Name: synthesis and functionalization of 3d nano-graphene materials: graphene aerogels and graphene macro assemblies
Uploaded: 2015-11-05T14:00:00.000+00:00
Duration: 10 min 23 s
Description: Watch this Scientific Journal Video about Synthesis and Functionalization of 3D Nano-graphene Materials: Graphene Aerogels and Graphene Macro Assemblies at JoVE.com

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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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?...

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><tbody><tr><td>Single Layer Graphene Oxide</td><td>Cheap Tubes</td><td>n/a</td><td>300-800&amp;#160;nm 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% NH&lt;sub&gt;3&lt;/sub&gt; 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?...

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

Universidad San Sebastian

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

A Technique to Functionalize and Self-assemble Macroscopic Nanoparticle-ligand Monolayer Films onto Template-free Substrates

This protocol describes a self-assembly technique to create macroscopic monolayer films composed of ligand-coated nanoparticles1,2. The simple, robust and scalable technique efficiently functionalizes metallic nanoparticles with thiol-ligands in a miscible water/organic solvent mixture allowing for rapid grafting of thiol groups onto the gold nanoparticle surface. The hydrophobic ligands on the nanoparticles then quickly phase separate the nanoparticles from the aqueous based suspension and confine them to the air-fluid interface. This drives the ligand-capped nanoparticles to form monolayer domains at the air-fluid interface.&#160; The use of water-miscible organic solvents is important as it enables the transport of the nanoparticles from the interface onto template-free substrates.&#160; The flow is mediated by a surface tension gradient3,4 and creates macroscopic, high-density, monolayer nanoparticle-ligand films.&#160; This self-assembly technique may be generalized to include the use of particles of different compositions, size, and shape and may lead to an efficient assembly method to produce low-cost, macroscopic, high-density, monolayer nanoparticle films for wide-spread applications.

A simple, robust and scalable technique to functionalize and self-assemble macroscopic nanoparticle-ligand monolayer films onto template-free substrates is described in this protocol.

一种技术，功能化和自组装纳米宏观 - 配体单层膜模板上无基材

This protocol describes a self-assembly technique to create macroscopic monolayer films composed of ligand-coated nanoparticles1,2. The simple, robust and ...

化学

Preparation of Carbon Nanosheets at Room Temperature

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

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

碳纳米片在室温下准备

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

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 ...

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

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

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

单壁碳纳米管与热可逆嵌段共聚物及表征功能化小角度中子散射

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

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We present methods for depositing and passively manipulating C60 molecules on rippled graphene that advance the pursuit of realizing applications involving 1D C60/graphene hybrid structures. The techniques applied in this exposition are geared towards high vacuum systems with preparation areas capable of supporting molecular deposition as well as thermal annealing of the samples. We focus on C60 deposition at low pressure using a homemade Knudsen cell connected to a scanning tunneling microscopy (STM) system. The number of molecules deposited is regulated by controlling the temperature of the Knudsen cell and the deposition time. One-dimensional (1D) C60 chain structures with widths of two to three molecules can be prepared via tuning of the experimental conditions. The surface mobility of the C60 molecules increases with annealing temperature allowing them to move within the periodic potential of the rippled graphene. Using this mechanism, it is possible to control the transition of 1D C60 chain structures to a hexagonal close packed quasi-1D stripe structure.

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Here we present a protocol for the fabrication of C60/graphene hybrid nanostructures by physical thermal evaporation. Particularly, the proper manipulation of deposition and annealing conditions allow the control over the creation of 1D and quasi 1D C60 structures on rippled graphene.

C 型60/石墨烯混合纳米结构的制备与表征

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We ...

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various precursor noble metal ions with reducing agents in a 1:1 (v/v) ratio results in the formation of metal gels within seconds to minutes compared to much longer synthesis times for other techniques such as sol-gel. Conducting the reduction step in a microcentrifuge tube or small volume conical tube facilitates a proposed nucleation, growth, densification, fusion, equilibration model for gel formation, with final gel geometry smaller than the initial reaction volume. This method takes advantage of the vigorous hydrogen gas evolution as a by-product of the reduction step, and as a consequence of reagent concentrations. The solvent accessible specific surface area is determined with both electrochemical impedance spectroscopy and cyclic voltammetry. After rinsing and freeze drying, the resulting aerogel structure is examined with scanning electron microscopy, X-ray diffractometry, and nitrogen gas adsorption. The synthesis method and characterization techniques result in a close correspondence of aerogel ligament sizes. This synthesis method for noble metal aerogels demonstrates that high specific surface area monoliths may be achieved with a rapid and direct reduction approach.

A rapid, direct solution-based reduction synthesis method to obtain Au, Pd, and Pt aerogels is presented.

直接溶液还原法快速合成金、钯、铂气凝胶的研究

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...

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 ...

Synthesis Method for Cellulose Nanofiber Biotemplated Palladium Composite Aerogels

Here, a method to synthesize cellulose nanofiber biotemplated palladium composite aerogels is presented. Noble metal aerogel synthesis methods often result in fragile aerogels with poor shape control. The use of carboxymethylated cellulose nanofibers (CNFs) to form a covalently bonded hydrogel allows for the reduction of metal ions such as palladium on the CNFs with control over both nanostructure and macroscopic aerogel monolith shape after supercritical drying. Crosslinking the carboxymethylated cellulose nanofibers is achieved using 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC) in the presence of ethylenediamine. The CNF hydrogels maintain their shape throughout synthesis steps including covalent crosslinking, equilibration with precursor ions, metal reduction with high concentration reducing agent, rinsing in water, ethanol solvent exchange, and CO2 supercritical drying. Varying the precursor palladium ion concentration allows for control over the metal content in the final aerogel composite through a direct ion chemical reduction rather than relying on the relatively slow coalescence of pre-formed nanoparticles used in other sol-gel techniques. With diffusion as the basis to introduce and remove chemical species into and out of the hydrogel, this method is suitable for smaller bulk geometries and thin films. Characterization of the cellulose nanofiber-palladium composite aerogels with scanning electron microscopy, X-ray diffractometry, thermal gravimetric analysis, nitrogen gas adsorption, electrochemical impedance spectroscopy, and cyclic voltammetry indicates a high surface area, metallized palladium porous structure.

A synthesis method for cellulose nanofiber biotemplated palladium composite aerogels is presented.The resulting composite aerogel materials offer potential for catalysis, sensing, and hydrogen gas storage applications.

纤维素纳米纤维生物模板复合气凝胶的合成方法

Here, a method to synthesize cellulose nanofiber biotemplated palladium composite aerogels is presented. Noble metal aerogel synthesis methods often ...

Synthesis of Graphene Nanofluids with Controllable Flake Size Distributions

A method for synthesizing graphene nanofluids with controllable flake size distributions is presented. Graphene nanoflakes can be obtained by the exfoliation of graphite in the liquid phase, and the exfoliation time is used to control the lower limits of the graphene nanoflake size distributions. Centrifugation is successfully used to control the upper limits of the nanoparticle size distributions. The objective of this work is to combine exfoliation and centrifugation to control the graphene nanoflake size distributions in the resulting suspensions.

A method for synthesizing graphene nanofluids with controllable flake size distributions is presented.

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

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