这项工作得到了蒙特雷工艺学院和加州大学尔湾分校的支持。

3D人造毛发碳结构制作注意:使用个人防护装备。按照实验室指导使用仪器并在实验室内工作。 <ol><li>通过用DI水洗涤并用N 2气体干燥来准备收集的人发。 </li><li>根据需要排列毛发，例如平行的股线，交叉，两根毛发缠绕在一起等。 </li><li>使用SU8将毛发连接到硅基板上，或将它们直接保留在陶瓷舟皿中。 </li><li>将头发附着的硅衬底或舟子放入炉中。 </li><li>打开炉子并打开惰性气体（N 2 ）罐的阀门。 注意:最佳气体流速取决于炉管的体积。 6L / min的流量用于管体积为6L。为了在炉管中建立完全惰性的环境，气体流量比最佳气体f前15分钟采用低速率。 </li><li> 设置参数，包括最大热解温度，温度升温速率和惰性气体流量，并运行炉。 <ol><li>例如，以5℃/ min的升温速率将温度从室温升至300℃。保持在300°C 1小时稳定。进一步将温度升高至900℃，并将其保持1小时以进行碳化。 </li><li>将炉子以10℃/ min的速度冷却至300℃，并关闭炉的加热器，因为在300℃后不需要受控的冷却。将样品放入炉中，直到温度达到室温N 2流量。 </li></ol></li><li>完成热解过程后，关闭炉子和气体流。 </li><li>将样品从炉中取出。 </li></ol> 3D聚合物结构制造:光刻<ol><li>梅使用适当的软件包来点燃所需3D光刻胶结构的2D布局并准备印刷的掩模（ 即，聚乙烯photofilm掩模）。 注意:使用商业服务来打印设计。面罩的尺寸一般取决于设计。 </li><li>在一个干净的实验室设施中，打开两个热板，将温度分别设定为65°C和95°C。 </li><li>打开旋涂机和真空泵。确保真空泵通过管道连接到旋转头。 </li><li>设置两步旋转的参数，如旋转速度，斜坡和持续时间。对于第一步，将旋转速度设置为500 rpm，斜坡至100 rpm / s，旋转时间设置为10 s以开始旋转循环。对于下一步骤，将旋转速度设置为1,000 rpm，斜坡至100 rpm / s，旋转时间设置为30 s，以均匀铺展光致抗蚀剂。 </li><li>放置基板（ 即 4英寸x 4英寸和550英寸）1;具有1μm厚SiO 2层的m±25μm厚的Si晶片）。 </li><li>将光敏聚合物（即 SU8光致抗蚀剂）直接沉积到基底的中心。足够用于覆盖表面。 </li><li>按"真空"按钮固定基板。 </li><li>按"运行"按钮用SU8涂覆基材，达到250μm的最终厚度。 </li><li>纺丝工序完成后，再次按下"真空"按钮，将涂布的基材从支架上释放出来。 </li><li>使用镊子小心地握住涂覆的基材，以保持表面光滑和清洁。将基板直接在65℃温度下转移到热板上6分钟，然后在95℃的温度下将其放置在热板上40分钟（软烘烤）。 注意:为了确保溶剂蒸发缓慢，需要在65°C烘烤，导致更好的涂层和更好的附着力在95℃下烘烤时，进一步使SU8致密化。 </li><li>同时，按开关打开UV曝光系统，并使用系统中的设置按钮将曝光时间设置为"12秒"。 注意:对于250μm厚的SU8层，曝光能量必须为360 mJ / cm 2 。 </li><li>一旦烘烤步骤（步骤2.10）完成，将基材放入UV曝光系统中，并将光掩模（来自步骤2.1）的印刷面放置在其上。使用整个面罩区域覆盖涂覆的基材，轻轻按压，以确保面罩和基材之间没有间隙。 </li><li>通过使用预定义的UV设置，通过光掩模将SU8涂覆的基材曝光于UV辐射。 </li><li>通过将其直接放置在65℃的热板上5分钟，并在95℃放置14分钟以进行后曝光烘烤（PEB），再次加热基材。 注意:PEB增加了紫外线曝光区域的交联度，在显影步骤中涂层更耐溶剂。 </li><li>将基材浸入专用显影剂溶液中，放置在烧杯中20分钟，去除未曝光的光致抗蚀剂区域。连续摇动溶液（小心）以确保完全除去未曝光的抗蚀剂区域。 </li><li>通过保持底物并将氮气或压缩空气吹入其中来干燥显影结构。 </li><li>在50倍放大倍率的显微镜下检查晶片，以将所转移到光致抗蚀剂上的图案与所需的图案进行比较。 </li></ol> 3D碳结构制造:热解<ol><li>将使用光刻（步骤2.1-2.17）制备的样品放在加压的开放式管式炉内。 </li><li>打开炉子并设置热解参数，如上述步骤1所述。重复步骤1.6-1.8中的过程。 </li><li>使用镊子仔细处理样品，并进行特征处理通货膨胀。 </li></ol>

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作者没有什么可以披露的。

在本文中，报道了基于天然前体材料或光致图案化聚合物结构的热解制备各种碳微结构的方法。由传统的和非常规的C-MEMS / C-NEMS工艺产生的碳材料通常被发现是玻璃碳。玻璃碳是广泛使用的电化学电极材料，也适用于高温应用。玻璃碳的微结构由结晶和非晶区组成。玻璃碳具有高导电性，耐高温性，低密度，低电阻，以及较高的硬度和高耐化学腐蚀性。 我们提出了一种简单且低成本的方法来从人类头发制造中空玻璃碳微纤维，并描述了其应用于抗坏血酸和多巴胺的电化学感测。制造长，霍尔低导电性的碳微纤维可以通过低成本的一步热处理作为废料的人发。由髓质，皮层和角质层组成的人体毛发在热解后产生中空碳纤维。髓质消失，而角质层和皮质组合在一起，形成长而中空的碳纤维。人类头发的独特解剖特征，特别是其热解后的中空结构，其特征在于表面积显着增加，导致其在电化学感测中的应用。对于用毛发衍生的碳改性的工作电极，多巴胺和抗坏血酸的峰值电位分别转移到更多的负值和正值。头发衍生的碳的表面几乎没有带负电荷，其吸收正电荷的多巴胺，因此，多巴胺的峰电流增加，抗坏血酸降低。结果，人类头发衍生的中空碳在抗坏血酸存在下，微纤维可用于检测多巴胺。已经进行了裸电极和改性电极（含有毛发碳和CNT）的电化学感测性能的比较研究。毛发来源的碳改性电极比未修饰的电极显示出更好的感测性能，但是如预期的那样，CNT涂覆的电极在这些实验条件下显示出用于感测多巴胺和抗坏血酸的最佳性能。由于碳纳米管的表面积与体积之比大于头发衍生的中空碳纤维，因此显示出较高的灵敏度。然而，使用头发衍生的碳微纤维超过CNT的主要优点是极低的成本。易于制备头发衍生的碳也使它们在CNT上占主导地位。可以通过在热分解之前或之后进一步修饰或官能化人毛来提高感测性能。 收缩效应由于热解是不可避免的，因为非碳原子在高温下与碳键分离，导致大量的质量损失。在设计所需的结构之前，应该对图案化结构的预期收缩率进行很好的估计。在这里，研究了使用常规C-MEMS工艺制造的碳结构的收缩率，其包括聚合物结构的光图案化和热解两个步骤。对于收缩研究考虑了不同内径（0,30,50,75和100μm）的五个结构，而对于所有结构，外径保持恒定在150μm。内径为0,30,50和75μm的结构在热解后表现出比内径更大的外径收缩率。在这些情况下，外表面积大于内表面积。因此，在收缩过程中外表面是主导的，允许更多的非碳原子檐下结构。在内径为100μm的结构中，内表面积也占总表面积的很大一部分，内表面和外表面都收缩。 热解参数，如热解时间，最大热解温度，大气环境等因素，对导电性，化学成分，电化学性能等碳结构的性能有明显的影响。揭示了热解条件对碳结构质量和性能的影响。在常规C-MEMS的情况下，也可以制造具有不同电学和机械性能的碳结构，通过改变光刻条件，例如烘烤时间，烘烤温度，光致抗蚀剂的类型，可以产生各种各样的应用，和添加剂。这是我们的相信这项研究可以为研究人员在碳结构纳米/微细加工领域为各种应用提供实质和有用的信息。

碳具有许多同素异形体，并且根据具体应用，可以选择以下同素异形体之一:碳纳米管（CNT），石墨，金刚石，无定形碳，代斯尼石，勃姆斯特富勒烯（C 60 ），充铁矿（C 540 ），富勒烯C 70 ）和玻璃碳1,2,3,4 。玻璃碳是最广泛使用的同素异形体之一，因为它的物理性质，包括高各向同性。它还具有以下性能:良好的导电性，低热膨胀系数和气体不渗透性。 已经不断地寻找富含碳的前体材料来获得碳结构。这些前体可以是具有特定形状的人造材料或天然产物，甚至包括废物。各种微型<html> o /纳米结构本质上是通过生物或环境过程形成的，产生了使用常规制造工具极难创造的独特特征。由于在这种情况下自然发生了图案化，使用天然和废碳氢化合物前体的纳米材料的合成可以在惰性或真空气氛中使用简单的一步热分解方法进行，称为热解5 。已经通过热分解或植物来源的前体和废物（包括种子，纤维和油类）的热分解产生了高质量的石墨烯，单壁CNT，多壁碳纳米管和碳点，例如松节油，芝麻油，楝树油（ Azadirachta indica ），桉树油，棕榈油和麻疯树油。此外，茉莉花产品，茶树提取物，废物食品，昆虫，农业废物和食品已被利用6，7 ，最近，研究人员甚至使用丝茧作为前体材料来制备多孔碳微纤维10 。这个团队最近使用人造毛，通常被认为是废料。它由约91％的多肽组成，含多于50％的碳;其余的元素如氧，氢，氮和硫11 。头发还具有许多有趣的性质，例如非常缓慢的降解，高抗拉强度，高绝热性和高弹性恢复性。最近，它已经被用于制备超级电容器12中使用的碳薄片，并且为电化学传感13创建中空碳微纤维13 。 用于制造三维（3D）结构的散装碳材料的加工是一项困难的任务，因为该材料非常脆弱。聚焦离子在这种情况下，am 14,15或反应离子蚀刻16可能是有用的，但是它们是昂贵和耗时的过程。基于图案化聚合物结构的热解的碳微机电系统（C-MEMS）技术代表了多功能的替代方案。在过去二十年中，C-MEMS和碳纳米机电系统（C-NEMS）由于涉及简单且廉价的制造步骤而受到很多关注。传统的C-MEMS制造工艺分两个步骤进行:（i）通过光刻图案化聚合物前体（ 例如，光致抗蚀剂）和（ii）图案化结构的热解。通常使用紫外（UV）可固化的聚合物前体，例如SU8光致抗蚀剂，以基于光刻法来图案化结构。通常，光刻工艺包括旋涂，软烘烤，紫外线曝光，后烘烤和烘烤的步骤lopment。在C-MEMS的情况下;硅;二氧化硅;氮化硅;石英;并且最近，蓝宝石已被用作底物。在无氧环境中，光图案化聚合物结构在高温（800-1100℃）下碳化。在真空或惰性气氛中的这些高温下，除去所有非碳元素，仅留下碳。这种技术允许实现高质量的玻璃碳结构，其对于许多应用非常有用，包括电化学传感17 ，能量存储18 ，摩擦电纳米发生19和电动粒子操作20.此外，制造具有使用C-MEMS的高纵横比变得相对容易，并且已经导致各种各样的碳电极应用18,21 ， </sup&gt; 22,23 ，经常代替贵金属电极。 在这项工作中，引入了使用非常规C-MEMS技术13从人发制造中空碳微纤维的简单和成本有效的方法的最新发展。这里也描述了常规的基于SU8聚合物的C-MEMS工艺。具体来说，高纵横比固体和中空SU8结构的制造程序描述24。

<table border="0" cellpadding="0" cellspacing="0" width="690">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">SU8-2100</td>
			<td style="width:141px;">Microchem</td>
			<td style="width:167px;">Product number-Y1110750500L</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">Spinner</td>
			<td style="width:141px;">Laurell Technologies Corporation</td>
			<td style="width:167px;">Model-WS650HZB-23NPP/UD3</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Hotplate</td>
			<td style="width:141px;">Torrey Pines Scientific</td>
			<td style="width:167px;">HS61</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">UV-exposer</td>
			<td style="width:141px;">Mercury Lamp, SYLVANIA</td>
			<td style="width:167px;">H44GS-100M, P/N-34-0054-01</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Photomask</td>
			<td style="width:141px;">CAD/Art</td>
			<td style="width:167px;"></td>
			<td>No number</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Developer&#160;</td>
			<td style="width:141px;">Microchem</td>
			<td style="width:167px;">Y020100 4000L&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">DI water system</td>
			<td style="width:141px;">Milli Q</td>
			<td style="width:167px;">ZOOQOVOTO</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">IPA</td>
			<td style="width:141px;">CTR Sientific</td>
			<td style="width:167px;">CTR 01244</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">N2 gas</td>
			<td style="width:141px;">AOC Mexico</td>
			<td style="width:167px;"></td>
			<td>No number</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Furnace</td>
			<td style="width:141px;">PEO 601, ATV Technologie GMBH</td>
			<td style="width:167px;">Model-PEO 601, Serial no.-195</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Si/SiO2</td>
			<td style="width:141px;">Noel Technologies</td>
			<td style="width:167px;"></td>
			<td></td>
		</tr>
	</tbody>
</table>

fabrication of 3d carbon microelectromechanical systems (c-mems)

大量的碳源可用于各种微/纳米结构配置。这里引入了一种制造从人类毛发衍生的长而中空的玻璃碳微纤维的新技术。长和中空的碳结构通过人造毛发在900℃在N 2气氛中的热解制备。使用扫描电子显微镜（SEM）和电子分散X射线光谱（EDX）分别研究天然和热解的人毛的形态和化学成分，以估计热解引起的物理和化学变化。拉曼光谱法用于证实碳微观结构的玻璃性质。引入热解的毛发碳以修饰丝网印刷的碳电极;然后将修饰的电极应用于多巴胺和抗坏血酸的电化学感测。与unmodi相比，改进的传感器的感测性能得到改善传感器。为了获得所需的碳结构设计，开发了碳微/纳米机电系统（C-MEMS / C-NEMS）技术。最常见的C-MEMS / C-NEMS制造方法包括两个步骤:（i）使用光刻法富集富含碳的基底材料，例如光敏聚合物;和（ii）在无氧环境中通过图案化聚合物的热解进行碳化。 C-MEMS / NEMS工艺已经广泛用于开发微电子器件，包括微电池，超级电容器，葡萄糖传感器，气体传感器，燃料电池和摩擦电纳米发生器等各种应用。在这里，讨论了具有SU8光致抗蚀剂的高纵横比固体和中空碳微观结构的近期发展。使用共焦显微镜和SEM研究了热解过程中的结构收缩。拉曼光谱法用于证实结构的结晶度，元素的原子百分比使用EDX测量热解前后的材料中的nt。

人头发衍生的中空碳微纤维的制造方法的示意图如图1所示 。使用SEM来表征碳化的人发，以估计收缩。由于热解，毛发直径从82.88±0.003μm缩小到31.42±0.003μm。使用毛发衍生的碳微纤维制成的各种图案的扫描电子显微镜（SEM）图像示于图2中 。在热解之前和之后毛发中存在的元素的原子百分比示于表1中 。本研究中使用的人类头发（原子百分比）为66.57％碳，16.19％氧气，7.94％氮气，9.14％硫磺，以及少量矿物质如钙。在热解后，碳和氧的原子百分比分别为80.84％和14.83％。毛发的拉曼光谱分析b此外， 如图3所示，也进行热分解之后和之后。在热解后，发现对应于D和G带的两个宽峰为毛发。毛发来源的碳纤维中的D带与G带的强度之比计算为0.99，表明毛发纤维主要是玻璃状碳。 应用毛发来源的碳纤维，用电化学传感器检测多巴胺和抗坏血酸。丝网印刷碳电极用毛发衍生的碳纤维改性，并用作传感器的工作电极。用于电化学感测的碳电极的示意图如图4a所示。在pH 7.4的0.1M磷酸盐缓冲溶液中的100μM多巴胺和100μM抗坏血酸的循环伏安图示于图4b和c，分别tively。使用裸碳电极，用毛发衍生的碳改性的碳电极和用CNT改性的碳电极作为传感器的工作电极，以比较检测多巴胺和抗坏血酸的性能。对于裸碳电极，在333mV测量多巴胺的氧化峰，用毛发衍生的碳纤维改性的碳电极为266mV，用CNT改性的电极为96mV。这些电极分别在414 mV，455 mV和297 mV处观察到抗坏血酸的氧化峰。 传统的C-MEMS工艺，聚合物前体的光刻图案和随后的热解的示意图如图5所示 。使用共焦显微镜和SEM来估计这些制造的结构，以估计由于热解引起的收缩。五个圆柱结构t对于本研究，制造了相同的高度（250μm）和外径（150μm），但具有各种内径（ 即， 0（固体），30,50,75和100μm（中空））。测量由于热解引起的圆柱形结构的几何变化。对于不同的内外径结构，收缩的百分比是变化的。内径为0μm（实心微观结构）时，外径缩小约35％。当内径为30,50和75μm时，外径和内径分别减少了约42％和30-35％。在内径为100μm的情况下，内径扩大了12％，而不是收缩，外径仅缩小了15％。在图6中 ，示出了原始内径为30,40和75μm的实心和中空碳微观结构的SEM图像。热解前后空心微结构的3D光学图像ysis也显示在图7中 。根据共聚焦显微镜图像，所有的微观结构均收缩高度近30％（250〜175μm）。 <img alt="图1" class="xfigimg" src="/files/ftp_upload/55649/55649fig1.jpg" /> 图1:人毛发中空碳微纤维制造工艺的示意图。转载自参考文献13的许可。版权所有2016 Elsevier Ltd. <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55649/55649fig1large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图2" class="xfigimg" src="/files/ftp_upload/55649/55649fig2.jpg" /> 图2:头发衍生的碳微纤维的不同图案的SEM图像。 （ a和b ）对齐的straight碳微纤维。刻度棒=50μm。 （ c和d ）线状碳超细纤维。刻度棒分别为20和100μm。 （ e和f ）破碎的中空碳超细纤维。转载自参考文献13的许可。版权所有2016 Elsevier Ltd. <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55649/55649fig2large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图3" class="xfigimg" src="/files/ftp_upload/55649/55649fig3.jpg" /> 图3:热解前后人毛发的拉曼光谱。转载自参考文献13的许可。版权所有2016 Elsevier Ltd. <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55649/55649fig3large.jpg" target="_blank">请点击此处查看此图的较大版本。</a><img alt="图4" class="xfigimg" src="/files/ftp_upload/55649/55649fig4.jpg" /> 图4:多巴胺和抗坏血酸的电化学感应。 （ a ）电化学传感碳电极示意图。 （ b ）100μM多巴胺和（ c ）100μM抗坏血酸的循环伏安图。转载自参考文献13的许可。版权所有2016 Elsevier Ltd. <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55649/55649fig4large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图5" class="xfigimg" src="/files/ftp_upload/55649/55649fig5.jpg" /> 图5:基于光刻和热解的常规C-MEMS工艺的示意图。 （ a ）Spin co（ b ）UV曝光，（ c ）显影和（ d ）热解。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55649/55649fig5large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图6" class="xfigimg" src="/files/ftp_upload/55649/55649fig6.jpg" /> 图6:通过常规C-MEMS工艺制造的碳微结构的扫描电子显微镜图像。 （ a ）固体和（ b ）具有各种内径的中空结构。刻度棒=500μm。放大的图像（c）固体和中空结构，其中热解前的内径为（ d ）30，（ e ）50和（ f ）75μm。刻度棒=50μm。转载自参考资料24的许可。版权所有16，电化学学会。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55649/55649fig6large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <img alt="图7" class="xfigimg" src="/files/ftp_upload/55649/55649fig7.jpg" /> 图7:空心微结构的3D光学图像。 （ a ）热解之前和（ b ）。转载许可转介24 。版权所有2016，电化学学会。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55649/55649fig7large.jpg" target="_blank">请点击此处查看此图的较大版本。</a> <table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always"><tbody><tr><td> 元件 </td><td> 热解前 </td><td> 热解后 </td></tr> &lt;TR&gt; <td></td><td> 原子％ </td><td> 原子％ </td></tr><tr><td>碳</td><td> 66.57 </td><td> 80.84 </td></tr><tr><td>氧</td><td> 16.19 </td><td> 14.83 </td></tr><tr><td>氮</td><td> 7.94 </td><td> 0 </td></tr><tr><td>硫</td><td> 9.14 </td><td> 0.21 </td></tr><tr><td>钙</td><td> 0.16 </td><td> 0.21 </td></tr><tr><td>钠</td><td> 0 </td><td> 0.22 </td></tr><tr><td>硅</td><td> 1.82 </td><td> 3.69 </td></tr></tbody></table> 表1:热溶解前后人毛发EDX分析化学成分。转载自参考文献13的许可。版权所有2016 Elsevier Ltd.

Watch this Scientific Journal Video about Fabrication of 3D Carbon Microelectromechanical Systems C-MEMS at JoVE.com

Fabrication of 3D Carbon Microelectromechanical Systems C-MEMS

基于天然产物，人发的热解制造长而中空的玻璃碳微纤维。碳微机电和碳纳米机电系统或C-MEMS和C-NEMS的两个制造步骤是:（i）富碳聚合物前体的光刻和（ii）图案化聚合物前体的热解。

3D碳微机电系统（C-MEMS）的制造

A wide range of carbon sources are available in nature, with a variety of micro-/nanostructure configurations. Here, a novel technique to fabricate long ...

fabrication-of-3d-carbon-microelectromechanical-systems-c-mems

Nanyang Technological University

Research

JoVE Journal

Engineering

Fabrication of 3D Carbon Microelectromechanical Systems (C-MEMS)

12.0K 次观看.  Tecnologico de Monterrey. 基于天然产物，人发的热解制造长而中空的玻璃碳微纤维。碳微机电和碳纳米机电系统或C-MEMS和C-NEMS的两个制造步骤是:（i）富碳聚合物前体的光刻和（ii）图案化聚合物前体的热解。 

视频: Fabrication of 3D Carbon Microelectromechanical Systems C-MEMS

Fabrication, Densification, and Replica Molding of 3D Carbon Nanotube Microstructures

The introduction of new materials and processes to microfabrication has, in large part, enabled many important advances in microsystems, lab-on-a-chip devices, and their applications. In particular, capabilities for cost-effective fabrication of polymer microstructures were transformed by the advent of soft lithography and other micromolding techniques 1, 2, and this led a revolution in applications of microfabrication to biomedical engineering and biology. Nevertheless, it remains challenging to fabricate microstructures with well-defined nanoscale surface textures, and to fabricate arbitrary 3D shapes at the micro-scale. Robustness of master molds and maintenance of shape integrity is especially important to achieve high fidelity replication of complex structures and preserving their nanoscale surface texture. The combination of hierarchical textures, and heterogeneous shapes, is a profound challenge to existing microfabrication methods that largely rely upon top-down etching using fixed mask templates. On the other hand, the bottom-up synthesis of nanostructures such as nanotubes and nanowires can offer new capabilities to microfabrication, in particular by taking advantage of the collective self-organization of nanostructures, and local control of their growth behavior with respect to microfabricated patterns. 
Our goal is to introduce vertically aligned carbon nanotubes (CNTs), which we refer to as CNT "forests", as a new microfabrication material. We present details of a suite of related methods recently developed by our group: fabrication of CNT forest microstructures by thermal CVD from lithographically patterned catalyst thin films; self-directed elastocapillary densification of CNT microstructures; and replica molding of polymer microstructures using CNT composite master molds. In particular, our work shows that self-directed capillary densification ("capillary forming"), which is performed by condensation of a solvent onto the substrate with CNT microstructures, significantly increases the packing density of CNTs. This process enables directed transformation of vertical CNT microstructures into straight, inclined, and twisted shapes, which have robust mechanical properties exceeding those of typical microfabrication polymers. This in turn enables formation of nanocomposite CNT master molds by capillary-driven infiltration of polymers. The replica structures exhibit the anisotropic nanoscale texture of the aligned CNTs, and can have walls with sub-micron thickness and aspect ratios exceeding 50:1. Integration of CNT microstructures in fabrication offers further opportunity to exploit the electrical and thermal properties of CNTs, and diverse capabilities for chemical and biochemical functionalization 3.

We present methods for fabrication of patterned microstructures of vertically aligned carbon nanotubes (CNTs), and their use as master molds for production of polymer microstructures with organized nanoscale surface texture. The CNT forests are densified by condensation of solvent onto the substrate, which significantly increases their packing density and enables self-directed formation of 3D shapes.

制备，致密，副本三维碳纳米管微结构成型

The introduction of new materials and processes to microfabrication has, in large part, enabled many important advances in microsystems, lab-on-a-chip ...

科研

工程学

High-resolution, High-speed, Three-dimensional Video Imaging with Digital Fringe Projection Techniques

Digital fringe projection (DFP) techniques provide dense 3D measurements of dynamically changing surfaces.&#160;Like the human eyes and brain, DFP uses triangulation between matching points in two views of the same scene at different angles to compute depth.&#160;However, unlike a stereo-based method, DFP uses a digital video projector to replace one of the cameras1. The projector rapidly projects a known sinusoidal pattern onto the subject, and the surface of the subject distorts these patterns in the camera&#8217;s field of view. Three distorted patterns (fringe images) from the camera can be used to compute the depth using triangulation.
Unlike other 3D measurement methods, DFP techniques lead to systems that tend to be faster, lower in equipment cost, more flexible, and easier to develop.&#160;DFP systems can also achieve the same measurement resolution as the camera.&#160;For this reason, DFP and other digital structured light techniques have recently been the focus of intense research (as summarized in1-5). Taking advantage of DFP, the graphics processing unit, and optimized algorithms, we have developed a system capable of 30&#160;Hz 3D video data acquisition, reconstruction, and display for over 300,000 measurement points per frame6,7.&#160;Binary defocusing DFP methods can achieve even greater speeds8.
Diverse applications can benefit from DFP techniques. Our collaborators have used our systems for facial function analysis9, facial animation10, cardiac mechanics studies11, and fluid surface measurements, but many other potential applications exist.&#160;This video will teach the fundamentals of DFP techniques and illustrate the design and operation of a binary defocusing DFP system.

This video describes the fundamentals of digital fringe projection techniques, which provide dense 3D measurements of dynamically changing surfaces.&#160;It also demonstrates the design and operation of a high-speed binary defocusing system based on these techniques.

Digital fringe projection (DFP) techniques provide dense 3D measurements of dynamically changing surfaces.&#160;Like the human eyes and brain, DFP uses ...

Fabrication of Spatially Confined Complex Oxides

Complex materials such as high Tc superconductors, multiferroics, and colossal magnetoresistors have electronic and magnetic properties that arise from the inherent strong electron correlations that reside within them. These materials can also possess electronic phase separation in which regions of vastly different resistive and magnetic behavior can coexist within a single crystal alloy material. By reducing the scale of these materials to length scales at and below the inherent size of the electronic domains, novel behaviors can be exposed. Because of this and the fact that spin-charge-lattice-orbital order parameters each involve correlation lengths, spatially reducing these materials for transport measurements is a critical step in understanding the fundamental physics that drives complex behaviors. These materials also offer great potential to become the next generation of electronic devices 1-3. Thus, the fabrication of low dimensional nano- or micro-structures is extremely important to achieve new functionality. This involves multiple controllable processes from high quality thin film growth to accurate electronic property characterization. Here, we present fabrication protocols of high quality microstructures for complex oxide manganite devices. Detailed descriptions and required equipment of thin film growth, photo-lithography, and wire-bonding are presented.

We describe the use of pulsed laser deposition (PLD), photolithography and wire-bonding techniques to create micrometer scale complex oxides devices. The PLD is utilized to grow epitaxial thin films. Photolithography and wire-bonding techniques are introduced to create practical devices for measurement purposes.

空间密闭的复合氧化物制备

Complex materials such as high Tc superconductors, multiferroics, and colossal magnetoresistors have electronic and magnetic properties that arise from ...

Fabrication and Testing of Microfluidic Optomechanical Oscillators

Cavity optomechanics experiments that parametrically couple the phonon modes and photon modes have been investigated in various optical systems including microresonators. However, because of the increased acoustic radiative losses during direct liquid immersion of optomechanical devices, almost all published optomechanical experiments have been performed in solid phase. This paper discusses a recently introduced hollow microfluidic optomechanical resonator. Detailed methodology is provided to fabricate these ultra-high-Q microfluidic resonators, perform optomechanical testing, and measure radiation pressure-driven breathing mode and SBS-driven whispering gallery mode parametric vibrations. By confining liquids inside the capillary resonator, high mechanical- and optical- quality factors are simultaneously maintained.

Parametric optomechanical excitations have recently been experimentally demonstrated in microfluidic optomechanical resonators by means of optical radiation pressure and stimulated Brillouin scattering. This paper describes the fabrication of these microfluidic resonators along with methodologies for generating and verifying optomechanical oscillations.

制造和微流控光机振荡器测试

Cavity optomechanics experiments that parametrically couple the phonon modes and photon modes have been investigated in various optical systems including ...

Fabrication of Low Temperature Carbon Nanotube Vertical Interconnects Compatible with Semiconductor Technology

We demonstrate a method for the low temperature growth (350 &#176;C) of vertically-aligned carbon nanotubes (CNT) bundles on electrically conductive thin-films. Due to the low growth temperature, the process allows integration with modern low-&#954; dielectrics and some flexible substrates. The process is compatible with standard semiconductor fabrication, and a method for the fabrication of electrical 4-point probe test structures for vertical interconnect test structures is presented. Using scanning electron microscopy the morphology of the CNT bundles is investigated, which demonstrates vertical alignment of the CNT and can be used to tune the CNT growth time. With Raman spectroscopy the crystallinity of the CNT is investigated. It was found that the CNT have many defects, due to the low growth temperature. The electrical current-voltage measurements of the test vertical interconnects displays a linear response, indicating good ohmic contact was achieved between the CNT bundle and the top and bottom metal electrodes. The obtained resistivities of the CNT bundle are among the average values in the literature, while a record-low CNT growth temperature was used.

A method for the growth of low temperature vertically-aligned carbon nanotubes, and the subsequent fabrication of vertical interconnect electrical test structures using semiconductor fabrication is presented.

低温碳纳米管垂直互连的制作兼容半导体技术

We demonstrate a method for the low temperature growth (350 &#176;C) of vertically-aligned carbon nanotubes (CNT) bundles on electrically conductive ...

Fabrication and Characterization of Superconducting Resonators

Superconducting microwave resonators are of interest for a wide range of applications, including for their use as microwave kinetic inductance detectors (MKIDs) for the detection of faint astrophysical signatures, as well as for quantum computing applications and materials characterization. In this paper, procedures are presented for the fabrication and characterization of thin-film superconducting microwave resonators. The fabrication methodology allows for the realization of superconducting transmission-line resonators with features on both sides of an atomically smooth single-crystal silicon dielectric. This work describes the procedure for the installation of resonator devices into a cryogenic microwave testbed and for cool-down below the superconducting transition temperature. The set-up of the cryogenic microwave testbed allows one to do careful measurements of the complex microwave transmission of these resonator devices, enabling the extraction of the properties of the superconducting lines and dielectric substrate (e.g., internal quality factors, loss and kinetic inductance fractions), which are important for device design and performance.

Superconducting microwave resonators are of interest for detection of light, quantum computing applications and materials characterization. This work presents a detailed procedure for fabrication and characterization of superconducting microwave resonator scattering parameters.

制备与表征超导谐振器的

Superconducting microwave resonators are of interest for a wide range of applications, including for their use as microwave kinetic inductance detectors ...

Two-way Valorization of Blast Furnace Slag: Synthesis of Precipitated Calcium Carbonate and Zeolitic Heavy Metal Adsorbent

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with sufficient heavy metal adsorption capacity. To this end, blast furnace slag, a residue from iron-making, is utilized as the starting material. Calcium is selectively extracted from the slag by leaching with acetic acid (2 M CH3COOH) as the extraction agent. The filtered leachate is subsequently physico-chemically purified and then carbonated to form precipitated calcium carbonate (PCC) of high purity (&lt;2 wt% non-calcium impurities, according to ICP-MS analysis). Sodium hydroxide is added to neutralize the regenerated acetate. The morphological properties of the resulting calcitic PCC are tuned for its potential application as a filler in papermaking. In parallel, the residual solids from the extraction stage are subjected to hydrothermal conversion in a caustic solution (2 M NaOH) that leads to the predominant formation of a particular zeolitic mineral phase (detected by XRD), namely analcime (NaAlSi2O6&#8729;H2O). Based on its ability to adsorb Ni2+, as reported from batch adsorption experiments and ICP-OES analysis, this product can potentially be used in wastewater treatment or for environmental remediation applications.

A protocol for the parallel production of precipitated calcium carbonate and zeolitic material from blast furnace slag via mineral carbonation and alkaline hydrothermal conversion, respectively, is presented. The performance of the zeolitic material towards nickel adsorption is tested.

高炉矿渣的双向稳定物价:沉淀碳酸钙和沸石重金属吸附剂的合成

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

通过纳米氧化钇稳定的二氧化锆（YSZ）的支架的高温加工<em&gt;原位</em&gt;碳模板干凝胶

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

Production and Characterization of Vacuum Deposited Organic Light Emitting Diodes

A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex donor-acceptor emitters is presented. With a step-by-step procedure, readers will be able to repeat and produce OLED devices based on simple organic emitters. A patterning procedure allowing the creation of personalized indium tin oxide (ITO) shape is shown. This is followed by the evaporation of all layers, encapsulation and characterization of each individual device. The end goal is to present a procedure that will give the opportunity to repeat the information presented in cited publication but also using different compounds and structures in order to prepare efficient OLEDs.

A protocol for the production of simple structured organic light-emitting diodes (OLEDs) is presented.

真空沉积有机发光二极管的生产与表征

A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex ...

Atmospheric Pressure Fabrication of Large-Sized Single-Layer Rectangular SnSe Flakes

Tin selenide (SnSe) belongs to the family of layered metal chalcogenide materials with a buckled structure like phosphorene, and has shown potential for applications in two-dimensional nanoelectronics devices. Although many methods to synthesize SnSe nanocrystals have been developed, a simple way to fabricate large-sized single-layer SnSe flakes remains a great challenge. Herein, we show the experimental method to directly grow large-sized single-layer rectangular SnSe flakes on commonly used SiO2/Si insulating substrates using a straightforward two-step fabrication method in an atmospheric pressure quartz tube furnace system. The single-layer rectangular SnSe flakes with an average thickness of ~6.8 &#197; and lateral dimensions of about 30 &#181;m &#215; 50 &#181;m were fabricated by a combination of vapor transport deposition technique and nitrogen etching route. We characterized the morphology, microstructure, and electrical properties of the rectangular SnSe flakes and obtained excellent crystallinity and good electronic properties. This article about the two-step fabrication method can help researchers grow other similar two-dimensional, large-sized, single-layer materials using an atmospheric pressure system.

A protocol is presented demonstrating a two-step fabrication technique to grow large-sized single-layer rectangular shaped SnSe flakes on low-cost SiO2/Si dielectrics wafers in an atmospheric pressure quartz tube furnace system.

大型单层矩形 SnSe 片的常压制备

Tin selenide (SnSe) belongs to the family of layered metal chalcogenide materials with a buckled structure like phosphorene, and has shown potential for ...