This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344. IM release LLNL-JRNL-667016.

1.间苯二酚 - 甲醛（RF）的衍生的石墨烯气凝胶<ol><li>的Na 2 CO 3催化碳气凝胶（11％固体，CRF） <ol><li>在40 ml的闪烁管中，去离子水（7.1毫升）加入到间苯二酚（0.625克，5.68毫摩尔）和混合在涡流1分钟。粉碎使用研钵和研杵之前水添加大间苯二酚件成粉末。需要注意的是，他们可能无法完全溶解，直到下一个步骤。 </li><li>添加37％甲醛溶液（为0.900克，11.4毫摩尔）的间苯二酚浆料，涡旋1分钟。 </li><li>添加碳酸钠（0.003克，0.028毫摩尔）至反应混合物中并涡旋1分钟。 </li><li>将反应混合物转移到玻璃模具可密封气密（例如，小瓶或载玻片是由硅酮垫圈隔开）限定了所得固体的一部分的形状。 </li><li>将密封的模具到一个80℃的烘箱，固化72小时。 </li><li>固化后，取出溶胶从玻璃模具和洗涤用水的id整料以除去残留的未反应的起始原料和催化剂。通常情况下，我们执行3×12小时冲洗用新鲜的DI H 2 O.该材料现在已准备好进行干燥。 </li></ol></li><li>醋酸催化碳气凝胶（AARF）17 <ol><li>在40 ml的闪烁管中，将去离子水（15毫升）加入间苯二酚（12.3克，0.112摩尔）和混合在涡流1分钟。粉碎使用研钵和研杵之前水添加大间苯二酚件成粉末。需要注意的是，他们可能无法完全溶解，直到下一个步骤。 </li><li>添加37％甲醛溶液（17.9克，0.224摩尔）的间苯二酚浆料，涡旋1分钟。 </li><li>加冰醋酸（0.44克，0.007摩尔）添加到反应混合物中，并涡旋混合1分钟。 </li><li>将反应混合物转移到玻璃模具可密封气密（例如，小瓶或载玻片是由一个硅胶垫片分开），它定义了地区环境部门一道的形状lting固体部分。 </li><li>将密封的模具到一个80℃的烘箱，固化72小时。 </li><li>固化后，从玻璃模具去除固体整料和用水冲洗以除去残留的未反应的起始原料和催化剂。通常情况下，我们执行3×12小时冲洗用新鲜的DI H 2 O.该材料现在已准备好进行干燥。 </li></ol></li><li>碳添加剂到RF前体溶液（CNT，GO） <ol><li>碳纳米管/ RF复合材料11 <ol><li>暂停1重量％的单壁碳纳米管在去离子水中，并使用超声波浴（声波功率90瓦，频率40千赫）完全分散。 </li><li>加入间苯二酚（1.235克，11.2毫摩尔），甲醛（1.791克，22.1毫摩尔）和碳酸钠催化剂（5.95毫克，0.056毫摩尔）至1.5g该CNT分散液。 </li><li>将反应混合物转移到玻璃模具可密封气密（例如，小瓶或载玻片是由一个硅胶垫片分开），这define是生成的固体部分的形状。 </li><li>将密封的模具到一个80℃的烘箱，固化72小时。 </li><li>固化后，从玻璃模具去除固体整料和用水冲洗以除去残留的未反应的起始原料和催化剂。通常执行3×12小时冲洗用新鲜的DI H 2 O.该材料现在已准备好进行干燥。 </li></ol></li><li>石墨烯氧化物/ RF复合材料12 <ol><li>暂停1％（重量）氧化石墨烯（GO，300-800纳米直径）在去离子水中，并用超声波浴（声功率90 W，频率40 kHz）的彻底散去。 </li><li>加入间苯二酚（1.235克，11.2毫摩尔），甲醛（1.791克，22.1毫摩尔，37％溶液）和碳酸钠催化剂（5.95毫克，0.056毫摩尔）至1.5克对GO分散体。 </li><li>将反应混合物转移到玻璃模具可密封气密（例如，小瓶或载玻片是由硅酮垫圈隔开）限定的形状产生的固体部分。 </li><li>将密封的模具到一个80℃的烘箱，固化72小时。 </li><li>固化后，从玻璃模具去除固体整料和用水冲洗以除去残留的未反应的起始原料和催化剂。通常执行3×12小时冲洗用新鲜的DI H 2 O.该材料现在已准备好进行干燥。 </li></ol></li></ol></li><li>干燥<ol><li>超临界CO 2 <ol><li>准备洗净的样品用超临界CO 2用丙酮交换H 2 O的溶剂干燥。从水浴中取出样品并放入干净的丙酮浴。更换新的丙酮两次在12小时的时间间隔。 </li><li>负载丙酮交换的样品成为超临界干燥装置，填充有丙酮中，用在12-15℃的循环冷却剂。 </li><li>密封超临界机和液态二氧化碳交换，直到没有丙酮遗体（4-24小时取决于Øn个采样的大小，密度，孔隙形态等 ）。 </li><li>切断的 CO 2的供应和提高循环的冷却剂至55℃的温度，同时保持压力在超临界干燥机1,200-1,600磅（80-110巴）之间。保持在55℃1小时。 </li><li>慢慢排气的 CO 2（2-12小时），同时保持循环冷却剂的温度在55℃。取出样品。 </li></ol></li><li>环境干燥（干凝胶） <ol><li>通过用丙酮交换H 2 O的溶剂制备洗过的样品在环境条件下干燥。从水浴中取出样品并放入干净的丙酮浴。更换新的丙酮两次在12小时的时间间隔。 </li><li>将丙酮交换的样品在一个干净的表面（ 如聚四氟乙烯块）。缓慢溶剂蒸发的速度，以防止开裂和收缩不均匀，覆盖的足够体积的倒烧杯，以提供充足的HEA的样品dSPACE的。 </li><li>允许溶剂蒸发为（24-72小时）。 </li></ol></li></ol></li><li>碳化<ol><li>在1050℃ 的 N 2气氛下进行干燥泡沫碳化 ​​。从室温斜以5℃/分钟的速度，并保持在1050℃下进行3小时。注意，薄样品可能需要被放置在两片石墨纸（或其他温度稳定，非反应性材料）之间，体重在上面，以防止卷曲和"土豆碎裂"。 </li></ol></li><li>激活<ol><li>激活AARF碳泡沫部件（2厘米×3厘米×4毫米，1.2克），以产生在950℃下进行5小时的流动的 CO 2（10标准立方厘米）根据3D纳米石墨烯（3D-NG）。7 </li></ol></li></ol> 2.氧化石墨烯衍生的石墨烯宏组件<ol><li> NH 4 OH催化GO总成<ol><li>在40 ml的闪烁管中，将去离子水（20毫升）添加至400mg单层石墨烯氧化氮E（GO，300-800纳米的直径）。彻底分散使用超声波浴（声功率90 W，频率40 kHz）的O / N。 </li><li>加浓NH 4 OH溶液（每克GO悬挂0.211毫升）。 </li><li>转移到玻璃模具可气密密封（例如，小瓶或玻璃是由硅酮密封垫，它定义所得到的固体部分的形状隔开幻灯片）。 </li><li>将密封的模具到一个80℃的烘箱，固化72小时。 </li><li>固化后，从玻璃模具去除固体整料和用水冲洗以除去残留的未反应的起始原料和催化剂。通常执行3×12小时冲洗用新鲜的DI H 2 O.该材料现在已准备好进行干燥。 </li></ol></li><li>干燥<ol><li>超临界CO 2 <ol><li>准备洗净的样品用超临界CO 2用丙酮交换H 2 O的溶剂干燥。从水浴中取出样品并放入浴合作ntaining干净丙酮。更换新的丙酮两次在12小时的时间间隔。 </li><li>负载丙酮交换的样品成为超临界干燥装置，填充有丙酮中，用在12-15℃的循环冷却剂。 </li><li>密封超临界干燥机与交流液态CO 2，直到没有丙酮遗体（4-24小时，取决于样品的大小，密度，孔隙形态等 ）。完整交换由停止丙酮滴在超临界干燥机的排气阀指示。 </li><li>切断的 CO 2的供应和提高循环的冷却剂至55℃的温度，同时保持压力在超临界干燥机1,200-1,600磅（80-110巴）之间。保持在55℃1小时。 </li><li>慢慢排气的 CO 2（2-12小时），同时保持循环冷却剂的温度在55℃。取出样品。 </li></ol></li><li>环境干燥（干凝胶） 注意，薄样品可能需要被放置之间用重量在顶部两个片特氟隆（或其他不粘材料），以防止卷曲和"土豆碎裂"。 <ol><li>通过用丙酮交换H 2 O的溶剂制备洗过的样品在环境条件下干燥。从水浴中取出样品并放入干净的丙酮浴。更换新的丙酮两次在12小时的时间间隔。 </li><li>将丙酮交换的样品在一个干净的表面（ 如聚四氟乙烯块）。缓慢溶剂蒸发的速度，以防止开裂和收缩不均匀，覆盖的足够体积的倒烧杯，以提供充足的顶空的样品。 </li><li>允许溶剂蒸发为（24-72小时）。 </li></ol></li></ol></li><li>碳化<ol><li>在1050℃ 的 N 2气氛下进行干燥泡沫碳化 ​​。从室温斜以5℃/分钟的速度，并保持在1050℃下进行3小时。注意，薄样品可能需要被放置b切口白内障手术挽二与重量上顶片的石墨纸（或其他温度稳定的，非反应性材料），以防止卷曲和"土豆碎裂"。 </li><li>热退火高度结晶GMA。执行泡沫炭化温度的附加热处理高达He气氛下，2500℃。从室温斜以100℃/分钟的速度，并保持在升高的温度下进行1小时。 </li></ol></li><li>后炭化功能化<ol><li>非共价蒽醌官能化（AQ-GMA） <ol><li>准备蒽醌（AQ）在干乙醇为3毫米的解决方案。热在密封小瓶中在75℃以确保完全溶解。 </li><li>加热AQ溶液到GMA样品（〜2毫升/样品的毫克）。浸泡在密封小瓶中进行2小时，在75℃。 </li><li>从瓶中取出多余的AQ的解决方案，让样品干燥，在75°CO / N（瓶盖关闭）。 </li></ol></li></ol></li></ol>

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A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultra-Low+Density,+Monolithic+WS2,+MoS2,+and+MoS2+Graphene+Aerogels.">Ultra-Low Density, Monolithic WS2, MoS2, and MoS2 Graphene Aerogels.</a> ACS Nano. 9 (5), 4698-4705 (2015).</li></ol>

The authors have nothing to disclose.

需要注意的是这里描述的程序是唯一的代表是重要的。许多调整是可能的调整材料用于特定应用。例如，改变起始材料的浓度，同时保持间苯二酚/甲醛（RF）的比率恒定，可以对最终材料的密度产生影响。催化剂负载可以改变孔结构，作为一个较高的负荷在RF过程导致更小的一次颗粒，反之亦然。激活时能起到一定作用，以​​及;在更短的激活时间，新的孔隙率在微孔的形式产生的，而在较长的激活时间微孔扩大至交叉微孔中孔边界尺寸15。另外，在激活时间必须考虑到原料碳泡沫的重量计。从上述的激活处理典型收率长约 25％-30％，基于起始碳泡沫的重量。 <p clasS ="jove_content"&gt;同样类型的调整可以对于添加剂如碳纳米管和GO到RF起始溶液。使用上述的普通技术中，泡沫材料的CNT负载量范围为0〜60重量％（相对于射频固体）制备。实现这种方法的最高电导率石墨烯气凝胶使用1重量％的GO和4％（重量）的射频在最初的反应混合物;使用较高的RF的:GO比率导致较低电导率值。石墨烯macroassemblies一般仅限于≤20毫克/毫升初始浓度，因为它是难以达到稳定的悬浮液在较高浓度;小于10毫克悬浮液/毫升仍然会形成整体结构，然而，它们大大收缩固化时和碳化制备很低密度的材料难以达到通过单独初始浓度。 炭化温度还提供了材料调整的机会。电导率增加š大大高于800℃的基于RF的材料。在碳化温度高于1500℃，GMAS失去表面积并且变得更加石墨，随着在石墨烯片更少的缺陷。 在对比中上述材料的合成的灵活性，我们发现，官能化的GMA材料蒽醌，增加的浓度和更长的时的保温时间不导致更高的AQ负载。这可以归因于大致单层AQ覆盖面，超出与GMA衬底第一缺乏稳定范德华相互作用层。 合成协议未来的应用在这里描述的包括并入牺牲模板为材料制作，以确定大孔隙和优化质量传输，例如，液流电池的电极，18,19工作也正在进行制定的RF，去与先进制造业的兼容性前体解决方案（3D打印）技术，如直接墨水书写和投影microstereo光刻技术。20最后，我们将继续基于三维石墨烯支架，以开发新的复合材料。21

由于石墨烯的在2004年的隔离，在利用其独特的性能1兴趣已经导致朝向组装石墨烯强烈的努力成保持单个的石墨烯片的特性的立体感，整体结构。2-5这些努力受到阻碍的事实上，石墨烯本身是昂贵的和耗时的，以产生并倾向于聚集在溶液中，这限制了基于石墨烯积木材料的可伸缩性。另外，石墨烯组件典型地包括单个的石墨烯片材之间的物理交联的互动（例如，范德华力），这是更导电的和比化学键交联机械坚固的。劳伦斯·利弗莫尔国家实验室曾参与新型多孔，低密度的碳材料的开发，因为20世纪80年代。6几种策略已经确定制作质量，机生产线从两个低成本聚合物衍生的碳泡沫材料，这是所谓的石墨烯气凝胶（气），7以及通过直接交联的石墨烯氧化物的（GO）片，埚基于石墨烯的单片散装材料被称为石墨烯宏观组件（GMAS）。8,9-这些超高表面积散装材料具有高电导率和热导，优异的机械强度和弹性，以及可调孔隙形态。气体和GMAS发现实用程序在许多应用中，包括在超级电容器的电极材料和可再充电电池，先进的催化剂载体，吸附剂，热绝缘，传感器和脱盐。10 石墨烯气凝胶的合成与间苯二酚和甲醛的水溶液溶胶 - 凝胶聚合开始产生高度交联的有机凝胶。这些凝胶用水和丙酮洗涤，然后干燥使用超临界的 CO 2和热解中的inert气氛，得到碳气凝胶具有相对低的表面积和孔体积。碳气凝胶是由控制除去温和氧化条件下碳原子的活化（例如，CO 2），以形成无定形碳和石墨纳米片组成的交联材料，具有较高的表面积，开放的孔结构。7的一个独特的优点溶胶 - 凝胶合成的是，气体可以被制造成各种形式，包括整料和薄膜，这取决于应用的需要。碳纳米管11和/或石墨烯片12可以通过包括这些添加剂中的溶胶-凝胶前体溶液被整合到气体。这产生在其中添加剂成为主碳网络结构的一部分的复合结构。此外，遗传算法的框架可以官能碳化/活化之后或者通过气凝胶表面的修饰或通过材料的沉积，例如催化剂纳米颗粒，上框架结构13 石墨烯宏组件（GMAS）由制备直接交联悬浮石墨烯氧化物（GO）片，利用其固有的化学功能方面具有优势。9 GO片含有多种官能团，包括环氧化物和氢氧化物的部分，可以作为化学交联位点。正如GA准备，组装GMAS是超临界干燥，保持多孔网络，再热解，以减少化学交联成提供的组装结构支撑导电碳桥梁。由于石墨烯片之间的共价碳桥，GMAS具有电导率和机械刚度是幅度比与物理交联形成的石墨烯组件更高的数量级。此外，GMAS具有接近单个石墨烯片的理论值的表面区域。后期合成热牛逼reatment在升高的温度（&gt; 1050℃）能显著改善GMAS的结晶，导致甚至更高的传导性和杨氏模量以及更好的耐热氧化性。GMAS 14后合成的化学治疗与氧化还原活性的有机分子，如蒽醌可以增强电荷存储容量在超级电容器的应用。15 气体和GMAS的可调材料性质，部分的仔细改变合成条件，如试剂和催化剂浓度，固化时间和温度，干燥条件，和碳化/活化处理的结果。16此细节视频协议旨在解决歧义在公开的方法，并引导研究者试图再现材料和条件。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Single Layer Graphene Oxide</td>
			<td>Cheap Tubes</td>
			<td>n/a</td>
			<td>300-800nm XY dimensions</td>
		</tr>
		<tr>
			<td>single wall carbon nano tubes (SWCNTs)</td>
			<td>Carbon Solutions</td>
			<td>P2-SWNT</td>
			<td></td>
		</tr>
		<tr>
			<td>resorcinol</td>
			<td>aldrich</td>
			<td>398047-500G</td>
			<td></td>
		</tr>
		<tr>
			<td>37% formaldehyde solution in water</td>
			<td>aldrich</td>
			<td>252549</td>
			<td></td>
		</tr>
		<tr>
			<td>acetic acid</td>
			<td>aldrich</td>
			<td>320099</td>
			<td></td>
		</tr>
		<tr>
			<td>ammonium hydroxide solution 28-30% NH3 basis</td>
			<td>aldrich</td>
			<td>320145</td>
			<td></td>
		</tr>
		<tr>
			<td>sodium carbonate</td>
			<td>aldrich</td>
			<td>791768</td>
			<td></td>
		</tr>
		<tr>
			<td>anthraquinone</td>
			<td>aldrich</td>
			<td>a90004</td>
			<td></td>
		</tr>
		<tr>
			<td>Polaron supercritical dryer</td>
			<td>Electron Microscopy Sciences</td>
			<td>EMS 3100</td>
			<td>this is a representative model, any critical point dryer compatible with acetone should work</td>
		</tr>
	</tbody>
</table>

synthesis and functionalization of 3d nano-graphene materials: graphene aerogels and graphene macro assemblies

努力组装石墨成三维整体结构而受到阻碍的高成本和石墨烯的加工性差。此外，大多数报道的石墨烯组件被一起通过物理相互作用（例如，范德华力），而不是化学键，这限制了它们的机械强度和导电性保持。此视频的方法的细节最近开发战略，制造大量生产，石墨烯基无论从聚合物泡沫材料或单层氧化石墨烯衍生的散装物料。这些材料主要包括通过共价键合的碳的接头连接单个的石墨烯片。它们保持石墨烯的有利性质，例如高表面积和高导电和导热性，并结合可调孔隙形态和优异的机械强度和弹性。这种灵活的合成方法可以扩展到聚合物/碳纳米管（CNT）的制造ð聚合物/氧化石墨烯（GO）复合材料。此外，附加的后合成官能与蒽醌被描述，这使得在超级电容器应用中电荷存储性能的显着增加。

材料组成和形态的制造过程中的演化可以跟踪各种方式，包括X-射线衍射，喇曼和NMR光谱法，电子显微镜，和孔度计。例如，在合成，热解和CO 2的活化气体中，转化率，接着通过X射线衍射（XRD）（图1E）。由于没有在激活（蓝色迹线）后的X射线衍射图案的堆叠相关（002）衍射峰的表示从含纳米石墨片的一个选自由单层石墨烯的结构的过渡。扫描电子显微镜（SEM）和高分辨透射电子显微镜（HRTEM）揭示短，线性特征，这可能被识别为观察边缘上（图1C 和 D）单个的石墨烯片。拉曼特征为GA类似于观察通过化学气相沉积生长的商业石墨烯样品（图1F）。固态核磁共振（NMR）来跟随GO为转化的GMA（图2），9揭示了显著环氧化物和羟基官能度（50和75ppm的之间的峰值），以及羰基（168 ppm的）在它的13 C NMR谱在固化后基本消除，和脂族碳峰（26 ppm的）出现，这表明环氧化物和羟基都参与了交联机制。后热解/碳化，只有藻2碳峰遗体和1 H NMR谱（图2B）也示出了消除-CH 2 -和-CH 2 O-基团表明SP3碳交联进行热转换为导电SP 2碳结。该GMA微观结构用SEM进行分析，并出现类似报道在其他石墨烯组装（ 图3 </strong&gt;的信息）。 在图4A中所示的氮孔隙吸附/解吸等温线是IV型，表示中孔材料构成。 GMA的交与蒽醌的合成修饰的特点是热重分析（TGA）， 与图5B和 C呈现代表等温线。的质量损失曲线的衍生物显示出在不同温度下的AQ-GMA和散装AQ峰由于碳基板上的AQ分子的吸附。电化学表征包括循环伏安（CV），这表明AQ吸附到GMA电极产生的可逆且稳定法拉第电荷存储（图6A）。 <img alt="图1" src="/files/ftp_upload/53235/53235fig1.jpg" /> 图1.处理及3D-NG（GA）的架构的聚合物基（A）示意图自上而下的方法。 （B）图一厘米大小的3D-NG样品的机械强度的。 （C）的微米级孔隙和韧带组成的开放式大孔网络结构。 （ 四）韧带弯曲和交织石墨烯片组成的内部结构。选定的双层区域由椭圆标出，和过这样的双层区域一个典型的强度分布示出在左侧。 （E）的X射线衍射数据证实了最初的多层石墨烯组分与一个由单层石墨烯为主的转变。 （ 六）从3D-NG和多项层石墨烯的D / G带区的拉曼光谱的比较。这个数字已经被修改参考。 7. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53235/53235fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 薄页="总是"&gt; <img alt="图2" src="/files/ftp_upload/53235/53235fig2.jpg" /> GMA装配和热加工期间图2. NMR表征。（A）的13 C NMR谱为GO粉末，GO初始凝胶化后，和三维石墨烯macroassembly。 （B）的前和热处理后1 H NMR光谱的GMA。这个数字已经被修改参考。 9. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53235/53235fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" src="/files/ftp_upload/53235/53235fig3.jpg" /> 图3.三维石墨烯macroassembly的断裂面的FE-SEM图像。（A）低倍。 （二）高放大倍率。这个数字已经被修改参考。 9。S://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53235/53235fig3large.jpg"目标="_空白"&gt;点击此处查看该图的放大版本。 <img alt="图4" src="/files/ftp_upload/53235/53235fig4.jpg" /> 图4.孔结构GMAS的。（A）氮吸附/脱附等温线。 （B）的孔径分布。这个数字已经被修改参考。 9. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53235/53235fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图5" src="/files/ftp_upload/53235/53235fig5.jpg" /> 图5.合成和AQ-GMAS表征。（A）的合成过程和GMA的电极非共价AQ官能化示意图。 （B </strong&gt; 250毫米厚的AQ-GMA盘）的TGA曲线与11.2％（重量）的AQ加载总质量的（10.1％）和（C）的TGA曲线。散装AQ（氩流10 ml的分钟-1，10℃分钟-1温度匝道）。衍生物的质量损失曲线（虚线）在不同温度下对所述的AQ-GMA与散装的AQ显示峰。超过60℃的较高的温度表示吸附在碳基板上的AQ分子。这个数字已经被修改参考。 15. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53235/53235fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图6" src="/files/ftp_upload/53235/53235fig6.jpg" /> 图6.电化学性能AQ-GMAS的。（A）循环伏安（2毫伏秒 -1，1 M盐酸）250毫米厚的GMA磁盘，为准备（实丽ね）中，用12.4重量％的AQ加载（虚线）。 （ 二）个人简历在不同电位的扫描速率相同的12.4％（重量）AQ-GMA样品。插图剧情说明，AQ贡献充电存储容量保持不变，直到&gt; 60毫伏秒-1，其中溶液电阻引起如此大的超电势的AQ不能完全施加的电压范围内进行充电。 （能力值，推导出通过整合与AQ相关的排放峰值，并减去基本GMA的能力。）这个数字已经被修改参考。 15. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53235/53235fig6large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

Watch this Scientific Journal Video about Synthesis and Functionalization of 3D Nano-graphene Materials: Graphene Aerogels and Graphene Macro Assemblies at JoVE.com

Synthesis and Functionalization of 3D Nano-graphene Materials: Graphene Aerogels and Graphene Macro Assemblies

This video method describes the synthesis of high surface area, monolithic 3D graphene-based materials derived from polymer precursors as well as single layer graphene oxide.

合成和3D纳米石墨烯材料的功能化:石墨烯气凝胶和石墨烯宏组件

Efforts to assemble graphene into three-dimensional monolithic structures have been hampered by the high cost and poor processability of graphene. ...

synthesis-functionalization-3d-nano-graphene-materials-graphene

Nanyang Technological University

Research

JoVE Journal

Engineering

14.1K 次观看.  Lawrence Livermore National Laboratory. This video method describes the synthesis of high surface area, monolithic 3D graphene-based materials derived from polymer precursors as well as single layer graphene oxide.

视频: Synthesis and Functionalization of 3D Nano-graphene Materials: Graphene Aerogels and Graphene Macro Assemblies

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 ...

科研

工程学

Novel 3D/VR Interactive Environment for MD Simulations, Visualization and Analysis

The increasing development of computing (hardware and software) in the last decades has impacted scientific research in many fields including materials science, biology, chemistry and physics among many others. A new computational system for the accurate and fast simulation and 3D/VR visualization of nanostructures is presented here, using the open-source molecular dynamics (MD) computer program LAMMPS. This alternative computational method uses modern graphics processors, NVIDIA CUDA technology and specialized scientific codes to overcome processing speed barriers common to traditional computing methods. In conjunction with a virtual reality system used to model materials, this enhancement allows the addition of accelerated MD simulation capability. The motivation is to provide a novel research environment which simultaneously allows visualization, simulation, modeling and analysis. The research goal is to investigate the structure and properties of inorganic nanostructures (e.g., silica glass nanosprings) under different conditions using this innovative computational system. The work presented outlines a description of the 3D/VR Visualization System and basic components, an overview of important considerations such as the physical environment, details on the setup and use of the novel system, a general procedure for the accelerated MD enhancement, technical information, and relevant remarks. The impact of this work is the creation of a unique computational system combining nanoscale materials simulation, visualization and interactivity in a virtual environment, which is both a research and teaching instrument at UC Merced.

A new computational system featuring GPU-accelerated molecular dynamics simulation and 3D/VR visualization, analysis and manipulation of nanostructures has been implemented, representing a novel approach to advance materials research and promote innovative investigation and alternative methods to learn about material structures with dimensions invisible to the human eye.

新颖的3D / VR互动环境MD模拟，可视化和分析

The increasing development of computing (hardware and software) in the last decades has impacted scientific research in many fields including materials ...

Development of a 3D Graphene Electrode Dielectrophoretic Device

The design and fabrication of a novel 3D electrode microdevice using 50 &#181;m thick graphene paper and 100 &#181;m double sided tape is described. The protocol details the procedures to construct a versatile, reusable, multiple layer, laminated dielectrophoresis chamber. Specifically, six layers of 50 &#181;m x&#160;0.7 cm x&#160;2 cm graphene paper and five layers of double sided tape were alternately stacked together, then clamped to a glass slide. Then a 700 &#956;m diameter micro-well was drilled through the laminated structure using a computer-controlled micro drilling machine. Insulating properties of the tape layer between adjacent graphene layers were assured by resistance tests. Silver conductive epoxy connected alternate layers of graphene paper and formed stable connections between the graphene paper and external copper wire electrodes. The finished device was then clamped and sealed to a glass slide. The electric field gradient was modeled within the multi-layer device. Dielectrophoretic behaviors of 6 &#956;m polystyrene beads were demonstrated in the 1 mm deep micro-well, with medium conductivities ranging from 0.0001 S/m to 1.3 S/m, and applied signal frequencies from 100 Hz to 10 MHz. Negative dielectrophoretic responses were observed in three dimensions over most of the conductivity-frequency space and cross-over frequency values are consistent with previously reported literature values. The device did not prevent AC electroosmosis and electrothermal flows, which occurred in the low and high frequency regions, respectively. The graphene paper utilized in this device is versatile and could subsequently function as a biosensor after dielectrophoretic characterizations are complete.

A microdevice with high throughput potential is used to demonstrate three-dimensional (3D) dielectrophoresis (DEP) with novel materials. Graphene nanoplatelet paper and double sided tape were alternately stacked; a 700 &#956;m micro-well was drilled transverse to the layers. DEP behavior of polystyrene beads was demonstrated in the micro-well.

三维石墨电极介电泳装置的研制

The design and fabrication of a novel 3D electrode microdevice using 50 &#181;m thick graphene paper and 100 &#181;m double sided tape is described. The ...

Fabrication of Gate-tunable Graphene Devices for Scanning Tunneling Microscopy Studies with Coulomb Impurities

Owing to its relativistic low-energy charge carriers, the interaction between graphene and various impurities leads to a wealth of new physics and degrees of freedom to control electronic devices. In particular, the behavior of graphene&#8217;s charge carriers in response to potentials from charged Coulomb impurities is predicted to differ significantly from that of most materials. Scanning tunneling microscopy (STM) and scanning tunneling spectroscopy (STS) can provide detailed information on both the spatial and energy dependence of graphene&#39;s electronic structure in the presence of a charged impurity.&#160;The design of a hybrid impurity-graphene device, fabricated using controlled deposition of impurities onto a back-gated graphene surface, has enabled several novel methods for controllably tuning graphene&#8217;s electronic properties.1-8 Electrostatic gating enables control of the charge carrier density in graphene and the ability to reversibly tune the charge2 and/or molecular5 states of an impurity. This paper outlines the process of fabricating a gate-tunable graphene device decorated with individual Coulomb impurities for combined STM/STS studies.2-5 These studies provide valuable insights into the underlying physics, as well as signposts for designing hybrid graphene devices.

This paper details the fabrication process of a gate-tunable graphene device, decorated with Coulomb impurities for scanning tunneling microscopy studies. Mapping the spatially dependent electronic structure of graphene in the presence of charged impurities unveils the unique behavior of its relativistic charge carriers in response to a local Coulomb potential.

对于扫描隧道显微学与库仑杂质制造门可调谐石墨烯器件

Owing to its relativistic low-energy charge carriers, the interaction between graphene and various impurities leads to a wealth of new physics and degrees ...

Visible-light Induced Reduction of Graphene Oxide Using Plasmonic Nanoparticle

Present work demonstrates the simple, chemical free, fast, and energy efficient method to produce reduced graphene oxide (r-GO) solution at RT using visible light irradiation with plasmonic nanoparticles. The plasmonic nanoparticle is used to improve the reduction efficiency of GO. It only takes 30 min&#160;at RT by illuminating the solutions with Xe-lamp, the r-GO solutions can be obtained by completely removing gold nanoparticles through simple centrifugation step. The spherical gold nanoparticles (AuNPs) as compared to the other nanostructures is the most suitable plasmonic nanostructure for r-GO preparation. The reduced graphene oxide prepared using visible light and AuNPs was equally qualitative as chemically reduced graphene oxide, which was supported by various analytical techniques such as UV-Vis spectroscopy, Raman spectroscopy, powder XRD and XPS. The reduced graphene oxide prepared with visible light shows excellent quenching properties over the fluorescent molecules modified on ssDNA and excellent fluorescence recovery for target DNA detection. The r-GO prepared by recycled AuNPs is found to be of same quality with that of chemically reduced r-GO. The use of visible light with plasmonic nanoparticle demonstrates the good alternative method for r-GO synthesis.

A simple protocol for the preparation of reduced graphene oxide using visible light and plasmonic nanoparticle is described.

可见光诱导的还原氧化石墨烯的使用电浆纳米粒子

Present work demonstrates the simple, chemical free, fast, and energy efficient method to produce reduced graphene oxide (r-GO) solution at RT using ...

Strain Sensing Based on Multiscale Composite Materials Reinforced with Graphene Nanoplatelets

The electrical response of NH2-functionalized graphene nanoplatelets composite materials under strain was studied. Two different manufacturing methods are proposed to create the electrical network in this work: (a) the incorporation of the nanoplatelets into the epoxy matrix and (b) the coating of the glass fabric with a sizing filled with the same nanoplatelets. Both types of multiscale composite materials, with an in-plane electrical conductivity of ~10-3 S/m, showed an exponential growth of the electrical resistance as the strain increases due to distancing between adjacent functionalized graphene nanoplatelets and contact loss between overlying ones. The sensitivity of the materials analyzed during this research, using the described procedures, has been shown to be higher than commercially available strain gauges. The proposed procedures for self-sensing of the structural composite material would facilitate the structural health monitoring of components in difficult to access emplacements such as offshore wind power farms. Although the sensitivity of the multiscale composite materials was considerably higher than the sensitivity of metallic foils used as strain gauges, the value reached with NH2 functionalized graphene nanoplatelets coated fabrics was nearly an order of magnitude superior. This result elucidated their potential to be used as smart fabrics to monitor human movements such as bending of fingers or knees. By using the proposed method, the smart fabric could immediately detect the bending and recover instantly. This fact permits precise monitoring of the time of bending as well as the degree of bending.

The integration of conductive nanoparticles, such as graphene nanoplatelets, into glass fiber composite materials creates an intrinsic electrical network susceptible to strain. Here, different methods to obtain strain sensors based on the addition of graphene nanoplatelets into the epoxy matrix or as a coating on glass fabrics are proposed.

基于多尺度复合材料的增强与石墨烯纳米片应变传感

The electrical response of NH2-functionalized graphene nanoplatelets composite materials under strain was studied. Two different manufacturing methods are ...

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 ...

Bulk and Thin Film Synthesis of Compositionally Variant Entropy-stabilized Oxides

Here, we present a procedure for the synthesis of bulk and thin film multicomponent (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O (Co variant) and (Mg0.25(1-x)Co0.25(1-x)Ni0.25(1-x)CuxZn0.25(1-x))O (Cu variant) entropy-stabilized oxides. Phase pure and chemically homogeneous (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O (x = 0.20, 0.27, 0.33) and (Mg0.25(1-x)Co0.25(1-x)Ni0.25(1-x)CuxZn0.25(1-x))O (x = 0.11, 0.27) ceramic pellets are synthesized and used in the deposition of ultra-high quality, phase pure, single crystalline thin films of the target stoichiometry. A detailed methodology for the deposition of smooth, chemically homogeneous, entropy-stabilized oxide thin films by pulsed laser deposition on (001)-oriented MgO substrates is described. The phase and crystallinity of bulk and thin film materials are confirmed using X-ray diffraction. Composition and chemical homogeneity are confirmed by X-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy. The surface topography of thin films is measured with scanning probe microscopy. The synthesis of high quality, single crystalline, entropy-stabilized oxide thin films enables the study of interface, size, strain, and disorder effects on the properties in this new class of highly disordered oxide materials.

The synthesis of high quality bulk and thin film (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O and (Mg0.25(1-x)Co0.25(1-x)Ni0.25(1-x)CuxZn0.25(1-x))O entropy-stabilized oxides is presented.

组分变熵稳定氧化物的体积和薄膜合成

Here, we present a procedure for the synthesis of bulk and thin film multicomponent (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O (Co variant) and ...

Fabrication of Three-Dimensional Graphene-Based Polyhedrons via Origami-Like Self-Folding

The assembly of two-dimensional (2D) graphene into three-dimensional (3D) polyhedral structures while preserving the graphene's excellent inherent properties has been of great interest for the development of novel device applications. Here, fabrication of 3D, microscale, hollow polyhedrons (cubes) consisting of a few layers of 2D graphene or graphene oxide sheets via an origami-like self-folding process is described. This method involves the use of polymer frames and hinges, and aluminum oxide/chromium protection layers that reduce tensile, spatial, and surface tension stresses on the graphene-based membranes when the 2D nets are transformed into 3D cubes. The process offers control of the size and shape of the structures as well as parallel production. In addition, this approach allows the creation of surface modifications by metal patterning on each face of the 3D cubes. Raman spectroscopy studies show the method allows the preservation of the intrinsic properties of the graphene-based membranes, demonstrating the robustness of our method.

Fabrication of Three-Dimensional Graphene-Based Polyhedrons via Origami-Like Self-Folding

Here, we present a protocol for fabrication of 3D graphene-based polyhedrons via origami-like self-folding.

基于折纸式自折叠的三维石墨烯正多面体的制备

The assembly of two-dimensional (2D) graphene into three-dimensional (3D) polyhedral structures while preserving the graphene's excellent inherent ...

Preparation of Graphene Liquid Cells for the Observation of Lithium-ion Battery Material

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between two graphene sheets, and the facile synthesis of one-dimensional nanostructures using electrospinning. The GLC enables in situ transmission electron microscopy (TEM) for the lithiation dynamics of electrode materials. The in situ GLC-TEM using an electron beam for both imaging and lithiation can utilize not only realistic battery electrolytes, but also the high-resolution imaging of various morphological, phase, and interfacial transitions.

Here, we present a protocol for the fabrication and preparation of a graphene liquid cell for in situ transmission electron microscopy observation, along with a synthesis of electrode materials and electrochemical battery cell tests.

锂离子电池材料用石墨烯液位的制备

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between ...