この作品は、ローランド ・ ハーバード研究所大学ローランド ・ フェロー プログラムによって支えられました。本研究は、ナノスケール システム (CNS)、賞の下の国立科学財団によってサポートされて国家ナノテクノロジー インフラストラクチャ ネットワークのメンバーの中心に一部で行われたないです。ECS 0335765。中枢神経系は、ハーバード大学の一部です。

1. Ni 単原子触媒 (ニン GS) の調製
<ol><li>エレクトロスピニング前駆体溶液の調製<ol>
<li>20 mL シンチレーション バイアルを取る、ポリアクリロニ トリルの 0.5 g を溶解 (Mw= 150,000)、polypyrrolidone の 0.5 g (Mw= 1,300,000)、Ni (3)2·6H2の 0.5 g O およびジシアンジアミド 10 mL に 0.1 gジメチルホルムアミド (DMF)。</li>
		<li>80 ° C に DMF の混合物を加熱して、すべてのポリマーと塩を溶解し、透明な溶液が観測されるまでに一定の攪拌を 80 ° C で混合物。</li>
	</ol>
</li>
	<li>ポリマー繊維を生成するエレクトロスピニング<ol>
<li>として従来のエレクトロスピニング パラメーターを設定: 15 kV 静的電気電圧、空気の 15 cm のギャップ距離、8 × 8 cm 炭素繊維紙 (CFP) - のコレクション基板 4 kV の電圧。</li>
		<li>5 mL 注射器に用いた前駆体溶液の 5 mL を抽出し、1.2 mL の流量シリンジ ポンプを開始 h−1、そして、スタート、エレクトロスピニング。 注意: 静電紡糸用高電圧が使用されます。にもかかわらず、非常に低い電流を通過システム紡糸過程中に、断熱の木製キャビネットが示唆されました。</li>
		<li>静電紡糸プロセスが完了、CFP 基板を取り出してください。高分子繊維の膜は、CFP の表面をカバーしています。</li>
	</ol>
</li>
	<li>単層カーボンナノ チューブに高分子繊維を熱処理<ol>
<li>ボックス炉 1.5 h で 300 ° C まで準備としてポリマー繊維フィルム/CFP を熱し、ポリマー、酸化を 0.5 時間温度を保ちます。 注: 酸化処理後ナノファイバー (NFs)、独立したフィルム、カーボン紙から自己デタッチ。</li>
		<li>小さい部分にそれらのナノファイバーをカットするはさみのペアを使用 (〜 0.5 cm × 2 cm) ・石英ボートにそれらを置きます。</li>
		<li>チューブ炉に石英ボートを置き、ガス (Ar の2 5 %h) 雰囲気を形成中で deaerate。100 sccm としてガス流量、圧力 1 Tor を維持します。</li>
		<li>熱を 300 ° c で 10 分間ランプと 2 h 750 ° c、別 1 時間維持し、自然冷却が続くそれはランプ内にあります。</li>
	</ol>
</li>
	<li>ボール ミル ニン GS として合成した触媒ナノ触媒のキャラクタリゼーションに 5 分間、</li>
</ol>2. 電気化学の CO2削減測定
<ol><li>セル ・電極<ol>
<li>次の測定に備えて 0.1 M KHCO3電解質、最初 KHCO3 250 mL の超純水の水に 2.5 g を溶解しを 0.1 で 2 つのグラファイト棒の間電気分解による電解質を浄化するには、mA 24 h のいずれかを削除する微量金属のイオン。</li>
		<li>新鮮な (電気化学) 洗練されたガラス状炭素 (1 cm × 2 cm) をとり、働く電極基板としての電気化学的不活性、疎水性ワックスとその裏側をカバーします。</li>
		<li>4 mL シンチレーション バイアルを取る、エタノール 1 mL とグラスアイオノマー溶液 (2 proponal の 5%)、バイアル内の 100 μ L ニン GS 触媒の準備として 5 mg を混合し、均一系触媒インクの懸濁液を得るために 20 分間超音波。</li>
		<li>ピペット 80 μ L 触媒インク滴を 2 cm2グラッシー カーボン表面 (0.2 mg cm-2質量負荷)、および真空乾燥の触媒使用する前に乾燥器で覆われた電極。</li>
		<li>それぞれ、カウンターと参照電極として白金箔とカロメル電極 (SCE) を使用しています。</li>
		<li>セルを使用するカスタマイズされた気密性 H 型ガラス、組立上の 3 つの電極と電気化学的テストを実行するためのプロトン交換膜で区切られました。</li>
		<li>他の商工会議所で作用電極と H-電池の 1 つのコンパートメントで SCE 参照電極と白金箔電極を配置します。挿入 〜 H セルの各区画に電解液 25 mL。</li>
		<li>潜在的な制御のための電気化学的仕事駅に H セルに 3 つの電極を接続します。</li>
		<li>N2に向かって 30 分 N2 (マスフロー コント ローラーによって監視) 50.0 sccm で電解質をバブル-0.1 M KHCO3を飽和。</li>
		<li>EC ラボのソフトウェアでサイクリック ・ ボルタンメトリー (CV) 技法を選択、「-10 V を 10 V」として「電子レンジ (潜在性)」を設定 N2で 50 mV/秒のスキャン レートで (sce)-1.8 V に-0.5 V から 5 連続 CV スキャンを実行「私範囲 (現在の)」"Auto"、として-0.1 M KHCO3を飽和。</li>
		<li>50 sccm CO2ガス流へ変更、CO2に向かって 30 分待つ-0.1 M KHCO3電解液を飽和し、次電解全体同じ CO2の流れを維持します。</li>
		<li>EC ラボのソフトウェアで CV 技術を選択し、「-10 V を 10 V」として「電子レンジ (潜在性)」を設定 CO2で 50 mV/秒のスキャン レートで (sce)-1.8 V に-0.5 V から 5 連続 CV スキャンを実行「私範囲 (現在の)」"Auto"、として-0.1 M KHCO3を飽和。</li>
		<li>PH メーターを使用し、電解質、すなわちpH 値。、0.1 M KHCO3 N2と CO2飽和。</li>
		<li>この作業を使用して可逆水素電極 (RHE) スケールに SCE に対して測定されたすべての電位に変換 E (対 RHE) = 0.0591 × pH + 0.244 V E (対 SCE)。</li>
		<li>抵抗値を記録、200 kHz を 0.1 Hz から定電位電気化学インピー ダンス分光法 (PEIS) 技術、[設定周波数範囲を選択して EC ラボのソフトウェア ソリューション抵抗 (Ru) を決定します。</li>
		<li>手動でiRを補償-E としてドロップ (iR 補正対 RHE) = E (対 RHE) - Ru × 私 (平均電流のアンペア)。</li>
	</ol>
</li>
	<li>オンライン ガスクロマト グラフ (GC) による CO2削減製品分析<ol>
<li>GC で CO2RR 中ガス製品分析、分子ふるい 5 a および micropacked 列の組み合わせ装備を採用してください。 注: 詳細な GC の列の型は、添付資料表で見つけることが。</li>
		<li>定量分析共同コンテンツに methanizer および/または他のアルカン種と熱伝導度検出器 (TCD) H2濃度を定量化して炎イオン化検出器 (FID) を使用します。</li>
		<li>H2と CO 濃度の検量線の 2 つの種類の標準ガスを使用して (H2: 100 と 1042 ppm;CO: 100 と 496.7 ppm;アルゴンとバランス)。</li>
		<li>電解中に CO2ガス流量 50.0 sccm を維持、CO2を含んでいる陰極コンパートメントに CO2を提供-飽和の 0.1 M KHCO3電解質と GC に排気口。</li>
		<li>段階的な調整に至る-0.3-1.0 V vs. RHE、作用電極上の電圧維持 〜 可能性および対応する chronoamperimetric 曲線のレコードごとに 15 分。</li>
		<li>H2と CO TCD と FID 信号からの排気をそれぞれ決定します。 注: ガス製品の連続電解後サンプリング 〜 各ポテンシャル下で 10 分。継続的に混合して、50 sccm CO2ガス生産 H2と CO、電解中に GC のサンプリング ループ (1 mL) を流れます。</li>
		<li>として、以下の指定されたガス製品の部分の電流密度を計算します。 <img alt="Equation" src="/files/ftp_upload/57380/57380eq2.jpg"> オンライン GC 較正曲線を参照によって決定される特定の製品の体積xは私が 2 つの標準ガス試料から (スコット ・ ガス)、 vは 50 sccm の流量、 n の私は数電子の関与、 p0 = 101.3 kPa、 Fはファラデー定数、 Rはガス定数。</li>
		<li>として可能性のあるに対応するファラデー効率 (FE) を計算する<img alt="Equation" src="/files/ftp_upload/57380/57380eq7.jpg">。 注: 全体的な生成効率はガス流量、電流密度、ガス濃度分析 GC からエラーのため 90 ~ 110% の範囲内かもしれません。</li>
	</ol>
</li>
</ol>

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上記の静電紡糸プロセスで 2 つの重要な手順は、材料合成の手順で注目すべき: 1) 暖房 DMF 混合物 (ステップ 1.1.2) と 2) ポンプ率の調整 (ステップ 1.2.2) 回転率に一致します。図 1 aに SEM 画像を示していますお互いに相互接続された得られた炭素ナノファイバー (~ 200 nm の直径)。図 1 bに示すように特性のボールミルによって小さな断片に壊れていた?...

化学薬品や燃料のクリーンな電力を使用してに変換する CO2はさらに CO2排出量1,2,3,4を防ぐために潜在的なルートとしてますます重要になって 5,6。しかし、この実用的なアプリケーションは現在低活性および CO2還元反応 (CO2RR) 高速度論的障壁との競争による水溶液中の水素 (彼女) との選択の挑戦です。メディア。Fe、Co、Ni など、伝統的な遷移金属触媒のほとんどは、その見事な彼女の活動7,8による CO2RR 選択度の低い展示します。これらの遷移金属触媒の反応経路を変更する、素材の性質を効果的にチューニングの CO2RR の選択性を改善するために重要になります。触媒の電子特性を変更するさまざまな方法の間でに彼らのバルクの相手と比較して劇的に変更された触媒行動により最近集中的な注目を集めている単一原子形態に金属原子を分散9,10,11します。 しかし、無制限原子の高移動度のため支持物が存在しなくても 1 つの金属原子を取得する非常に困難です。したがって、閉じ込めるし、遷移金属原子との調整に作成された欠陥を有するホスト マトリックス材料は必要です。これは新たな機会を開くことができません: 1) 2 CO2RR アクティブ サイトと遷移金属の電子特性をチューニング) 同時に維持機構は、研究の比較的単純な原子調整。また、限られた環境の中に閉じ込めその遷移金属原子簡単に移動できません防止する核生成または多くの場合12,13 で観測された表面原子の触媒作用の中に、14。
二次元多層グラフェンは、特に関心の CO2還元と彼女の触媒反応の両方に高電子伝導性、化学的安定性、不活性など金属単原子のホストとして。もっと重要なは、Fe、Co と Ni 金属は、その表面15炭素黒鉛化プロセスを触媒できるように知られていた。一言で言えば、これらの遷移金属は、高温熱処理プロセス中に炭素合金でしょう。温度が低下すると、炭素合金相析出を開始し、遷移金属表面上のグラフェン層を作るのため触媒です。このプロセス中に生成、グラフェン欠陥を有する金属単原子に閉じ込められるそれらのグラフェンの欠陥で CO2RR16,17,18,19のアクティブなサイトとして。2削減製品分析オンライン CO の明示的なデモンストレーションを提供するため、単一原子触媒化学の分野で新しい医師を助けるために意図この詳細なプロトコルを報告する.詳細については、私たちの最近発行された記事19および関連作品20,21,22,23のシリーズで見つけることが。

<table border="0" cellpadding="0" cellspacing="0" width="829">
	<tbody>
		<tr height="23">
			<td height="23" style="height:23px;width:216px;">syringe pump&#160;</td>
			<td style="width:164px;">KD Scientific</td>
			<td style="width:151px;">KDS-100</td>
			<td style="width:299px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:216px;">tube furnance</td>
			<td style="width:164px;">Lindberg/Blue M</td>
			<td style="width:151px;">TF55035A-1</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">ball miller</td>
			<td style="width:164px;">SPEX SamplePrep</td>
			<td style="width:151px;">5100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">electrochemical work station</td>
			<td style="width:164px;">BioLogic</td>
			<td style="width:151px;">VMP3</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">pH meter</td>
			<td style="width:164px;">Orion</td>
			<td style="width:151px;">320 PerpHecT&#160;</td>
			<td>2 points calibration before use</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">gas chromatograph</td>
			<td style="width:164px;">Shimadzu</td>
			<td style="width:151px;">GC-2014</td>
			<td>a combined seperation system consisting of molecular sieve 5A, Hayesep Q, Hayesep T, and Hayesep N</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">mass flow controller</td>
			<td>Alicat Scientific&#160;</td>
			<td style="width:151px;">MC-50SCCM-D/5M</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">ultrapure water system</td>
			<td>Millipore</td>
			<td>Synergy</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">vacuum desiccator&#160;</td>
			<td>PolyLab</td>
			<td>55205</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">polyacrylonitrile</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">181315</td>
			<td>Mw=150,000</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">polypyrrolidone</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">437190</td>
			<td>Mw=1,300,000</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Ni(NO3)26H2O</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">244074</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">dicyandiamide</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">D76609</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">dimethylformamide</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">227056</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">carbon fiber paper&#160;</td>
			<td style="width:164px;">AvCarb</td>
			<td style="width:151px;">MGL370</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Nafion 117 membrane</td>
			<td style="width:164px;">Fuel Cell Store</td>
			<td style="width:151px;">117</td>
			<td>used as proton exchange membrane in H-cell</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">KHCO3</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td style="width:151px;">431583</td>
			<td>further purified by electrolysis</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">platinum foil&#160;</td>
			<td style="width:164px;">Beantown Chemical</td>
			<td style="width:151px;">126580</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">saturated calomel electrode</td>
			<td style="width:164px;">CH Instruments</td>
			<td style="width:151px;">CHI150</td>
			<td></td>
		</tr>
		<tr height="27">
			<td height="27" style="height:27px;width:216px;">glassy carbon electrode</td>
			<td style="width:164px;">HTW GmbH</td>
			<td style="width:151px;">SIGRADUR</td>
			<td>1 cm &#215; 2 cm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">wax</td>
			<td>Apiezon</td>
			<td style="width:151px;">W-W100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Nafion 117 solution</td>
			<td>Sigma-Aldrich</td>
			<td>70160</td>
			<td>used as ionomer in catalyst ink preparation&#160;</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">forming gas</td>
			<td>Airgas</td>
			<td>UHP</td>
			<td>5% H2 balanced with Ar</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">carbon dioxide</td>
			<td>Airgas</td>
			<td>LaserPlus</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">sandard gas</td>
			<td>Airgas</td>
			<td>customized</td>
			<td>500 ppm CO, 500 ppm CH4, 1000 ppm H2 balanced with Ar</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">sandard gas</td>
			<td>Air Liquide</td>
			<td>customized</td>
			<td>100 ppm H2, 100 ppm CO and other alkanes balanced with Ar</td>
		</tr>
	</tbody>
</table>

synthesis and performance characterizations of transition metal single atom catalyst for electrochemical co2 reduction

このプロトコルは、Ni 単一原子触媒の合成法とその触媒活性と選択性水溶液中の CO2削減電気化学のテストの両方を提示します。伝統的な金属ナノ結晶とは異なり、金属単原子の合成を含むマトリックス材料をそれらの単一原子を閉じ込めるし、凝集からそれらを防ぐことができます。エレクトロスピニングと熱処理 Ni 単一原子の分散し、CO に CO2還元の活性中心としてグラフェン シェルでコーディネートを準備する方法を報告する.合成の中には、N のドーパントは Ni 原子をトラップするグラフェン空孔の生成に重要な役割を果たします。収差補正走査透過電子顕微鏡と 3次元アトム プローブ トモグラフィーは、単一グラフェン欠員の Ni 原子サイトを識別するために用いられました。またオンラインのガス ・ クロマトグラフィーと相まって電気化学的 CO2削減装置の詳細なセットアップを示した。Ni 単一原子の触媒は金属 Ni と比較して、大幅に CO2削減を展示し、H2進化側反応を抑制します。

走査電子顕微鏡 (SEM)、走査透過電子顕微鏡 (STEM) とエネルギー分散型 x 線分光法 (EDX) マッピング像がニン GS の形態特性図 1に表示されます。3次元アトム プローブ断層レントゲン写真撮影 (3 D APT) 結果は近隣の化学物質の環境と同様に、単一の Ni サイト分布の直接同定法を図 2に示します。オンライン電気化学 GC 測定セッ?...

Watch this Scientific Journal Video about Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction at JoVE.com

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

合成と電気化学的 CO2削減のため単一原子の遷移金属触媒の性能評価

ここでは、合成のためのプロトコルを提案して水溶液中の一酸化炭素に選択的な二酸化炭素削減のための活性中心としてグラフェン欠員の調整遷移金属単原子の電気化学的テストします。

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

synthesis-performance-characterizations-transition-metal-single-atom

Research

JoVE Journal

Chemistry

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

18.0K ビュー.  Harvard University. ここでは、合成のためのプロトコルを提案して水溶液中の一酸化炭素に選択的な二酸化炭素削減のための活性中心としてグラフェン欠員の調整遷移金属単原子の電気化学的テストします。

ビデオ: Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Anticancer Metal Complexes: Synthesis and Cytotoxicity Evaluation by the MTT Assay

Titanium (IV) and vanadium (V) complexes are highly potent anticancer agents. A challenge in their synthesis refers to their hydrolytic instability; therefore their preparation should be conducted under an inert atmosphere. Evaluation of the anticancer activity of these complexes can be achieved by the MTT assay.
The MTT assay is a colorimetric viability assay based on enzymatic reduction of the MTT molecule to formazan when it is exposed to viable cells. The outcome of the reduction is a color change of the MTT molecule. Absorbance measurements relative to a control determine the percentage of remaining viable cancer cells following their treatment with varying concentrations of a tested compound, which is translated to the compound anticancer activity and its IC50 values. The MTT assay is widely common in cytotoxicity studies due to its accuracy, rapidity, and relative simplicity.
Herein we present a detailed protocol for the synthesis of air sensitive metal based drugs and cell viability measurements, including preparation of the cell plates, incubation of the compounds with the cells, viability measurements using the MTT assay, and determination of IC50 values.

A method for synthesis of air-sensitive titanium and vanadium anticancer agents is described, along with the evaluation of their cytotoxic activity towards human cancer cell line by the MTT Assay.

MTTアッセイにより合成と細胞毒性の評価：抗がん金属錯体

Titanium (IV) and vanadium (V) complexes are highly potent anticancer agents. A challenge in their synthesis refers to their hydrolytic instability; ...

化学

Synthesis and Characterization of Functionalized Metal-organic Frameworks

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy.

Synthesis, activation, and characterization of intentionally designed metal-organic framework materials is challenging, especially when building blocks are incompatible or unwanted polymorphs are thermodynamically favored over desired forms. We describe how applications of solvent-assisted linker exchange, powder X-ray diffraction in capillaries and activation via supercritical CO2 drying, can address some of these challenges.

官能化有機金属構造体の合成とキャラクタリゼーション

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

モノとバイメタル早期遷移金属炭化物と窒化物ナノ粒子の逆マイクロエマルジョン媒介合成

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

A Method to Manipulate Surface Tension of a Liquid Metal via Surface Oxidation and Reduction

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where interfacial tension is a dominant force. A variety of methods exist for controlling the interfacial tension of aqueous and organic liquids on this scale; however, these techniques have limited utility for liquid metals due to their large interfacial tension.
Liquid metals can form soft, stretchable, and shape-reconfigurable components in electronic and electromagnetic devices. Although it is possible to manipulate these fluids via mechanical methods (e.g., pumping), electrical methods are easier to miniaturize, control, and implement. However, most electrical techniques have their own constraints: electrowetting-on-dielectric requires large (kV) potentials for modest actuation, electrocapillarity can affect relatively small changes in the interfacial tension, and continuous electrowetting is limited to plugs of the liquid metal in capillaries.
Here, we present a method for actuating gallium and gallium-based liquid metal alloys via an electrochemical surface reaction. Controlling the electrochemical potential on the surface of the liquid metal in electrolyte rapidly and reversibly changes the interfacial tension by over two orders of magnitude ( &#820;500 mN/m to near zero). Furthermore, this method requires only a very modest potential (&#60; 1 V) applied relative to a counter electrode. The resulting change in tension is due primarily to the electrochemical deposition of a surface oxide layer, which acts as a surfactant; removal of the oxide increases the interfacial tension, and vice versa. This technique can be applied in a wide variety of electrolytes and is independent of the substrate on which it rests.

We present a method to control the interfacial energy of a liquid metal in an electrolyte via electrochemical deposition (or removal) of a surface oxide layer. This simple method can control the capillary behavior of gallium-based liquid metals by tuning the interfacial energy rapidly, significantly, and reversibly using modest voltages.

表面酸化と還元を経て液体金属の表面張力を操作する方法

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where ...

HKUST-1 as a Heterogeneous Catalyst for the Synthesis of Vanillin

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately 200 different odorant compounds in addition to vanillin. The natural extraction of vanillin (from the orchid Vanilla planifolia, Vanilla tahitiensis and Vanilla pompon) represents only 1% of the worldwide production and since this process is expensive and very long, the rest of the production of vanillin is synthesized. Many biotechnological approaches can be used for the synthesis of vanillin from lignin, phenolic stilbenes, isoeugenol, eugenol, guaicol, etc., with the disadvantage of harming the environment since these processes use strong oxidizing agents and toxic solvents. Thus, eco-friendly alternatives on the production of vanillin are very desirable and thus, under current investigation. Porous coordination polymers (PCPs) are a new class of highly crystalline materials that recently have been used for catalysis. HKUST-1 (Cu3(BTC)2(H2O)3, BTC = 1,3,5-benzene-tricarboxylate) is a very well known PCP which has been extensively studied as a heterogeneous catalyst. Here, we report a synthetic strategy for the production of vanillin by the oxidation of trans-ferulic acid using HKUST-1 as a catalyst.

The conversion of trans-ferulic acid to vanillin was achieved by heterogeneous catalysis. HKUST-1 was employed in this synthesis and the essential step in the catalytic process was the generation of unsaturated metal sites. Thus, when the catalyst was activated under vacuum, full vanillin conversion (yield of 95%) was obtained.

HKUST-1バニリンの合成のための不均一触媒として、

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately ...

Facile Synthesis of Worm-like Micelles by Visible Light Mediated Dispersion Polymerization Using Photoredox Catalyst

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins with the synthesis of a hydrophilic poly(oligo(ethylene glycol) methyl ether methacrylate) (POEGMA) homopolymer using reversible addition-fragmentation chain-transfer (RAFT) polymerization. Under mild visible light irradiation (&#955; = 460 nm, 0.7 mW/cm2), this macro-chain transfer agent (macro-CTA) in the presence of a ruthenium based photoredox catalyst, Ru(bpy)3Cl2 can be chain extended with a second monomer to form a well-defined block copolymer in a process known as Photoinduced Electron Transfer RAFT (PET-RAFT). When PET-RAFT is used to chain extend POEGMA with benzyl methacrylate (BzMA) in ethanol (EtOH), polymeric nanoparticles with different morphologies are formed in situ according to a polymerization-induced self-assembly (PISA) mechanism. Self-assembly into nanoparticles presenting POEGMA chains at the corona and poly(benzyl methacrylate) (PBzMA) chains in the core occurs in situ due to the growing insolubility of the PBzMA block in ethanol. Interestingly, the formation of highly pure worm-like micelles can be readily monitored by observing the onset of a highly viscous gel in situ due to nanoparticle entanglements occurring during the polymerization. This process thereby allows for a more reproducible synthesis of worm-like micelles simply by monitoring the solution viscosity during the course of the polymerization. In addition, the light stimulus can be intermittently applied in an ON/OFF manner demonstrating temporal control over the nanoparticle morphology.

This article describes a process for producing polymeric self-assembled nanoparticles using visible light mediated dispersion polymerization. Using low energy visible light to control the polymerization allows for the reproducible formation of self-assembled worm-like micelles at high solids content.

Photoredox触媒を用いた可視光媒介分散重合によるワームのようなミセルの簡便な合成

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins ...

Synthesis of a Water-soluble Metal&#8211;Organic Complex Array

We demonstrate a method for the synthesis of a water-soluble multimetallic peptidic array containing a predetermined sequence of metal centers such as Ru(II), Pt(II), and Rh(III). The compound, named as a water-soluble metal-organic complex array (WSMOCA), is obtained through 1) the conventional solution-chemistry-based preparation of the corresponding metal complex monomers having a 9-fluorenylmethyloxycarbonyl (Fmoc)-protected amino acid moiety and 2) their sequential coupling together with other water-soluble organic building units on the surface-functionalized polymeric resin by following the procedures originally developed for the solid-phase synthesis of polypeptides, with proper modifications. Traces of reactions determined by mass spectrometric analysis at the representative coupling steps in stage 2 confirm the selective construction of a predetermined sequence of metal centers along with the peptide backbone. The WSMOCA cleaved from the resin at the end of stage 2 has a certain level of solubility in aqueous media dependent on the pH value and/or salt content, which is useful for the purification of the compound.

A potential general method for the synthesis of water-soluble multimetallic peptidic arrays containing a predetermined sequence of metal centers is presented.

水溶性有機金属錯体アレイの合成

We demonstrate a method for the synthesis of a water-soluble multimetallic peptidic array containing a predetermined sequence of metal centers such as ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

ナノワイヤーの合成プラチナ ニッケルと酸素還元性能の最適化

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Synthesis of a Thiol Building Block for the Crystallization of a Semiconducting Gyroidal Metal-sulfur Framework

We present a method for preparing thioester molecules as the masked form of the thiol linkers and their utilization for accessing a semiconducting and porous metal-dithiolene network in the highly ordered single crystalline state. Unlike the highly reactive free-standing thiols, which tend to decompose and complicate the crystallization of metal-thiolate open frameworks, the thioester reacts in situ to provide the thiol species, serving to mitigate the reaction between the mercaptan units and the metal centers, and to improve crystallization consequently. Specifically, the thioester was synthesized in a one-pot procedure: an aromatic bromide (hexabromotriphenylene) reacted with excess sodium thiomethoxide under vigorous conditions to first form the thioether intermediate product. The thioether was then demethylated by the excess thiomethoxide to provide the thiolate anion that was acylated to form the thioester product. The thioester was conveniently purified by standard column chromatography, and then used directly in the framework synthesis, wherein NaOH and ethylenediamine serve to revert in situ the thioester to the thiol linker for assembling the single-crystalline Pb(II)-dithiolene network. Compared with other methods for thiol synthesis (e.g., by cleaving alkyl thioether using sodium metal and liquid ammonia), the thioester synthesis here uses simple conditions and economical reagents. Moreover, the thioester product is stable and can be conveniently handled and stored. More importantly, in contrast to the generic difficulty in accessing crystalline metal-thiolate open frameworks, we demonstrate that using the thioester for in situ formation of the thiol linker greatly improves the crystallinity of the solid-state product. We intend to encourage broader research efforts on the technologically important metal-sulfur frameworks by disclosing the synthetic protocol for the thioester as well as the crystalline framework solid.

Here, we present a one-pot, transition-metal-free synthesis of thiols and thioesters from aromatic halides and sodium thiomethoxide, followed by the preparation of single crystals of a metal-dithiolene network using thiol species generated in situ from the more stable and tractable thioester.

半導体 Gyroidal 金属硫黄フレームワークの結晶化に対するチオール ビルディング ブロックの合成

We present a method for preparing thioester molecules as the masked form of the thiol linkers and their utilization for accessing a semiconducting and ...

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.

Au、Pd、およびソリューションに基づく還元を介して Pt エアロゲルの迅速合成法

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