感謝するキー研究・科学省の開発プログラムと中国 (2016YFB0600305)、国家自然科学基金、中国の (21573031, 21373038 番)、プログラムの技術によって提供される金融サポート大連市 (2016RD09) の技術及び高等教育研究所の香港 (THEi SG1617105 THEi SG1617127) の優れた才能。

注意:適切な処理メソッド、プロパティおよび本稿に記載されている化学物質の毒性、関連する化学物質安全性データ シート (MSDS) を参照してください。使用される化学薬品のいくつかは有毒であり、発癌性、特別な心配は取られなければなりません。安全性と健康への影響、ナノ材料はなる可能性があります。吸引および皮膚接触は避けるべきであります。オートクレーブ原子炉とヒューム フードと触媒性能評価で触媒の合成を行うなど、安全予防策を行使しなければなりません。個人用保護具を着用する必要があります。
1. Ni0.97Nb0.030.03 Nb:(Ni+Nb) のモル比と一致する、O 触媒の調製
<ol><li>攪拌棒 250 mL 三つ口丸底フラスコに脱イオン水 100 mL に硝酸ニッケルの 2.821 g とニオブ (V) シュウ酸水和物の 0.161 g を組み合わせます。</li>
	<li>暖房マグネチックスターラーを使用して沈殿物の消失までの化合物を溶解する 50 rpm、70 ° C でソリューションをかき混ぜます。</li>
	<li>80 ° C 2 ° C/分の速度で急速に温度を上げます。</li>
	<li>Ni/Nb 溶液の pH は 9.0 に達するまで反応混合物に滴下 [水性水酸化アンモニウム (50 mL、1.0 M) と水酸化ナトリウム (50 mL、0.2 M)] 混合の基本的なソリューションを追加します。</li>
	<li>反応混合物を攪拌しながら 2 ° C/分で 120 ° C に温度を上げます。</li>
	<li>ソリューションの緑の色の完全な消失まで、120 ° C で 50 rpm で一晩反応混合物をかき混ぜます。</li>
	<li>残り Ni2 +と Nb5 +イオン溶液中の濃度を評価し、残りのニッケルの完全な沈殿物を確保するを解決するための誘導結合プラズマ発光分析法 (ICP-OES) 分析を実行します。硝酸態窒素。</li>
	<li>吸引ビンを使用してろ過で固体を収集します。残留の Na+陽イオンを削除する 20 分以内繰り返し 2 L の脱イオン水を加えることで固体を洗います。</li>
	<li>時計ガラス中の固形物を収集します。乾燥オーブンで 12 h 110 ° C で固体を乾燥させます。</li>
	<li>カルサイン チューブ炉で 5 h 450 ° C で合成空気 (20 mL/分 O2と 80 mL/分 N2) 中の固形物を加熱することによって。反応の高温を使用する前に欠陥のすべてのガラス製品を確認してください。</li>
	<li>焼成後 Ni0.97Nb0.03O 触媒の 1 g を入手します。安全眼鏡、手袋、白衣など適切な保護具を使用して、潜在的な安全上の問題とナノマテリアルの健康影響によるナノ結晶反応を実行するドラフトチャンバーします。</li>
</ol>2. Ni0.92Nb0.08Nb:(Ni+Nb) モル比が 0.08 に等しい O 触媒の調製
<ol><li>この手順は、最初の 2 つの手順を除いて 1 に似ています。<ol>
<li>100 mL の脱イオン水でニオブ (V) シュウ酸水和物の 0.43 g を溶解します。</li>
		<li>別に、脱イオン水 100 mL に硝酸ニッケルの 2.675 g を溶解します。</li>
	</ol>
</li>
</ol>3. Ni0.85Nb0.15Nb:(Ni+Nb) モル比が 0.15 に等しい O 触媒の調製
<ol><li>手順は、最初の 2 つの手順を除いて 1 と同様です。<ol>
<li>100 mL の脱イオン水でニオブ (V) シュウ酸水和物の 0.807 g を溶解します。</li>
		<li>別に、脱イオン水 100 mL に硝酸ニッケルの 2.472 g を溶解します。</li>
	</ol>
</li>
</ol>4. Ni0.80Nb0.20Nb:(Ni+Nb) モル比が 0.20 と等しい O 触媒の調製
<ol><li>手順は、最初の 2 つの手順を除いて 1 と同様です。<ol>
<li>100 mL の脱イオン水でニオブ (V) シュウ酸水和物の 1.076 g を溶解します。</li>
		<li>別に、脱イオン水 100 mL に硝酸ニッケルの 2.326 g を溶解します。</li>
	</ol>
</li>
</ol>5. 化学析出法による Nb2O5の準備
<ol><li>カルサイン ニオビウム酸 (Nb2O5·nH2O) O5粒子純粋な Nb2を取得する 450 ° C で 5 時間合成空気中。 注: x 線粉末回折 (XRD) 解析、Nb2O5·nH2O は、アモルファス、Nb2O5は結晶を用いた反応の完了を確認します。分析によると、450 ° C で 5 時間焼成は反応を完了するのに十分だった。</li>
</ol>6. 2-(2-methoxyphenoxy)-1-phenylethan-1-one β O 4 リグニン モデル化合物の合成
<ol><li>Bromoacetophenone (9.0 g、45 ミリ モル) と 2-メトキシフェノール (6.6 g、53 モル) 磁性攪拌器を 500 mL の三角フラスコにジメチルホルムアミド (DMF) の 200 mL に溶解します。腐食性と発癌性の化学薬品、試薬を用いた反応を実行するのにには、適切な保護機器とヒューム フードを使用します。</li>
	<li>水酸化カリウム (3.0 g、53 モル) で上記の DMF 溶液を混合し、磁気スターラーを利用して常温で 50 rpm で混合物を一晩攪拌します。</li>
	<li>H2O の 200 mL、600 mL のジエチル エーテルの混合液に製品を抽出 (1:3 v/v) 分離漏斗を使用しています。ソリューションの上部のジエチル エーテル層を取得します。</li>
	<li>MgSO4 (10 g) ジエチル エーテル溶液中の水分を吸収するを追加します。濾紙と漏斗を用いてジエチル エーテル溶液を取得する MgSO4をフィルター処理します。</li>
	<li>回転蒸発器を用いて 0.08 MPa に減圧下でジエチル エーテル溶液を除去した後エタノール 5 mL で溶解します。</li>
	<li>ゆっくりと 10 mL のビーカーに製品を recrystallize にエタノール溶媒を蒸発させます。黄色粉体として製品 (11.5 g) を取得し、製品の歩留まりが 90 %bromoacetophenone に基づきます。1H NMR 分析、 1H NMR (DMSO) から: δ 3.78 (s、3 H OCH3)、5.54 (s、2 H、CH2)、6.82 8.01 (m、9 H、芳香) ppm。17
</li>
</ol>7. リグニン由来芳香族エーテルのフェノール
注: 選択したリグニン由来芳香族エーテルはこの実験でアニソールと触媒は Ni0.92Nb0.08o 適切な保護具と発がん性試薬を用いた反応を実行するヒューム フード。
<ol><li>ヒーターと磁性攪拌器 50 mL ステンレス製オートクレーブ原子炉を装備します。</li>
	<li>Ni0.92400 ° c 2 h H2雰囲気でオートクレーブ原子炉のステップ 2 から取得された Nb0.08O 触媒 (1 g) を削減し、アルゴン (50 mL/分) の下で触媒を一晩パッシベーションします。</li>
	<li>アニソール (1.1712 g、8 wt %) を定量ガス ・ クロマトグラフィー (GC) 分析用内部標準として n-ドデカン (0.2928 g、2 wt %) の使用とデカン (20 mL) に溶解します。</li>
	<li>空気 (< 5 分) と長い露出時間を避けるために急速にオートクレーブ反応器に還元触媒 (0.1 g) を紹介します。</li>
	<li>オートクレーブ反応器のシール、パージ H2繰り返し (3 回で 3 MPa 圧力)、空気、大気圧で反応混合物を除去するために。</li>
	<li>700 rpm で攪拌速度を設定します。</li>
	<li>2 ° C/分で 160-210 ° C で所望の温度に加熱後オートクレーブ炉 3 MPa に加圧し、ゼロの時間ポイントを設定 (t = 0)。 注: 160-210 ° C の温度はこのレポートで適切なです。</li>
	<li>その後、すぐに部屋の温度 10 ° C/分で混合物を冷却し、質量選択検出器付きガスクロマトグラフィーを用いた脱酸素化製品を分析します。17
</li>
	<li>リグニン モデル次の式に従って化合物の変換を決定します。 <img alt="Equation 1" src="/files/ftp_upload/56987/56987eq1.jpg">
</li>
	<li>次の式に従って生成物の選択性を確認します。 <img alt="Equation 2" src="/files/ftp_upload/56987/56987eq2.jpg">
</li>
</ol>

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A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cobalt+nanoparticles+as+recyclable+catalyst+for+aerobic+oxidation+of+alcohols+in+liquid+phase.">Cobalt nanoparticles as recyclable catalyst for aerobic oxidation of alcohols in liquid phase.</a> J. Nanopart. Res. 18 (5), 1-12 (2016).</li><li>Wang, K., Yang, L., Zhao, W., Cao, L., Sun, Z., Zhang, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+facile+synthesis+of+copper+nanoparticles+supported+on+an+ordered+mesoporous+polymer+as+an+efficient+and+stable+catalyst+for+solvent-free+sonogashira+coupling+Reactions.">A facile synthesis of copper nanoparticles supported on an ordered mesoporous polymer as an efficient and stable catalyst for solvent-free sonogashira coupling Reactions.</a> Green Chem. 19, 1949-1957 (2017).</li><li>Song, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High-Selectivity+Electrochemical+Conversion+of+CO2+to+Ethanol+using+a+Copper+Nanoparticle/N-Doped+Graphene+Electrode.">High-Selectivity Electrochemical Conversion of CO2 to Ethanol using a Copper Nanoparticle/N-Doped Graphene Electrode.</a> Chemistry Select. 1, 6055-6061 (2016).</li></ol>

何を開示する必要があります。

バルクのニッケルをドープしたニオブ酸化物ナノ粒子を準備する一般的な方法の 1 つは回転蒸着法です。9回転蒸発、溶媒をゆっくり除去と Ni Nb O 粒子商取引の沈殿物の処理中にさまざまな圧力や温度条件を採用しています。回転蒸着法と対照をなして本研究で報告された化学沈殿法は溶剤除去を必要としないこのナノ粒子を準備する注目を受けています。ナノ触媒を準備す...

ナノコンポジットの調製は、様々 な分野で重要な応用ゆえに注目を受けています。1,2,3,4,5,6さまざまな方法が乾燥混合方法、7など開発されている Ni-Nb-O 混合酸化物ナノ粒子を準備するには15 14熱分解法,9,10、11,12,13ゾル ゲル法8蒸着法と自動燃焼。16典型的な蒸発法9、金属前駆体の適切な量を含む水溶液ニッケル硝酸六水和物及びアンモニウム ニオブ シュウ酸に加熱した 70 ° C溶媒とさらに乾燥と焼成を除去した後、混合酸化物が得られました。これらの酸化物触媒展示優秀な触媒活性と選択性 NiO 結晶中のニオブ陽イオンの混入による電子・構造転位に関連しているエタンの酸化脱水素 (ODH) に向かって.11 Nb の挿入12エタンの酸化反応は、求電子的酸素が著しく減少しています。結果として、このメソッドの拡張機能は、混合の Ni 私 O 酸化物の種類の準備に行われているどこ私李, Mg, Al, Ga, Ti, Ta =。13金属ドーパントのバリエーションが NiO の選択的と求電子的酸素ラジカルを変更、したがって組織的にチューニング ODH 活性およびエタンに向かって選択ことがわかった。しかし、通常これらの酸化物の表面の面積は比較的小さい (< 100 m2/g)、拡張相分離と大規模な Nb2O5微結晶の形成のためにし、従って他の触媒の使用を妨げアプリケーション。
乾燥混合処理工法、固体の研磨法とも呼ばれますは、混合酸化物触媒を準備するもう一つの一般的に使用されるメソッドです。触媒材料は無溶剤型の方法で得られる、ので、このメソッドは、複合酸化物の作製に有望な緑と持続可能な代替手段を提供します。このメソッドによって得られる最高の表面積は Ni80焼成温度 250 ° C で Nb20 172 m2/g8ただし、この固体メソッドはない信頼性の高い反応が原子スケールでよく混合されていないものとして。したがって、化学的均一性と特定の粒子サイズ分布と形態のより良いコントロールの Ni-Nb-O を準備する他の適当な方法混合酸化物ナノ粒子はまだ求められています。7
ナノ粒子の開発にさまざまな戦略の中で、化学沈殿物は、金属イオンの完全な沈殿物をことができますので、ナノ触媒を開発する有力な方法の一つとして提供しています。また、高い表面領域のナノ粒子はよくこのメソッドを使用して準備されます。ニーニョ Nb ナノ粒子の触媒特性を改善するために本明細書化学沈殿法による一連の高表面積と Ni-Nb-O 混合酸化物触媒の合成のためのプロトコルを報告します。我々 は Nb:Ni のモル比がに向かってリグニン由来有機物のフェノール酸化物の触媒活性を決定する上で重要な要因であることを実証しました。0.087 上高 Nb:Ni 比と非アクティブな NiNb2O6種が形成されました。Ni0.92Nb0.08最大の表面積 (173 m2/g) を持っていた、O 倍のようなナノシート構造および最高の活動とシクロヘキサンをアニソールのフェノールへの選択性を示した。

<table><tbody><tr><td>Niobium(V) oxalate hydrate, 98%</td><td>Alfa</td><td>L04481902</td><td></td></tr><tr><td>Nickel nitrate hexahydrate, 99%</td><td>Aladdin</td><td>N108891</td><td></td></tr><tr><td>Sodium hydroxide, 98%</td><td>Aladdin</td><td>S111501</td><td></td></tr><tr><td>Ammonium hydroxide, 23-25%</td><td>Aladdin</td><td>A112077</td><td></td></tr><tr><td>Anisole, 99%</td><td>Sinopharm</td><td>81001728</td><td></td></tr><tr><td>Diphenyl ether, 98%</td><td>Aladdin</td><td>D110644</td><td></td></tr><tr><td>Phenol, 98%</td><td>Sinopharm</td><td>100153008</td><td></td></tr><tr><td>2-Methoxyphenol, 98%</td><td>Sinopharm</td><td>30114526</td><td></td></tr><tr><td>Vanillin, 99.5%</td><td>Sinopharm</td><td>69024316</td><td></td></tr><tr><td>Potassium hydroxide, AR</td><td>Aladdin</td><td>P112284</td><td></td></tr><tr><td>N,N-Dimethylformamide, 99.5%</td><td>Sinopharm</td><td>40016462</td><td></td></tr><tr><td>2-Bromoacetophenone,98%</td><td>Aladdin</td><td>B103328</td><td></td></tr><tr><td>Diethyl ether,99.5%</td><td>Sinopharm</td><td>10009318</td><td></td></tr><tr><td>Decane,98%</td><td>Aladdin</td><td>D105231</td><td></td></tr><tr><td>Dodecane,99%</td><td>Aladdin</td><td>D119697</td><td></td></tr><tr><td>Niobic acid</td><td>CBMM</td><td>1313968</td><td></td></tr><tr><td>Heating and Drying Oven</td><td></td><td></td><td>DHG Series (shanghai jinghong laboratory instrument co. ltd)</td></tr><tr><td>Autoclave Reactor</td><td></td><td></td><td>CJF-0.05&amp;mdash;0.1L (Dalian Tongda Equipment Technology Development Co., Ltd)</td></tr><tr><td>Tube&amp;nbsp;furnace</td><td></td><td></td><td>SK2-1-10/12 (Luoyang Huaxulier Electric Stove Co., Ltd)</td></tr><tr><td>Heating magnetic stirrer</td><td></td><td></td><td>DF-101 (Yu Hua Instrument Co. Ltd.)</td></tr><tr><td>Rotary evaporator</td><td></td><td></td><td>RE-3000A (Shanghai Yarong Biochemical Instrument Factory)</td></tr><tr><td>Synthetic air</td><td></td><td></td><td></td></tr><tr><td>Hydrogen gas</td><td></td><td></td><td></td></tr><tr><td>Argon gas</td><td></td><td></td><td></td></tr></tbody></table>

chemical precipitation method for the synthesis of nb2o5 modified bulk nickel catalysts with high specific surface area

NixNb1 xO 触媒スポンジ状と倍のようなナノ構造体の合成法を示す.NixNb1 xO ナノ粒子原子組成の異なるシリーズの Nb:Ni 比を変化させることにより (x = 0.20 0.15、0.08 0.03) 化学沈殿物によって準備されています。これらの NixNb1 xO 触媒は、走査型電子顕微鏡、x 線光電子分光法、x 線回折によって特徴付けられます。研究は、Ni0.97Nb0.03O のスポンジのようなおよび倍のような外観と Ni0.92Nb0.08O NiO 表面とこれら NixNb1 xO 触媒、バルクと比較して表面積を明らかにしました。NiO。Ni0.92Nb0.08O 触媒の 173 m2/g の最大の表面積が得られます。さらに、合成した Ni0.92Nb0.08O 触媒を用いたリグニン由来化合物の触媒の水素転換反応を検討しました。

X 線回折 (XRD) パターン (図 1および図 2) BET 比表面積、昇温化と水素 (H2- TPR)、走査電子顕微鏡 (SEM) と、エネルギー分散 x 線 (EDX を装備) ナノ粒子の NiO、Ni-Nb-O と Nb2O5酸化物17 (図 3および図 4) 収集されたアナライザー、x 線光電子分光法 (X...

Watch this Scientific Journal Video about Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area at JoVE.com

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

スポンジのような折るような Ni1 x化学沈殿物によって NbxO ナノ粒子の合成のためのプロトコルが表示されます。

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 ...

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Research

JoVE Journal

Chemistry

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

11.8K ビュー.  Dalian University of Technology. スポンジのような折るような Ni1 x化学沈殿物によって NbxO ナノ粒子の合成のためのプロトコルが表示されます。

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

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

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 ...

工学

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 ...

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

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity in aqueous CO2 reduction. Different from traditional metal nanocrystals, the synthesis of metal single atoms involves a matrix material that can confine those single atoms and prevent them from aggregation. We report an electrospinning and thermal annealing method to prepare Ni single atoms dispersed and coordinated in a graphene shell, as active centers for CO2 reduction to CO. During the synthesis, N dopants play a critical role in generating graphene vacancies to trap Ni atoms. Aberration-corrected scanning transmission electron microscopy and three-dimensional atom probe tomography were employed to identify the single Ni atomic sites in graphene vacancies. Detailed setup of electrochemical CO2 reduction apparatus coupled with an on-line gas chromatography is also demonstrated. Compared to metallic Ni, Ni single atom catalyst exhibit dramatically improved CO2 reduction and suppressed H2 evolution side reaction.

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

Here, we present a protocol for the synthesis and electrochemical testing of transition metal single atoms coordinated in graphene vacancies as active centers for selective carbon dioxide reduction to carbon monoxide in aqueous solutions.

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

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

A Continuous-flow Photocatalytic Reactor for the Precisely Controlled Deposition of Metallic Nanoparticles

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic nanoparticles is developed. Guidelines for the replication of the reactor and its operation are provided in detail. Three different composite systems (Pt/graphene, Pt/TiO2, and Au/TiO2) with monodisperse and uniformly distributed particles are produced by this reactor, and the photodeposition mechanism, as well as the synthesis optimization strategy, are discussed. The synthesis methods and their technical aspects are described comprehensively. The role of the ultraviolet (UV) dose (in each excitation pulse) on the photodeposition process is investigated and the optimum values for each composite system are provided.

For a continuous and scalable synthesis of noble-metal-based nanocomposites, a novel photocatalytic reactor is developed and its structure, operation principles, and product quality optimization strategies are described.

金属ナノ粒子の正確に制御された沈着量の連続的な流れの光触媒反応

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic ...

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 ...

Preparation of Silver-Palladium Alloyed Nanoparticles for Plasmonic Catalysis under Visible-Light Illumination

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular transformations. This opens possibilities for the use of visible or near-IR light as a sustainable input to drive and control reactions when plasmonic nanoparticles supporting LSPR excitation in these ranges are employed as catalysts. Unfortunately, this is not the case for several catalytic metals such as palladium (Pd). One strategy to overcome this limitation is to employ bimetallic NPs containing plasmonic and catalytic metals. In this case, the LSPR excitation in the plasmonic metal can contribute to accelerate and control transformations driven by the catalytic component. The method reported herein focuses on the synthesis of bimetallic silver-palladium (Ag-Pd) NPs supported on ZrO2 (Ag-Pd/ZrO2) that acts as a plasmonic-catalytic system. The NPs were prepared by co-impregnation of corresponding metal precursors on the ZrO2 support followed by simultaneous reduction leading to the formation of bimetallic NPs directly on the ZrO2 support. The Ag-Pd/ZrO2 NPs were then used as plasmonic catalysts for the reduction of nitrobenzene under 425 nm illumination by LED lamps. Using gas chromatography (GC), the conversion and selectivity of the reduction reaction under the dark and light irradiation conditions can be monitored, demonstrating the enhanced catalytic performance and control over selectivity under LSPR excitation after alloying non-plasmonic Pd with plasmonic metal Ag. This technique can be adapted to a wide range of molecular transformations and NPs compositions, making it useful for the characterization of the plasmonic catalytic activity of different types of catalysis in terms of conversion and selectivity.

Presented here is a protocol for the synthesis of silver-palladium (Ag-Pd) alloy nanoparticles (NPs) supported on ZrO2 (Ag-Pd/ZrO2). This system allows for harvesting energy from visible light irradiation to accelerate and control molecular transformations. This is illustrated by nitrobenzene reduction under light irradiation catalyzed by Ag-Pd/ZrO2 NPs.

可視光照明下におけるプラスモニック触媒のための銀パラジウム合金ナノ粒子の調製

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular ...

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 ...

マイクロ波による水酸化ニッケルナノシートの合成と評価

Effect of Microwave Synthesis Conditions on the Structure of Nickel Hydroxide Nanosheets

A protocol for rapid, microwave-assisted hydrothermal synthesis of nickel hydroxide nanosheets under mildly acidic conditions is presented, and the effect of reaction temperature and time on the material&#39;s structure is examined. All reaction conditions studied result in aggregates of layered &#945;-Ni(OH)2 nanosheets. The reaction temperature and time strongly influence the structure of the material and product yield. Synthesizing &#945;-Ni(OH)2 at higher temperatures increases the reaction yield, lowers the interlayer spacing, increases crystalline domain size, shifts the frequencies of interlayer anion vibrational modes, and lowers the pore diameter. Longer reaction times increase reaction yields and result in similar crystalline domain sizes. Monitoring the reaction pressure in situ shows that higher pressures are obtained at higher reaction temperatures. This microwave-assisted synthesis route provides a rapid, high-throughput, scalable process that can be applied to the synthesis and production of a variety of transition metal hydroxides used for numerous energy storage, catalysis, sensor, and other applications.

著者スポットライト:水酸化ニッケルナノシートの迅速なマイクロ波支援水熱合成 

Nickel hydroxide nanosheets are synthesized by a microwave-assisted hydrothermal reaction. This protocol demonstrates that the reaction temperature and time used for microwave synthesis affects the reaction yield, crystal structure, and local coordination environment.

マイクロ波合成条件が水酸化ニッケルナノシートの構造に及ぼす影響

A protocol for rapid, microwave-assisted hydrothermal synthesis of nickel hydroxide nanosheets under mildly acidic conditions is presented, and the effect ...

Nb₂O₅の合成化学沈殿法変更高表面積一括ニッケル触媒

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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

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

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

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

金属ナノ粒子の正確に制御された沈着量の連続的な流れの光触媒反応

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

可視光照明下におけるプラスモニック触媒のための銀パラジウム合金ナノ粒子の調製

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

マイクロ波合成条件が水酸化ニッケルナノシートの構造に及ぼす影響

Nb2O5の合成化学沈殿法変更高表面積一括ニッケル触媒

要約

さらに動画を探す

この動画の章

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

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

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

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

金属ナノ粒子の正確に制御された沈着量の連続的な流れの光触媒反応

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

可視光照明下におけるプラスモニック触媒のための銀パラジウム合金ナノ粒子の調製

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

マイクロ波合成条件が水酸化ニッケルナノシートの構造に及ぼす影響

Nb₂O₅の合成化学沈殿法変更高表面積一括ニッケル触媒

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

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