Name: synthesis and performance characterizations of transition metal single atom catalyst for electrochemical co2 reduction
Uploaded: 2018-04-10T14:45:00.000+00:00
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Description: Watch this Scientific Journal Video about Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction at JoVE.com

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><tbody><tr><td>syringe pump&amp;nbsp;</td><td>KD Scientific</td><td>KDS-100</td><td></td></tr><tr><td>tube furnance</td><td>Lindberg/Blue M</td><td>TF55035A-1</td><td></td></tr><tr><td>ball miller</td><td>SPEX SamplePrep</td><td>5100</td><td></td></tr><tr><td>electrochemical work station</td><td>BioLogic</td><td>VMP3</td><td></td></tr><tr><td>pH meter</td><td>Orion</td><td>320 PerpHecT&amp;nbsp;</td><td>2 points calibration before use</td></tr><tr><td>gas chromatograph</td><td>Shimadzu</td><td>GC-2014</td><td>a combined seperation system consisting of molecular sieve 5A, Hayesep Q, Hayesep T, and Hayesep N</td></tr><tr><td>mass flow controller</td><td>Alicat Scientific&amp;nbsp;</td><td>MC-50SCCM-D/5M</td><td></td></tr><tr><td>ultrapure water system</td><td>Millipore</td><td>Synergy</td><td></td></tr><tr><td>vacuum desiccator&amp;nbsp;</td><td>PolyLab</td><td>55205</td><td></td></tr><tr><td>polyacrylonitrile</td><td>Sigma-Aldrich</td><td>181315</td><td>M&lt;sub&gt;w&lt;/sub&gt;=150,000</td></tr><tr><td>polypyrrolidone</td><td>Sigma-Aldrich</td><td>437190</td><td>M&lt;sub&gt;w&lt;/sub&gt;=1,300,000</td></tr><tr><td>Ni(NO&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;6H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>244074</td><td></td></tr><tr><td>dicyandiamide</td><td>Sigma-Aldrich</td><td>D76609</td><td></td></tr><tr><td>dimethylformamide</td><td>Sigma-Aldrich</td><td>227056</td><td></td></tr><tr><td>carbon fiber paper&amp;nbsp;</td><td>AvCarb</td><td>MGL370</td><td></td></tr><tr><td>Nafion 117 membrane</td><td>Fuel Cell Store</td><td>117</td><td>used as proton exchange membrane in H-cell</td></tr><tr><td>KHCO&lt;sub&gt;3&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>431583</td><td>further purified by electrolysis</td></tr><tr><td>platinum foil&amp;nbsp;</td><td>Beantown Chemical</td><td>126580</td><td></td></tr><tr><td>saturated calomel electrode</td><td>CH Instruments</td><td>CHI150</td><td></td></tr><tr><td>glassy carbon electrode</td><td>HTW GmbH</td><td>SIGRADUR</td><td>1 cm &amp;times; 2 cm</td></tr><tr><td>wax</td><td>Apiezon</td><td>W-W100</td><td></td></tr><tr><td>Nafion 117 solution</td><td>Sigma-Aldrich</td><td>70160</td><td>used as ionomer in catalyst ink preparation&amp;nbsp;</td></tr><tr><td>forming gas</td><td>Airgas</td><td>UHP</td><td>5% H&lt;sub&gt;2&lt;/sub&gt; balanced with Ar</td></tr><tr><td>carbon dioxide</td><td>Airgas</td><td>LaserPlus</td><td></td></tr><tr><td>sandard gas</td><td>Airgas</td><td>customized</td><td>500 ppm CO, 500 ppm CH&lt;sub&gt;4&lt;/sub&gt;, 1000 ppm H&lt;sub&gt;2&lt;/sub&gt; balanced with Ar</td></tr><tr><td>sandard gas</td><td>Air Liquide</td><td>customized</td><td>100 ppm H&lt;sub&gt;2&lt;/sub&gt;, 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

Universidad San Sebastian

Research

JoVE Journal

Chemistry

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

18.1K 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

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 ...

化学

On the Preparation and Testing of Fuel Cell Catalysts Using the Thin Film Rotating Disk Electrode Method

We present a step-by-step tutorial to prepare proton exchange membrane fuel cell (PEMFC) catalysts, consisting of Pt nanoparticles (NPs) supported on a high surface area carbon, and to test their performance in thin film rotating disk electrode (TF-RDE) measurements. The TF-RDE methodology is widely used for catalyst screening; nevertheless, the measured performance sometimes considerably differs among research groups. These uncertainties impede the advancement of new catalyst materials and, consequently, several authors discussed possible best practice methods and the importance of benchmarking.
The visual tutorial highlights possible pitfalls in the TF-RDE testing of Pt/C catalysts. A synthesis and testing protocol to assess standard Pt/C catalysts is introduced that can be used together with polycrystalline Pt disks as benchmark catalysts. In particular, this study highlights how the properties of the catalyst film on the glassy carbon (GC) electrode influence the measured performance in TF-RDE testing. To obtain thin, homogeneous catalyst films, not only the catalyst preparation, but also the ink deposition and drying procedures are essential. It is demonstrated that an adjustment of the ink&#39;s pH might be necessary, and how simple control measurements can be used to check film quality. Once reproducible TF-RDE measurements are obtained, determining the Pt loading on the catalyst support (expressed as Pt wt%) and the electrochemical surface area is necessary to normalize the determined reaction rates to either surface area or Pt mass. For the surface area determination, so-called CO stripping, or the determination of the hydrogen underpotential deposition (Hupd) charge, are standard. For the determination of the Pt loading, a straightforward and cheap procedure using digestion in aqua regia with subsequent conversion of Pt(IV) to Pt(II) and UV-vis measurements is introduced.

Preparing and testing Pt/C fuel cell catalysts is subject to continuous discussion in the scientific community with respect to reproducibility and best practice. With the presented work, we intend to present a step-by-step tutorial to make and test Pt/C catalysts, which can serve as benchmark for novel catalyst systems.

準備および薄膜回転ディスク電極法を用いた燃料電池触媒のテストに

We present a step-by-step tutorial to prepare proton exchange membrane fuel cell (PEMFC) catalysts, consisting of Pt nanoparticles (NPs) supported on a ...

環境学

Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and composition of the material was characterized via powder X-ray diffraction (PXRD), M&#246;ssbauer spectroscopy (MB), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX). Two preparation methods of pentlandite bulk electrodes are presented. In the first approach a piece of synthetic pentlandite rock is directly contacted via a wire ferrule. The second approach utilizes pentlandite pellets, pressed from finely ground powder, which is immobilized in a Teflon casing. Both electrodes, whilst being prepared by an additive-free method, reveal high durability during electrocatalytic conversions in comparison to common drop-coating methods. We herein showcase the striking performance of such electrodes to accomplish the hydrogen evolution reaction (HER) and present a standardized method to evaluate the electrocatalytic performance by electrochemical and gas chromatographic methods. Furthermore, we report stability tests via potentiostatic methods at an overpotential of 0.6 V to explore the material limitations of the electrodes during electrolysis under industrial relevant conditions.

A facile preparation method of electrodes using the bulk material Fe4.5Ni4.5S8 is presented. This method provides an alternative technique to conventional electrode fabrication and describes prerequisites for unconventional electrode materials including a straightforward electrocatalytic testing method.

電気化学的応用のための非貴金属バルク電極の調製のための簡単な方法

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and ...

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 ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

Nb2O5の合成化学沈殿法変更高表面積一括ニッケル触媒

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Preparation of Polyoxometalate-based Photo-responsive Membranes for the Photo-activation of Manganese Oxide Catalysts

This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic polymers, with the aim of photo-activating oxygen-evolving manganese oxide catalysts, which are important components in artificial photosynthesis. The cross-linking technique was applied to obtain a self-standing membrane with a high PW12O403- content. Incorporation and structure retention of PW12O403- within the polymer matrix were confirmed by FT-IR and micro-Raman spectroscopy, and optical characteristics were investigated by UV-Vis spectroscopy, which revealed successful construction of the metal-to-metal charge transfer (MMCT) unit. After deposition of MnOx oxygen evolving catalysts, photocurrent measurements under visible light irradiation verified the sequential charge transfer, Mn &#8594; MMCT unit &#8594; electrode, and&#160;the photocurrent intensity was consistent with the redox potential of the donor metal (Ce or Co). This method provides a new strategy for preparing integrated systems involving catalysts and photon-absorption parts for use with photo-functional materials.

Here, we present a protocol to prepare charge transfer chromophores based on a polyoxometalate/polymer composite membrane.

マンガン酸化物触媒の光活性化用ポリ酸を用いた光応答性膜の作製

This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic ...

Multiscale Sampling of a Heterogeneous Water/Metal Catalyst Interface using Density Functional Theory and Force-Field Molecular Dynamics

A significant number of heterogeneously-catalyzed chemical processes occur under liquid conditions, but simulating catalyst function under such conditions is challenging when it is necessary to include the solvent molecules. The bond breaking and forming processes modeled in these systems necessitate the use of quantum chemical methods. Since molecules in the liquid phase are under constant thermal motion, simulations must also include configurational sampling. This means that multiple configurations of liquid molecules must be simulated for each catalytic species of interest. The goal of the protocol presented here is to generate and sample trajectories of configurations of liquid water molecules around catalytic species on flat transition metal surfaces in a way that balances chemical accuracy with computational expense. Specifically, force field molecular dynamics (FFMD) simulations are used to generate configurations of liquid molecules that can subsequently be used in quantum mechanics-based methods such as density functional theory or ab initio molecular dynamics. To illustrate this, in this manuscript, the protocol is used for catalytic intermediates that could be involved in the pathway for the decomposition of glycerol (C3H8O3). The structures that are generated using FFMD are modeled in DFT in order to estimate the enthalpies of solvation of the catalytic species and to identify how H2O molecules participate in catalytic decompositions.

The goal of the protocol presented here is to generate and sample trajectories of configurations of liquid water molecules around catalytic species on a flat transition metal surface. The sampled configurations can be used as starting structures in quantum mechanics-based methods.

密度汎関数理論と力場分子動力学を用いた異種水/金属触媒インタ フェースのマルチ サンプリング

A significant number of heterogeneously-catalyzed chemical processes occur under liquid conditions, but simulating catalyst function under such conditions ...

Tuning the Acidity of Pt/ CNTs Catalysts for Hydrodeoxygenation of Diphenyl Ether

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid nanosheets, a series of Pt/xHMNO6/CNTs with different solid acid compositions (x = 5, 20 wt%; M = Nb, Ta; N = Mo, W) have been prepared by carbon nanotube pretreatment, protonic exchange, solid acid exfoliation, aggregation and finally Pt particles impregnation. The Pt/xHMNO6/CNTs are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and NH3-temperature programmed desorption. The study revealed that HNbWO6 nanosheets were attached on CNTs, with some edges of the nanosheets being bent in shape. The acid strength of the supported Pt catalysts increases in the following order: Pt/CNTs &#60; Pt/5HNbWO6/CNTs &#60; Pt/20HNbMoO6/CNTs &#60; Pt/20HNbWO6/CNTs &#60; Pt/20HTaWO6/CNTs. In addition, the catalytic hydroconversion of lignin-derived model compound: diphenyl ether using the synthesized Pt/20HNbWO6 catalyst has been investigated.

A protocol for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs is presented.

ジフェニルエーテルのヒドロデオキシゲーションのためのPt/CNT触媒の酸性度のチューニング

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid ...

Versatile CO2 Transformations into Complex Products: A One-pot Two-step Strategy

CO2 transformations using a one-pot two-step method are presented herein. The purpose of the method is to give access to a variety of value-added products and notably to generate chiral carbon centers. The crucial first step consists in the selective double hydroboration of CO2 catalyzed by an iron hydride complex. The product obtained with this 4 e- reduction is a rare bis(boryl)acetal, compound 1, which is subjected in situ to three different reactions in a second step. The first reaction concerns a condensation reaction with (diisopropyl)phenylamine affording the corresponding imine 2. In the second and third reaction, intermediate 1 reacts with triazol-5-ylidene (Enders&#39; carbene) to afford compounds 3 or 4, depending on the reaction conditions. In both compounds, C-C bonds are formed, and chiral centers are generated from CO2 as the only source of carbon. Compound 4 exhibits two chiral centers obtained in a diastereoselective manner in a formose-type mechanism. We proved that the remaining boryl fragment plays a key role in this unprecedented stereocontrol. The interest of the method stands on the reactive and versatile nature of 1, giving rise to various complex molecules from a single intermediate. The complexity of a two-step method is compensated by the overall short reaction time (2 h for the larger reaction time), and mild reaction conditions (25 &#176;C to 80 &#176;C and 1 to 3 atm of CO2).

Versatile CO2 Transformations into Complex Products: A One-pot Two-step Strategy

CO2 transformations are conducted in a one-pot two-step procedure for the synthesis of complex molecules. The selective 4 e- reduction of CO2 with a hydroborane reductant affords a reactive and versatile bis(boryl)acetal intermediate which is subsequently involved in condensation reaction or carbene-mediated C-C coupling generation.

多彩なCO2の複雑な製品への変革:ワンポット2段階戦略

CO2 transformations using a one-pot two-step method are presented herein. The purpose of the method is to give access to a variety of value-added products ...

Synthesis of Metal Nanoparticles Supported on Carbon Nanotube with Doped Co and N Atoms and its Catalytic Applications in Hydrogen Production

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented herein. The novel strategy is based on a facile one-pot pyrolysis treatment of cobalt (II) acetylacetonate and nitrogen-rich organic precursors under Ar atmosphere at 800 &#176;C, resulting in the formation of Co- and N- co-doped carbon nanotube with earthworm-like morphology. The obtained catalyst was found to have a high density of defect sites, as confirmed by Raman spectroscopy. Here, cobalt (II) nanoparticles were stabilized on the atomically dispersed cobalt- and nitrogen-doped carbon nanotubes. The catalyst was confirmed to be effective in the catalytic hydrolysis of ammonia borane, in which the turnover frequency was 5.87 mol H2&#183;molCo-1&#183;min-1, and the specific hydrogen generation rate was determined to be 2447 mL H2&#183;gCo-1&#183;min-1. A synergistic function between the Co nanoparticle and the doped carbon nanotubes was proposed for the first time in the catalytic hydrolysis of ammonia borane reaction under a mild condition. The resulting hydrogen production with its high energy density and minimal refueling time could be suitable for future development as energy sources for mobile and stationary applications such as road trucks and forklifts in transport and logistics.

Here, we present a protocol to synthesize Co nanoparticles supported on carbon nanotubes with Co- and N- dopants for hydrogen productions.

Co原子およびN原子をドープしたカーボンナノチューブに担持された金属ナノ粒子の合成と水素製造における触媒応用

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented ...

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

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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

準備および薄膜回転ディスク電極法を用いた燃料電池触媒のテストに

電気化学的応用のための非貴金属バルク電極の調製のための簡単な方法

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

Nb₂O₅の合成化学沈殿法変更高表面積一括ニッケル触媒

マンガン酸化物触媒の光活性化用ポリ酸を用いた光応答性膜の作製

密度汎関数理論と力場分子動力学を用いた異種水/金属触媒インタフェースのマルチサンプリング

ジフェニルエーテルのヒドロデオキシゲーションのためのPt/CNT触媒の酸性度のチューニング

多彩_なCO2の複雑な製品への変革:ワンポット2段階戦略

Co原子およびN原子をドープしたカーボンナノチューブに担持された金属ナノ粒子の合成と水素製造における触媒応用

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

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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

準備および薄膜回転ディスク電極法を用いた燃料電池触媒のテストに

電気化学的応用のための非貴金属バルク電極の調製のための簡単な方法

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

Nb2O5の合成化学沈殿法変更高表面積一括ニッケル触媒

マンガン酸化物触媒の光活性化用ポリ酸を用いた光応答性膜の作製

密度汎関数理論と力場分子動力学を用いた異種水/金属触媒インタ フェースのマルチ サンプリング

ジフェニルエーテルのヒドロデオキシゲーションのためのPt/CNT触媒の酸性度のチューニング

多彩なCO2の複雑な製品への変革:ワンポット2段階戦略

Co原子およびN原子をドープしたカーボンナノチューブに担持された金属ナノ粒子の合成と水素製造における触媒応用

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

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

Nb₂O₅の合成化学沈殿法変更高表面積一括ニッケル触媒

密度汎関数理論と力場分子動力学を用いた異種水/金属触媒インタフェースのマルチサンプリング

多彩_なCO2の複雑な製品への変革:ワンポット2段階戦略