この作業は、NSFキャリアアワード番号0954345によってサポートされていました。

1。窒素ドープカーボンナノチューブカップのCVD合成（NCNCs） NCNCsは、液体前駆体（ 図1A）を使用して、石英基板上に化学蒸着（CVD）法を用いて合成した。 <ol><li>反応室としてリンドバーグ/ブルーチューブ炉で3フィート長い石英管（2.5センチid）を置きます。製品回収のための基質として管内の石英板（1 &quot;×12&quot;）を置きます。気体と液体注入接続/チューブを内蔵した自家製のステンレス鋼のキャップを使用して石英管を密封。 </li><li> 0.75重量％フェロセン、10重量％アセトニトリル及び89.25重量％のキシレンを含有する液体前駆体の溶液を作製。成長する前に、石英管への入口に接続されたガスタイトシリンジに液体前駆体の約5mlを描く。シリンジポンプに注射器を置きます。 </li><li> CVD装置を組み立てます。すべてのガス入口と出口を接続します。流れAR（845 SCCM）はCVD装置をパージ、漏れたちをチェックするINGは液漏れ検出器をスヌープ。 20分間パージした後、H 2をオンにします。 127 SCCMへのH 2から37.5 SCCMとArの流量を設定する。炉の電源をオンにします。 800炉の温度を設定し、それが800°で安定するまでCと待つ℃の</li><li>石英管に液体前駆体を注入するシリンジポンプを使用してください。インジェクタチューブのデッドボリュームを埋めるために6分間9ミリリットル/時間で注入速度を設定します。その後NCNCsの成長のための1ミリリットル/時に注入速度を下げてください。成長の90分後、シリンジポンプとH 2ガス流量をオフにし、炉をシャットダウンします。 Arは、炉を室温まで冷却されるまで不活性雰囲気を維持するために、流れを維持する。 </li><li>すべてのガス入口と出口、および噴射システムを取り外します。 CVD装置を分解し、石英板を取り出す。石英板からNCNCsフィルム剥離に一方的なカミソリの刃を使用してください。エタノールに収集した生成物を分散させる。呼吸器保護INHを防止するために必要とされる作業がヒュームフードの外側に行われる場合に可能な炭素材料を一直線に並ん。 </li></ol> 2。酸の混合物によって合成されたままのNCNCsの酸化<ol><li> 200ミリリットルの丸底フラスコに合成されたままのNCNCs約10mgを転送します。フラスコに、濃HNO 3の7.5ミリリットルを追加します。簡単に言えば、より良い分散水浴中混合物を超音波処理。その後徐々に濃H 2 SO 4の22.5ミリリットルを追加します。 （ 注意：強い酸混合物は非常に腐食性であり、慎重に安全保護機能を備えたこれらの酸を処理します。）4時間室温で水浴中で反応混合物を超音波処理。 </li><li>氷浴中で冷却しながら100mlの水で反応混合物を希釈する。水吸引器を使用して220ナノメートルの細孔径を有するポリテトラフルオロエチレン（PTFE）膜を介して混合物をフィルタリングする。 </li><li>任意の酸性残留副産物を除去するために0.01 M NaOH溶液200mlでフィルター膜上に材料を洗って18はその後洗うろ液のpHが中性が達成されるまで0.01 M HCl溶液200mlで、多量の水を行った。超音波処理によって水（20ml）で得られた物質（酸化NCNCs）を分散させる。得られた懸濁液を、さらなる実験を室温で保存することができる。 </li></ol> 3。プローブ先端の超音波処理によってNCNCsを物理的に分離<ol><li>氷浴に入れた100mlのプラスチックカップに水中で酸化NCNCsの懸濁物を移す。水で50ミリリットルマークにプラスチックカップを埋める。 60％最大の大きさ（12 W）で1/4 &quot;径のチタンマイクロチップを搭載したプローブ先端ソニケータを設定します。水没、ソリューション、その後30秒のオン/オフの間隔で12時間のプロセスの中心にマイクロチップ。変更氷の過熱を防ぐため、30分ごと。 </li><li>超音波処理を停止します。任意の大きな粒子を除去するために220 nmの細孔サイズのPTFEフィルター膜を通してNCNCサスペンションをフィルタリング。結果NCNCサンプルは、さらにアプリケーションのためのRTで保存することができます。 </lI&gt; <li> （オプション）比較実験として、DMFのような合成NCNCsの別のサンプルを分散し、直接上記と同じ設定で12時間、プローブ先端超音波処理とサスペンションを超音波処理。 </li></ol> 4。カイザー試験によるNCNCs上のアミン官能基の定量分析<ol><li>試薬を準備します。ミックスフェノール1gをし、EtOH250μlのをピリジン2.5mlに、混合物にH 2 O中0.01 M hydrindantin50μlのを追加します。試薬Bを準備のEtOH 1mlにニンヒドリン（50 mg）を溶解する。 </li><li>微量天秤上NCNCsサンプル（〜0.5 mg）を秤量3:2のEtOH /小さな試験管内の水1mlにそれらを分散させる。試料懸濁液に試薬Bの試薬と25μlを100μlのを追加します。 parafilmsで試験管を密封し、10分間100℃のオイルバスで混合物を加熱する。固体粒子を除去し、ろ液を収集するためのフィルタ、シリンジを通してサンプルをフィルタリング。 </li><li> FILに可視スペクトルを取るNCNCsを追加せずに同じプロセスで作られたブランク試料で比色分析用TRATE。 570nmで中心ピークの吸光度を記録し、ランベルト·ベールの法則によるとアミン負荷を計算します。 </li></ol> 5。 GNPSとNCNCsの機能化<ol><li>均一な分散を達成するために5分間水浴超音波処理を用いて分離NCNCs（0.01 mg / mlの）を含む水性懸濁液4mlの超音波処理。 </li><li>超音波処理中にNCNC懸濁液へのHAuCl 4水溶液1ミリリットル（1 mg / mlの）を追加します。その後、1重量％クエン酸三ナトリウム水溶液を滴下250μlのを追加します。精力的に反応混合物を2時間ホットプレート上で70℃であったかき混ぜる。 </li><li> 15分間3,400 rpmで反応混合物を遠心分離。沈殿物にGNPSで官能NCNCsを収集し、遠心分離により水で洗う。水中での沈殿（4 ml）を分散させる。 </li></ol>

<ol>
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著者らは競合する経済的利益を宣言しません。

実験の主な目的は、効果的に窒素をドープしたカーボンナノチューブから黒鉛nanocupsを生成することであった。しかし、CVD合成の窒素ドーピングは積み重ねカップ状構造の形成を保証するものではありません。前駆体及びその他の成長条件の化学組成に応じて、得られた生成物の形態は多くを変化させてもよい。窒素源の濃度が19の構造に影響を及ぼす主要な要因であるため、中の窒?...

その固有の内側空洞と多彩な表面化学、中空炭素系ナノ材料は、カーボンナノチューブ（CNT）などで薬物送達用途において良好なナノキャリアであると考えられる。1,2しかし、自然のままのCNTのフィブリル構造は中空ではなく、アクセス不能有するインテリアとは、重度の炎症反応および生物系における細胞毒性効果を引き起こすことがある。3,4窒素がドープされたCNTは、一方で、アンドープ多層カーボンナノチューブ（MWCNTの）5,6よりも高い生体適合性を有することが見出されており、良好な薬剤を有してもよい配信性能。 7,8は、アクセス可能なインテリアと200 nmの下に典型的な長さと個々の窒素ドープカーボンナノチューブカップ（NCNCs）を得るために外に分離することができ、積層カップに似た区画中空構造のナノチューブグラファイト格子の結果に窒素原子のドーピングとさらに化学物質を可能に窒素の機能官能化は、これらの個々の黒鉛カップは、薬物送達用途のために非常に有利である。 アーク放電9とDCマグネトロンスパッタリングを含む窒素ドープカーボンナノチューブに対して異なる合成方法のうち、10化学蒸着（CVD）は、より高い収率およびナノチューブの成長条件で容易に制御などのいくつかの利点のために最も一般的な方法であった。気相-液相-固相（VLS）成長メカニズムは、一般に窒素をドープしたCNTのCVD成長プロセスを理解するために用いられる。一般的に11は、成長中の金属触媒の種子を使用するには、2つの異なる方式がある。 &quot;固定床&quot;方式では、定義されたサイズの鉄ナノ粒子が第一鉄ペンタカルボニルの熱分解によって合成され、その後のCVD成長のためにスピンコート法により石英スライド上にめっき&quot;浮遊触媒&quot;方式、鉄触媒（典型的には12フェロセン）炭素とnと混合し、注射したitrogen前駆体、炭素および窒素前駆体が堆積された鉄触媒ナノ粒子の in situ生成に設けられたフェロセンの熱分解。固定床触媒が得られたNCNCsサイズのよりよい制御を提供しながら、生成物の収率は、典型的に低くなる（同じ前駆量および成長時間は&lt;（5mg）を1 mg）を浮遊触媒方式に比べ&gt;。フローティング触媒方式はまたNCNCsのかなり均一なサイズ分布を提供するとして、それはNCNCsのCVD合成のため、本稿で採用した。 CVD法は、多数の積み重ねられたカップからなるフィブリル形態を示す合成さNCNCsが得られる。隣接カップの間に化学結合が存在しないものの、それらはしっかりと互いのキャビティ内に挿入し、複数の非共有結合性相互作用および非晶質炭素の外層によって保持されているので、8課題は、個々のカップの有効な分離に残る。8 ATTE積み重ねられたカップを分離するためにMポイントは、化学的および物理的なアプローチの両方が含まれます。強酸の混合物中の酸化処理は、13,14 CNTを切断し、酸素官能基を導入するための典型的な手順であるが、それはまた短いセクションにNCNCsを切断するために適用することができる。マイクロ波プラズマエッチング手順もNCNCsを分離することが示されている。15の化学的ア ​​プローチと比較して、物理的な分離がより簡単である。我々の以前の研究は、単に乳鉢と乳棒個人NCNCsで粉砕することによって部分的にそれらの積層構造から単離することができることを示した。7に加えて、効果的に単層カーボンナノチューブを切断することが報告された高強度のプローブチップ音波処理、（単層カーボンナノチューブ） 16はまたNCNCsの分離に大きな影響を及ぼすことが示された。8プローブチップ音波処理は、本質的に積層されたカップ&quot;揺れ&quot;というNCNC溶液に高強度の超音波パワーを提供し、弱いinteraを破壊一緒にカップを握るctions。他の潜在的な分離方法は、カップ構造に非効率的なまたは破壊的のいずれかであるが、プローブ先端の超音波処理は、個々のグラファイトのコップを取得するために非常に効果的な、コスト効率と低い破壊的な物理的な分離方法を提供する。 合成されたフィブリルNCNCsは最初濃H 2 SO前プローブチップ超音波処理との分離〜4 / HNO 3酸混合物で処理した。結果分離NCNCsは非常に親水性のあった、効果的に水中に分散。我々は以前にそのようなNCNCs上のアミン基のような窒素官能基を同定しNCNCs官能のための彼らの化学反応を利用してきた。7,8,17、商用ナノ粒子とNCNCsをすてき私たちの以前に報告された方法に比べて、この仕事で8、金ナノ粒子（GNPS）があった効果的に塩化金酸からクエン酸還元によってカップの表面に固定。によるオープン時に窒素官能基の優先的分布がNCNCsの縁、金前駆体からその場で合成GNPSはコップにリムオープンとフォームGNP &quot;コルク栓&quot;とのより良い相互作用を持っている傾向があった。このような合成および官能方法は、薬物送達担体としての潜在的用途のための新規なGNP-NCNCハイブリッドナノ材料をもたらした。

<table border="1">
 <tbody>
 <tr>
 <td>Reagent Name</td>
 <td>Company</td>
 <td>Catalogue Number</td>
 <td>Comment</td>
 </tr>
 <tr>
 <td></td>
 <td></td>
 <td>&nbsp;</td>
 <td>Reagents</td>
 </tr>
 <tr>
 <td>H2</td>
 <td>Valley National Gases</td>
 <td>Grade 5.0</td>
 <td></td>
 </tr>
 <tr>
 <td>Ar</td>
 <td>Valley National Gases</td>
 <td>Grade 5.0</td>
 <td></td>
 </tr>
 <tr>
 <td>Ferrocene</td>
 <td>Sigma-Aldrich</td>
 <td>F408-500G</td>
 <td></td>
 </tr>
 <tr>
 <td>Xylenes</td>
 <td>Fisher Scientific</td>
 <td>X5-500</td>
 <td></td>
 </tr>
 <tr>
 <td>Acetonitrile</td>
 <td>EMD</td>
 <td>AXO149-6</td>
 <td></td>
 </tr>
 <tr>
 <td>H2SO4</td>
 <td>Fisher Scientific</td>
 <td>A300-500</td>
 <td></td>
 </tr>
 <tr>
 <td>HNO3</td>
 <td>EMD</td>
 <td>NX0409-2</td>
 <td></td>
 </tr>
 <tr>
 <td>DMF</td>
 <td>Fisher Scientific</td>
 <td>D119-500</td>
 <td></td>
 </tr>
 <tr>
 <td>Ethanol</td>
 <td>Decon</td>
 <td>2716</td>
 <td></td>
 </tr>
 <tr>
 <td>Phenol</td>
 <td>Sigma-Aldrich</td>
 <td>P1037-100G</td>
 <td></td>
 </tr>
 <tr>
 <td>Pyridine</td>
 <td>EMD</td>
 <td>PX2020-6</td>
 <td></td>
 </tr>
 <tr>
 <td>Hydridantin</td>
 <td>Sigma-Aldrich</td>
 <td>H2003-10G</td>
 <td></td>
 </tr>
 <tr>
 <td>Ninhydrin </td>
 <td>Alfa Aesar</td>
 <td>43846</td>
 <td></td>
 </tr>
 <tr>
 <td>HAuCl4</td>
 <td>Sigma-Aldrich</td>
 <td>52918-1G</td>
 <td></td>
 </tr>
 <tr>
 <td>Sodium Citrate</td>
 <td>SAFC</td>
 <td>W302600</td>
 <td></td>
 </tr>
 <tr>
 <td></td>
 <td></td>
 <td>&nbsp;</td>
 <td>Equipment</td>
 </tr>
 <tr>
 <td>CVD Furnace</td>
 <td>Lindberg/Blue</td>
 <td>&nbsp;</td>
 <td></td>
 </tr>
 <tr>
 <td>TEM (low-resolution)</td>
 <td>FEI Morgagni</td>
 <td>&nbsp;</td>
 <td></td>
 </tr>
 <tr>
 <td>TEM (high-resolution)</td>
 <td>JOEL</td>
 <td>2100F</td>
 <td></td>
 </tr>
 <tr>
 <td>Probe-tip Sonicator</td>
 <td>Qsonica</td>
 <td>XL-2000</td>
 <td></td>
 </tr>
 <tr>
 <td>UV-Vis Spectrometer</td>
 <td>Perkin-Elmer</td>
 <td>Lambda 900</td>
 <td></td>
 </tr>
 <tr>
 <td>Zeta Potential Analyzer</td>
 <td>Brookheaven</td>
 <td>ZetaPlus</td>
 <td></td>
 </tr>
 <tr>
 <td>EDX spectroscopy</td>
 <td>Phillips</td>
 <td>XL30 FEG</td>
 <td></td>
 </tr>
 </tbody>
</table>

synthesis and functionalization of nitrogen-doped carbon nanotube cups with gold nanoparticles as cork stoppers

窒素ドープカーボンナノチューブは、窒素ドープカーボンナノチューブカップ（NCNCs）と称される多くのカップ状黒鉛の区画から構成される。化学蒸着（CVD）法からこれらの合成された黒鉛nanocupsは非共有相互作用によってのみ保持された頭 - 尾状に積層した。個々のNCNCsは、化学的および物理的分離の一連のプロセスを通じて積層構造から単離することができる。まず、合成されたNCNCsは、グラファイト壁に酸素含有欠陥を導入する強酸の混合物中で酸化した。酸化NCNCs次いで、効果的に、個々のグラファイトnanocupsに積層NCNCsを分離した高強度のプローブチップ音波処理を用いて処理した。彼らの豊富な酸素と窒素の表面機能のおかげで、結果、個々のNCNCsは非常に親水性であり、効果的に優先的に開口部に収まる金ナノ粒子（GNPS）で官能化することができるコルク栓のようにカップの。 GNPSとコルクこれらグラファイトnanocupsは、ナノスケールのコンテナと薬物担体として有望なアプリケーションを見つけることができます。

CVD成長などから合成NCNCsは、石英基板上に黒色の材料のカーペットとして登場。数mg体重約NCNCsの厚さのフィルムをカミソリの刃（ 図1B）を剥離することによって得た。 TEM像は、異なる倍率で合成されたままのNCNCs（ 図1）の形態を示す。 30 nmの-低倍率（ 図1C）では、合成されたままNCNCsは全20の典型的には数マイクロメートルと直径の長さのフィブリル?...

Watch this Scientific Journal Video about Synthesis and Functionalization of Nitrogen-doped Carbon Nanotube Cups with Gold Nanoparticles as Cork Stoppers at JoVE.com

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

我々は、化学蒸着、酸酸化とプローブチップ音波処理を含む一連の手法を使用して、個々のグラファイトnanocupsの合成を説明した。のHAuClのクエン酸還元による<sub&gt; 4</sub&gt;、グラファイトnanocupsは金カップの化学反応のエッジに起因するナノ粒子と効果的にコルク栓をしました。

コルク栓のように金ナノ粒子と窒素ドープカーボンナノチューブカップの合成と機能化

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

synthesis-functionalization-nitrogen-doped-carbon-nanotube-cups-with

Research

JoVE Journal

Engineering

22.7K ビュー.  University of Pittsburgh. 我々は、化学蒸着、酸酸化とプローブチップ音波処理を含む一連の手法を使用して、個々のグラファイトnanocupsの合成を説明した。のHAuClのクエン酸還元による 4、グラファイトnanocupsは金カップの化学反応のエッジに起因するナノ粒子と効果的にコルク栓をしました。

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

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.

製造、ち密化、および3Dカーボンナノチューブの微細構造のレプリカ成形

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

工学

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

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

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

カーボンナノチューブアレイの濡れ特性をチューニングするための処置をアニーリングドライ酸化と真空

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

Ambient Method for the Production of an Ionically Gated Carbon Nanotube Common Cathode in Tandem Organic Solar Cells

A method of fabricating organic photovoltaic (OPV) tandems that requires no vacuum processing is presented. These devices are comprised of two solution-processed polymeric cells connected in parallel by a transparent carbon nanotubes (CNT) interlayer. This structure includes improvements in fabrication techniques for tandem OPV devices. First the need for ambient-processed cathodes is considered. The CNT anode in the tandem device is tuned via ionic gating to become a common cathode. Ionic gating employs electric double layer charging to lower the work function of the CNT electrode. Secondly, the difficulty of sequentially stacking tandem layers by solution-processing is addressed. The devices are fabricated via solution and dry-lamination in ambient conditions with parallel processing steps. The method of fabricating the individual polymeric cells, the steps needed to laminate them together with a common CNT cathode, and then provide some representative results are described. These results demonstrate ionic gating of the CNT electrode to create a common cathode and addition of current and efficiency as a result of the lamination procedure.

A method of fabricating, in ambient conditions, organic photovoltaic tandem devices in a parallel configuration is presented. These devices feature an air-processed, semi-transparent, carbon nanotube common cathode.

タンデム有機太陽電池におけるイオン的ゲーテッドカーボンナノチューブ共通カソードの生産のための周囲の方法

A method of fabricating organic photovoltaic (OPV) tandems that requires no vacuum processing is presented. These devices are comprised of two ...

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

Efforts to assemble graphene into three-dimensional monolithic structures have been hampered by the high cost and poor processability of graphene. Additionally, most reported graphene assemblies are held together through physical interactions (e.g., van der Waals forces) rather than chemical bonds, which limit their mechanical strength and conductivity. This video method details recently developed strategies to fabricate mass-producible, graphene-based bulk materials derived from either polymer foams or single layer graphene oxide. These materials consist primarily of individual graphene sheets connected through covalently bound carbon linkers. They maintain the favorable properties of graphene such as high surface area and high electrical and thermal conductivity, combined with tunable pore morphology and exceptional mechanical strength and elasticity. This flexible synthetic method can be extended to the fabrication of polymer/carbon nanotube (CNT) and polymer/graphene oxide (GO) composite materials. Furthermore, additional post-synthetic functionalization with anthraquinone is described, which enables a dramatic increase in charge storage performance in supercapacitor applications.

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.

グラフェンエアロゲルとグラフェンマクロアセンブリ：3Dナノグラフェン材料の合成と機能化

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

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.

半導体技術との互換性低温カーボンナノチューブ垂直相互接続の作製

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

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.

高炉スラグの双方向の物価安定政策：沈殿した炭酸カルシウムおよびゼオライト重金属吸着剤の合成

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 ...

Precision Milling of Carbon Nanotube Forests Using Low Pressure Scanning Electron Microscopy

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning electron microscope (ESEM) operating with a low pressure water vapor ambient. In this technique, a portion of the electron beam interacts with the water vapor in the vicinity of the CNT sample, dissociating the water molecules into hydroxyl radicals and other species by radiolysis. The remainder of the electron beam interacts with the CNT forest sample, making it susceptible to oxidation from the chemical products of radiolysis. This technique may be used to trim a selected region of an individual CNT, or it may be used to remove hundreds of cubic microns of material by adjusting ESEM parameters. The machining resolution is similar to the imaging resolution of the ESEM itself. The technique produces only small quantities of carbon residue along the boundaries of the cutting zone, with minimal effect on the native structural morphology of the CNT forest.

Low pressure scanning electron microscopy in a water vapor ambient is used to machine nanoscale to microscale features in carbon nanotube forests.

低圧走査型電子顕微鏡を用いたカーボンナノチューブの森の精密フライス

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning ...

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

層状チタン酸透明フィルムの層間空間で凝集することなく金ナノ粒子のその場合成で

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs ...

Controllable Nucleation of Cavitation from Plasmonic Gold Nanoparticles for Enhancing High Intensity Focused Ultrasound Applications

In this study, plasmonic gold nanoparticles were simultaneously exposed to pulsed near-infrared laser light and high intensity focused ultrasound (HIFU) for the controllable nucleation of cavitation in tissue-mimicking gel phantoms. This in vitro protocol was developed to demonstrate the feasibility of this approach, for both enhancement of imaging and therapeutic applications for cancer. The same apparatus can be used for both imaging and therapeutic applications by varying the exposure duration of the HIFU system. For short duration exposures (10 &#181;s), broadband acoustic emissions were generated through the controlled nucleation of inertial cavitation around the gold nanoparticles. These emissions provide direct localization of nanoparticles. For future applications, these particles may be functionalized with molecular-targeting antibodies (e.g. anti-HER2 for breast cancer) and can provide precise localization of cancerous regions, complementing routine diagnostic ultrasound imaging. For continuous wave (CW) exposures, the cavitation activity was used to increase the localized heating from the HIFU exposures resulting in larger thermal damage in the gel phantoms. The acoustic emissions generated from inertial cavitation activity during these CW exposures was monitored using a passive cavitation detection (PCD) system to provide feedback of cavitation activity. Increased localized heating was only achieved through the unique combination of nanoparticles, laser light and HIFU. Further validation of this technique in pre-clinical models of cancer is necessary.

This protocol demonstrates the controllable nucleation of cavitation in gel phantoms, through simultaneous exposure to both near-infrared pulsed laser light and high intensity focused ultrasound (HIFU). The cavitation activity can then be used for enhancing imaging and/or therapeutic uses of HIFU.

高強度を強化するため金ナノ粒子プラズモニックからキャビテーションの制御可能な核集中超音波アプリケーション

In this study, plasmonic gold nanoparticles were simultaneously exposed to pulsed near-infrared laser light and high intensity focused ultrasound (HIFU) ...

An Efficient Method for Selective Desalination of Radioactive Iodine Anions by Using Gold Nanoparticles-Embedded Membrane Filter

Here, we demonstrate a detail protocol for the preparation of nanomaterials-embedded composite membranes and its application to the efficient and ion-selective removal of radioactive iodines. By using citrate-stabilized gold nanoparticles (mean diameter: 13 nm) and cellulose acetate membranes, gold nanoparticle-embedded cellulose acetate membranes (Au-CAM) have easily been fabricated. The nano-adsorbents on Au-CAM were highly stable in the presence of high concentration of inorganic salts and organic molecules. The iodide ions in aqueous solutions could rapidly be captured by this engineered membrane. Through a filtration process using an Au-CAM containing filter unit, excellent removal efficiency (&gt;99%) as well as ion-selective desalination result was achieved in a short time. Moreover, Au-CAM provided good reusability without significant decrease of its performances. These results suggested that the present technology using the engineered hybrid membrane will be a promising process for the large-scale decontamination of radioactive iodine from liquid wastes.

An efficient method for the rapid and ion-selective desalination of radioactive iodine in several aqueous solutions is described by using gold nanoparticles-immobilized cellulose acetate membrane filters.