are then extrapolated from accumulated CO2 with a negative exponential model. Procedures for conducting this method are described.

Labile organic carbon (LOC) and the potential carbon turnover rate are sensitive indicators of changes in soil nutrient cycling processes. Details are provided for a method based on fumigating and incubating soil in a series of cycles and using the CO2 accumulated during the incubation periods to estimate these parameters.

活性有机碳评估土壤中连续熏蒸孵化程序

Management practices and environmental changes can alter soil nutrient and carbon cycling. Soil labile organic carbon, a readily decomposable C pool, is ...

Biofilm Removal Using Carbon Dioxide Aerosols without Nitrogen Purge

Biofilms can cause serious concerns in many applications. Not only can they cause economic losses, but they can also present a public health hazard. Therefore, it is highly desirable to remove biofilms from surfaces. Many studies on CO2 aerosol cleaning have employed nitrogen purges to increase biofilm removal efficiency by reducing the moisture condensation generated during the cleaning. However, in this study, periodic jets of CO2 aerosols without nitrogen purges were used to remove Pseudomonas putida biofilms from polished stainless steel surfaces. CO2 aerosols are mixtures of solid and gaseous CO2 and are generated when high-pressure CO2 gas is adiabatically expanded through a nozzle. These high-speed aerosols were applied to a biofilm that had been grown for 24 hr. The removal efficiency ranged from 90.36% to 98.29% and was evaluated by measuring the fluorescence intensity of the biofilm as the treatment time was varied from 16 sec to 88 sec. We also performed experiments to compare the removal efficiencies with and without nitrogen purges; the measured biofilm removal efficiencies were not significantly different from each other (t-test, p &gt; 0.55). Therefore, this technique can be used to clean various bio-contaminated surfaces within one minute.

Biofilms on surfaces can be effectively and rapidly removed by using a periodic jet of carbon dioxide aerosols without a nitrogen purge.

去除生物膜使用二氧化碳气溶胶没有氮气吹扫

Biofilms can cause serious concerns in many applications. Not only can they cause economic losses, but they can also present a public health hazard. ...

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The system comprises a high-pressure rheometer which is connected to a circulation loop. The rheometer has a rotational flow-through measurement cell with two alternative geometries: coaxial cylinder and double gap. The circulation loop contains a mixer, to bring the crude oil sample into equilibrium with CO2, and a gear pump that transports the mixture from the mixer to the rheometer and recycles it back to the mixer. The CO2 and crude oil are brought to equilibrium by stirring and circulation and the rheology of the saturated mixture is measured by the rheometer. The system is used to measure the rheological properties of Zuata crude oil (and its toluene dilution) in equilibrium with CO2 at elevated pressures up to 220 bar and a temperature of 50 &#176;C. The results show that CO2 addition changes the oil rheology significantly, initially reducing the viscosity as the CO2 pressure is increased and then increasing the viscosity above a threshold pressure. The non-Newtonian response of the crude is also seen to change with the addition of CO2.

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

A method for measuring the rheology of crude oil in equilibrium with carbon dioxide at reservoir conditions is presented.

与CO平衡的原油流变学测量<sub&gt; 2</sub&gt;在水库条件

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The ...

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 ...

Use of Principal Components for Scaling Up Topographic Models to Map Soil Redistribution and Soil Organic Carbon

Landscape topography is a critical factor affecting soil formation and plays an important role in determining soil properties on the earth surface, as it regulates the gravity-driven soil movement induced by runoff and tillage activities. The recent application of Light Detection and Ranging (LiDAR) data holds promise for generating high spatial resolution topographic metrics that can be used to investigate soil property variability. In this study, fifteen topographic metrics derived from LiDAR data were used to investigate topographic impacts on redistribution of soil and spatial distribution of soil organic carbon (SOC). Specifically, we explored the use of topographic principal components (TPCs) for characterizing topography metrics and stepwise principal component regression (SPCR) to develop topography-based soil erosion and SOC models at site and watershed scales. Performance of SPCR models was evaluated against stepwise ordinary least square regression (SOLSR) models. Results showed that SPCR models outperformed SOLSR models in predicting soil redistribution rates and SOC density at different spatial scales. Use of TPCs removes potential collinearity between individual input variables, and dimensionality reduction by principal component analysis (PCA) diminishes the risk of overfitting the prediction models. This study proposes a new approach for modeling soil redistribution across various spatial scales. For one application, access to private lands is often limited, and the need to extrapolate findings from representative study sites to larger settings that include private lands can be important.

Landscape processes are critical components of soil formation and play important roles in determining soil properties and spatial structure in landscapes. We propose a new approach using stepwise principal component regression to predict soil redistribution and soil organic carbon across various spatial scales.

利用主成分扩展地形模型绘制土壤再分配和土壤有机碳

Landscape topography is a critical factor affecting soil formation and plays an important role in determining soil properties on the earth surface, as it ...

Split Point Analysis and Uncertainty Quantification of Thermal-Optical Organic/Elemental Carbon Measurements

Researchers from myriad fields frequently seek to quantify and classify concentrations of carbonaceous aerosols as organic carbon (OC) or elemental carbon (EC). This is commonly accomplished using thermal-optical OC/EC analyzers (TOAs), which enable measurement via controlled thermal pyrolysis and oxidation under specific temperature protocols and within constrained atmospheres. Several commercial TOAs exist, including a semi-continuous instrument that enables on-line analyses in the field. This instrument employs an in-test calibration procedure that requires relatively frequent calibration. This article details a calibration protocol for this semi-continuous TOA and presents an open-source software tool for data analysis and rigorous Monte Carlo quantification of uncertainties. Notably, the software tool includes novel means to correct for instrument drift and identify and quantify the uncertainty in the OC/EC split point. This is a significant improvement on the uncertainty estimation in the manufacturer&#8217;s software, which ignores split point uncertainty and otherwise uses fixed equations for relative and absolute errors (generally leading to under-estimated uncertainties and often yielding non-physical results as demonstrated in several example data sets). The demonstrated calibration protocol and new software tool enabling accurate quantification of combined uncertainties from calibration, repeatability, and OC/EC split point are shared with the intent of assisting other researchers in achieving better measurements of OC, EC, and total carbon mass in aerosol samples.

This article presents a protocol and software tool for the quantification of uncertainties in the calibration and data analysis of a semi-continuous thermal-optical organic/elemental carbon analyzer.

热光学有机/元素碳测量的分割点分析与不确定性定量

Researchers from myriad fields frequently seek to quantify and classify concentrations of carbonaceous aerosols as organic carbon (OC) or elemental carbon ...

Measuring Phosphorus Release in Laboratory Microcosms for Water Quality Assessment

Phosphorus (P) is a critical limiting nutrient in agroecosystems requiring careful management to reduce transport risk to aquatic environments. Routine laboratory measures of P bioavailability are based on chemical extractions performed on dried samples under oxidizing conditions. While useful, these tests are limited with respect to characterizing P release under prolonged water saturation. Labile orthophosphate bound to oxidized iron and other metals can rapidly desorb to solution in reducing environments, increasing P mobilization risk to surface runoff and groundwater. To better quantify P desorption potential and mobility during extended saturation, a laboratory microcosm method was developed based on repeated sampling of porewater and overlying floodwater over time. The method is useful for quantifying P release potential from soils and sediments varying in physicochemical properties and can improve site-specific P mitigation efforts by better characterizing P release risk in hydrologically active areas. Advantages of the method include its ability to simulate in situ dynamics, simplicity, low cost, and flexibility.

Accurate quantification of phosphorus (P) desorption potential in saturated soils and sediments is important for P modeling and transport mitigation efforts. To better account for in situ soil-water redox dynamics and P mobilization under prolonged saturation, a simple approach was developed based on repeated sampling of laboratory microcosms.

测量实验室微量微生物中的磷释放,用于水质评估

Phosphorus (P) is a critical limiting nutrient in agroecosystems requiring careful management to reduce transport risk to aquatic environments. Routine ...

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

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