Name: solvothermal synthesis of mil-96 and uio-66-nh2 on atomic layer deposited metal oxide coatings on fiber mats
Uploaded: 2018-06-13T14:45:00.000+00:00
Duration: 6 min
Description: Watch this Scientific Journal Video about Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats at JoVE.com

著者は、RTI インターナショナル、米国陸軍ナティック兵士 RD & E センター、エッジウッド化学と生物センターで彼らの共作者をありがとうございます。彼らはまた彼らの資金源、防衛脅威の減少代理店を感謝します。

1 Al2O3繊維マットの上の原子層堆積法 (ALD)
<ol><li>原子炉ボート (薄い、剛性、金属メッシュ ホルダー) に 2.54 x 2.54 cm2ポリプロピレンの生地サンプルを配置します。原子炉の模式図を図 2に示します。</li>
	<li>圧力計を開きます。原子炉キャップから留め金を削除します。LabView システムで手動制御をオンにします。ALD リアクターのキャリア窒素およびゲート バルブを閉じます。ベント窒素を開きます。</li>
	<li>原子炉キャップを除去した後に、ALD リアクターに生地サンプルを読み込みます。原子炉のキャップを交換し、ゲート弁を開きます。口を閉じて、キャリア窒素を開きます。手動制御をオフにします。</li>
	<li>Al2O3生地のレシピをロードします。レシピが 1.2 ポリプロピオネート (TMA) 線量の代わりに s、30 s 乾燥窒素続いてパージまたは 1 のための水の線量 60 s 乾燥窒素続いて s パージします。レシピ 1000 サイクルを実行するを設定します。</li>
	<li>20 cfm と炉内温度 90 ° c (84 ° C 炉インターフェイス上) にマスフロー コント ローラーを設定します。</li>
	<li>TMA と水に手動バルブを開きます。圧力計を閉じます。原子炉キャップ留め金を交換してください。インターフェイスの開始を押します。</li>
	<li>レシピを修了すると、圧力ゲージを開きます。原子炉キャップから留め金を削除します。システムの手動制御をオンに。ALD リアクターのキャリア窒素およびゲート バルブを閉じます。ベント窒素を開きます。</li>
	<li>原子炉のキャップとサンプルのボートを削除します。原子炉を再シールします。 注: 手順はこの時点で一時停止可能性があります。</li>
</ol>2 ポリアミド 6 (PA 6) 繊維のマットの TiO2の原子層堆積法 (ALD)
<ol><li>原子炉ボート (薄い、剛性、金属メッシュ ホルダー) に 2.54 x 2.54 cm2 PA 6 の生地のサンプルを置きます。</li>
	<li>圧力計を開きます。原子炉キャップから留め金を削除します。LabView システムで手動制御をオンにします。ALD リアクターのキャリア窒素およびゲート バルブを閉じます。ベント窒素を開きます。</li>
	<li>原子炉キャップを除去した後に、ALD リアクターに生地サンプルを読み込みます。原子炉のキャップを交換し、ゲート弁を開きます。口を閉じて、キャリア窒素を開きます。手動制御をオフにします。</li>
	<li>生地の TiO2のレシピをロードします。レシピは TiCl4 1 線量の代わりに s、続いて 40 s 乾燥窒素パージまたは線量の 1 のための水 s 60 s 乾燥窒素続いてパージします。レシピ 300 サイクルを実行するを設定します。</li>
	<li>20 cfm と炉内温度 90 ° c (84 ° C 炉インターフェイス上) にマスフロー コント ローラーを設定します。</li>
	<li>TiCl4と水に手動バルブを開きます。圧力計を閉じます。原子炉キャップ留め金を交換してください。インターフェイスの開始を押します。</li>
	<li>レシピを修了すると、圧力ゲージを開きます。原子炉キャップから留め金を削除します。システムの手動制御をオンに。ALD リアクターのキャリア窒素およびゲート バルブを閉じます。ベント窒素を開きます。</li>
	<li>原子炉のキャップとサンプルのボートを削除します。原子炉を再シールします。 注: 手順はこの時点で一時停止可能性があります。</li>
</ol>3 ミル 96 のソルボサーマル合成
<ol><li>ガラス、80 mL のビーカーに H3BTC の 0.0878 g を追加します。</li>
	<li>H2O の 12 mL とエタノールの 12 mL をビーカーに追加します。</li>
	<li>10 分の磁気または H3BTC は完全に溶解するまで攪拌します。</li>
	<li>ライニング テフロン加圧容器にソリューションを配置します。</li>
	<li>Al2O3コーティング ソリューションにポリプロピレンと容器の底をフラットに入らないのでメッシュ サポートの生地を支える追加します。</li>
	<li>圧力容器を密封し、110 ° C で 24 時間の炉。</li>
	<li>クールにサンプルを可能にした後ビーカーにメッシュ バスケットに生地サンプルを配置します。エタノールは、12 時間ごとに 2 回洗います。</li>
	<li>サンプルの活性化は、真空下で 6 時間 85 ° C で加熱を必要とする真空下で 12 h 110 ° C で加熱が続きます。 注: 手順をここで停止できます。すべてのサンプルは、サンプル活性化を維持するために乾燥器で格納する必要があります。</li>
</ol>4. UiO-66-NH2のソルボサーマル合成
<ol><li>20 mL バイアル シンチレーションに ZrCl4 0.08 g を追加します。</li>
	<li>N, N-ジメチルホルムアミド (DMF) を 5 mL ずつ ZrCl4に 20 mL を追加します。単位間にバイアルのキャップし、放散するガスを許可します。</li>
	<li>1 分のためのソリューションを超音波照射します。</li>
	<li>、バイアルに 2 aminoterephthalic 酸 0.062 g を追加し、磁気攪拌 5 分のためのソリューション。</li>
	<li>バイアルに 25 μ L の脱イオン水を追加します。</li>
	<li>バイアルに 1.33 の mL の濃塩酸を追加します。</li>
	<li>ソリューションの TiO2 ALD コーティング生地見本が水没し、バイアルのキャップします。</li>
	<li>24 h 85 ° c の炉にサンプルを配置します。</li>
	<li>クールにサンプルを可能にした後ビーカーにメッシュ バスケットに生地サンプルを配置します。DMF、12 h. 洗浄 12 h ごとのエタノールの 80 mL で 3 回ごとの 80 mL で 2 回洗浄します。</li>
	<li>生地見本を削除した後に、残留の MOF 粉をフィルター処理します。DMF、12 h. 洗浄 12 h ごとのエタノールの 80 mL で 3 回ごとの 80 mL で 2 回洗浄します。</li>
	<li>サンプルの活性化は、真空下で 6 時間 85 ° C で加熱を必要とする真空下で 12 h 110 ° C で加熱が続きます。 注: 手順をここで停止できます。すべてのサンプルは、サンプル活性化を維持するために乾燥器で格納する必要があります。</li>
</ol>

<ol>
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ALD コーティングは、接着と MOF の読み込みに強く影響します。まず、基板と ALD 前駆体の種類に応じて ALD レイヤー、線維の周りの外殻を形成したり、金属酸化物コーティング20への緩やかな移行を作成する繊維に拡散します。適切な条件下におけるポリプロピレンの拡散層を観察できる間、綿とナイロンの基板上にハード シェルを観察されています。第二に、光ファイバー...

金属有機性フレームワークは、大きな気孔率と表面積を提供する有機分子リンカーによって架橋反応性金属クラスター中心から成る結晶構造です。その構造、気孔率、および機能は、リンカー、7,000 m2/gMOF1,2の高表面積につながる適切なクラスターを選択して設計できます。彼らの高い空隙率と表面積をした Mof まちまち適用、吸着、分離、触媒エネルギー生産から生物学的プロセス1,3、環境問題まで幅広い分野で 4,5,6。
多数の Mof 揮発性有機化合物と温室効果ガスを選択的に吸着または人間の健康や環境に有害証明するかもしれない化学物質を触媒劣化に成功を収めています。特に、弱いルイス酸のアルを金属クラスター7に存在と調整する窒素グループで孤立電子対の電子の可用性のため窒素揮発性有機化合物 (Voc) を選択的に吸着するミル-96 (Al) を示しています。ミル-96 は、CO2、 pなどのガスを吸着する示されている-キシレンとm-キシレン8,9。MOF 吸着選択性、気孔のサイズと同様、金属クラスターの両方ルイス酸に依存します。ミル 96 の細孔径は、温度上昇とトリメチル ベンゼン暴露の吸着量の増加容量内の温度とともに増加して吸着温度9選択性をチューニングの機会を提示します。
ここでの焦点の 2 番目の MOF、UiO-66-NH2触媒化学兵器剤 (CWAs) と模造を低下するのに示されています。リンカーのアミン グループは、ジルコニウム クラスターに不可逆的に結合し、MOF10の中毒から劣化品を防止しながら神経剤を分解で相乗効果を提供します。UiO-66-NH2が触媒加水分解ジメチルpnitrophenylphosphate (DMNP) 最短でバッファーに格納された状態で 0.7 分の半減期で約 20 倍、基本 MOF UiO-6611,12よりも速く。
Mof は、主にバルク粉の物理的な形が MOF の大きなバルクを追加、目詰まり毛穴、減らしたりせずガス回収、ろ過のためのプラットフォームに組み込むことは困難することができますこれらの吸着と触媒特性は有望なのですが、柔軟性。代わりに、修飾 MOF 生地を作成します。Mof は、スプレー コーティング、ソルボサーマル成長、マイクロ波合成と層によって成長方法13,14エレクトロスピニング MOF パウダー/ポリマー スラリー、接着剤のミックスを含む無数の方法で生地に組み込まれています。,15,16,17,18. これらのエレクトロスピニングと高分子接着剤、MOF の機能的なサイトをブロックと、ため有意に吸着・反応性ポリマーでカプセル化します。さらに、これらの技術の多くは視界困難または貧しい接着/発生・純粋静電相互作用依存による繊維にコーティングを作成する失敗します。MOF18,19表面相互作用より強いために金属酸化物の生地の最初のコートする代替方法です。
金属酸化物成膜方法の 1 つは、原子層堆積法 (ALD) です。ALD は、等角の薄膜、原子スケールに制御の手法です。プロセスは 2 つを利用してコーティングする基板の表面にのみ半分の反応。最初の手順は、線量の過剰反応がシステムから削除される間、金属表面を残して表面の水酸基と反応する、前兆を含む金属です。第二の反応は酸素を含む反応、通常金属酸化物を形成する金属のサイトと反応する水です。もう一度、水を過剰し、の反応生成物がシステムから削除されます。これらの交互投与量とパージは、必要な膜厚が得られるまで繰り返すことができます (図 1)。原子層堆積法は、小規模蒸気相前駆体繊維のマットなど、複雑なトポロジを有する基板のすべての面に等角のフィルムを可能にするために特に役立ちます。また、ポリプロピレンなどの高分子、ALD の条件は将来 MOF 成長20の強力なアンカーを提供する繊維表面に拡散して塗装できます。
金属酸化物コーティングにより繊維の高められた核生成サイト伝統的なソルボサーマル合成中に官能基と粗さ18,20増加します。私たちのグループ以前を示している ALD 金属酸化物ベース層 UiO 6 X、HKUST-1、ソルボサーマル層によって、ヒドロキシ二重塩変換方法13,17、さまざまな経路を通じて他の合成に効果的 18,21,22,23。ここで我々 は 2 つの合成タイプを示します。ミル材料は、MOF に直接有機リンカーの拡散による Al2O3 ALD コーティングを変換することによって形成されます。Al2O の3 ALD コーティング繊維マット trimesic 酸溶液で加熱、水没によってフォーム ミル 96 に金属酸化物コーティングに有機リンカーを拡散させます。これは、結果、すべての繊維の表面に強く付着、等角の MOF コーティング。2 番目の合成方法、金属、有機前駆体を使用して典型的な UiO-66-NH2水熱合成ですが MOF は nucleates を金属酸化物被覆繊維マットを追加します。両方の合成方法の結果の製品から成る MOF の等角薄膜結晶は強く支持の生地に付着します。ミル-96 の場合これらは、無揮発性有機化合物や温室効果ガスの吸着のためのフィルターに組み込むことができます。UiO-66-NH2これらの生地は簡単に軍人、最初のレスポンダーと CWA 攻撃連続防衛の一般市民のために軽量防護服に組み込むことができます。

<table><tbody><tr><td>trimethylaluminum</td><td>Strem Chemicals</td><td>93-1360</td><td></td></tr><tr><td>home-built ALD reactor</td><td>N/A</td><td></td><td></td></tr><tr><td>nitrogen cylinder</td><td>Arc3</td><td>UN1066</td><td></td></tr><tr><td>trimesic acid</td><td>Sigma-Aldrich</td><td>482749-500G</td><td></td></tr><tr><td>ethanol</td><td>Koptec</td><td>V1001</td><td></td></tr><tr><td>teflon lined autoclave</td><td>PARR Instrument Company</td><td>4760-1211</td><td></td></tr><tr><td>isotemp furnace</td><td>Fisher Scientific</td><td>F47925</td><td></td></tr><tr><td>Zirconium (IV) chloride</td><td>Alfa Aesar</td><td>12104</td><td></td></tr><tr><td>2-aminoterephthalic acid</td><td>Acros Organics</td><td>278031000</td><td></td></tr><tr><td>N,N-dimethylformamide</td><td>Fisher Scientific</td><td>D119-4</td><td></td></tr><tr><td>Hydrochloric Acid</td><td>Fisher Scientific</td><td>A481-212</td><td></td></tr><tr><td>Polypropylene fiber mats</td><td>N/A</td><td></td><td></td></tr><tr><td>Polyamide fiber mats</td><td>N/A</td><td></td><td></td></tr></tbody></table>

solvothermal synthesis of mil-96 and uio-66-nh2 on atomic layer deposited metal oxide coatings on fiber mats

反応性金属クラスターと大きな気孔率と表面積を可能にする有機配位子を含んだ有機金属フレームワーク (Mof) は、ガス吸着、分離、触媒作用で効果的な実証されています。Mof は、粉体の気孔率および吸着能力の低下リスク機能デバイスとファブリックをそれらを遵守する追加のプロセスを必要とするバルク粉末として最も一般的合成されます。ここでは、金属酸化物薄膜の原子層堆積法 (ALD) を使用して、最初のコーティング生地のメソッドを示します。このプロセスは、MOF 核形成反応表面を提供しながら各繊維に制御可能な厚さの等角のフィルムを作成します。ソルボサーマル MOF の合成時に、ソリューションに ALD コーティング生地を水没によって、Mof 作成共、よく付着コーティング繊維の MOF 毛穴をブロック可能性があります追加付着物なしの MOF 機能ファブリックの結果と機能的なサイト。ここで 2 つのソルボサーマル合成法を示す.最初に、金属酸化物を MOF に変換する合成の条件を用いたポリプロピレン繊維の MIL-96(Al) 層を形成します。さまざまな厚みの初期の無機膜を使用して、無機に有機リンカーの拡散により、MOF の範囲を制御するファブリック上の読み込み。第二に、ポリアミド 6 (PA 6) 繊維にコーティング、それにより生地に MOF の制服と共形薄膜フィルムの生産の等角の金属の酸化物の UiO-66-NH2 MOF は nucleates、ソルボサーマル合成を実行します。得られた材料はフィルター デバイスや防護服に直接組み込むことが、ルース パウダーの不器用の資質を排除します。

MOF/生地材料を記述するには、測定の表面領域に関連する 2 つの条件の輪郭を描きます。最初、投影面積、cm2投影、つまり定規で測るように生地見本の巨視的サイズを指します。、サンプルのシャドウを投影します。関心の 2 番目の面積は 77 K で得られる窒素等温線から計算した比表面積です。これらの値は、単位を m2/g生地m<sup...

Watch this Scientific Journal Video about Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats at JoVE.com

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

金属有機性フレームワークは、スマート材料を組み込むことは困難の緩い粉末で典型的な合成方法の結果、触媒、ガス貯蔵に効果的です。ソルボサーマル合成時に生地の MOF の等角のフィルムに終って ALD 金属酸化物でコーティング生地を最初のメソッドを紹介します。

ミル-96、UiO-66-NH2原子層のソルボサーマル合成繊維のマット上金属酸化皮膜に堆積

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven ...

solvothermal-synthesis-mil-96-uio-66-nh2-on-atomic-layer-deposited

Universidad de Cartagena UDEC

Research

JoVE Journal

Chemistry

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

11.4K ビュー.  North Carolina State University. 金属有機性フレームワークは、スマート材料を組み込むことは困難の緩い粉末で典型的な合成方法の結果、触媒、ガス貯蔵に効果的です。ソルボサーマル合成時に生地の MOF の等角のフィルムに終って ALD 金属酸化物でコーティング生地を最初のメソッドを紹介します。

ビデオ: Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

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

Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in combination with their outstanding thermal and chemical stability, and low densities. However, their insoluble nature causes problems in their processing since usually applied techniques such as spin coating are not available. Especially for membrane applications, where the processing of CMP as thin films is desirable, the processing problems have hindered their commercial application.
Here we describe the interfacial synthesis of CMP thin films on functionalized substrates via molecular layer-by-layer (l-b-l) synthesis. This process allows the preparation of films with desired thickness and composition and even desired composition gradients.
The use of sacrificial supports allows the preparation of freestanding membranes by dissolution of the support after the synthesis. To handle such ultra-thin freestanding membranes the protection with sacrificial coatings showed great promise, to avoid rupture of the nanomembranes. To transfer the nanomembranes to the desired substrate, the coated membranes are upfloated at the air-liquid interface and then transferred via dip coating.

In this paper we describe the interfacial synthesis of conjugated microporous polymers (CMP) on sacrificial substrates, and the dissolution of the substrate for the preparation of freestanding CMP nanomembranes. In addition, we will describe how the fragile nanomembranes can be transferred to other substrates.

層ごとの合成と自立共役高分子ナノ薄膜マイクロポーラスの譲渡

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in ...

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 and a superhydrophobic agent were coated on the HGM surface in one step. TBT and PFOTES were selected as the Ti source and the superhydrophobic agent, respectively. They were both coated on the HGM, and after the hydrothermal process, the TBT turned to anatase TiO2. In this way, a PFOTES/TiO2-coated HGM (MCHGM) was prepared. For comparison, PFOTES single-coated HGM (F-SCHGM) and TiO2 single-coated HGM (Ti-SCHGM) were synthesized as well. The PFOTES and TiO2 coatings on the HGM surface were demonstrated through X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive detector (EDS) characterizations. The MCHGM showed a higher contact angle (153&#176;) but a lower sliding angle (16&#176;) than F-SCHGM, with a contact angle of 141.2&#176; and a sliding angle of 67&#176;. In addition, both Ti-SCHGM and MCHGM displayed similar IR reflectivity values, which were about 5.8% higher than the original HGM and F-SCHGM. Also, the PFOTES coating barely changed the thermal conductivity. Therefore, F-SCHGM, with a thermal conductivity of 0.0479 W/(m&#183;K), was quite like the original HGM, which was 0.0475 W/(m&#183;K). MCHGM and Ti-SCHGM were also similar. Their thermal conductivity values were 0.0543 W/(m&#183;K) and 0.0543 W/(m&#183;K), respectively. The TiO2 coating slightly increased the thermal conductivity, but with the increase in reflectivity, the overall heat-insulation property was enhanced. Finally, since the IR-reflecting property is provided by the HGM coating, if the coating is fouled, the reflectivity decreases. Therefore, with the superhydrophobic coating, the surface is protected from fouling, and its lifetime is also prolonged.

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

This manuscript proposes a soft-chemistry method to synthesize superhydrophobic, TiO2-coated hollow glass microspheres (HGM) with high IR-reflective properties.

たTiO<sub&gt; 2</subソフト化学法により合成超疎水性と高IR反射特性を持つ&gt;でコーティングされた中空ガラスマイクロスフェア

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

によってナノ構造イットリア安定化ジルコニア（YSZ）足場の高温製作<em&gt;その場での</em&gt;カーボンテンプレート化キセロゲル

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

工学

Electrophoretic Crystallization of Ultrathin High-performance Metal-organic Framework Membranes

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and non-porous supports (polymer, ceramic, metal, carbon, and graphene). We developed a novel crystallization technique, which is termed the ENACT approach: the electrophoretic nuclei assembly for the crystallization of highly intergrown thin films (ENACT). This approach allows for a high density of heterogeneous nucleation of MOFs on a chosen substrate via the electrophoretic deposition (EPD) directly from the precursor sol. The growth of well-packed MOF nuclei leads to a highly intergrown polycrystalline MOF film. We show that this simple approach can be used for the synthesis of thin, intergrown zeolite imidazole framework (ZIF)-7 and ZIF-8 films. The resulting 500 nm-thick ZIF-8 membranes show a considerably high H2 permeance (8.3 x 10-6 mol m-2 s-1 Pa-1) and ideal gas selectivities (7.3 for H2/CO2, 15.5 for H2/N2, 16.2 for H2/CH4, and 2655 for H2/C3H8). An attractive performance for C3H6/C3H8 separation is also achieved (a C3H6 permeance of 9.9 x 10-8 mol m-2 s-1 Pa-1 and a C3H6/C3H8 ideal selectivity of 31.6 at 25 &#176;C). Overall, the ENACT process, owing to its simplicity, can be extended to synthesize intergrown thin films of a wide range of nanoporous crystalline materials.

A simple, reproducible, and versatile approach for the synthesis of intergrown, polycrystalline metal-organic framework membranes on a wide range of unmodified porous and non-porous supports is presented.

極薄高性能金属有機性フレームワーク膜の電気泳動の結晶化

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and ...

Molten-Salt Synthesis of Complex Metal Oxide Nanoparticles

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. Here, we introduce the molten-salt synthesis (MSS) method for making metal oxide nanomaterials. Advantages over other methods include its simplicity, greenness, reliability, scalability, and generalizability. Using pyrochlore lanthanum hafnium oxide (La2Hf2O7) as a representative, we describe the MSS protocol for the successful synthesis of complex metal oxide nanoparticles (NPs). Furthermore, this method has the unique ability to produce NPs with different material features by changing various synthesis parameters such as pH, temperature, duration, and post-annealing. By fine-tuning these parameters, we are able to synthesize highly uniform, non-agglomerated, and highly crystalline NPs. As a specific example, we vary the particle size of the La2Hf2O7&#160;NPs by changing the concentration of the ammonium hydroxide solution used in the MSS process, which allows us to further explore the effect of particle size on various properties. It is expected that the MSS method will become a more popular synthesis method for nanomaterials and more widely employed in the nanoscience and nanotechnology community in the upcoming years.

Here, we demonstrate a unique, relatively low-temperature, molten-salt synthesis method for preparing uniform complex metal oxide lanthanum hafnate nanoparticles.

複合金属酸化物ナノ粒子の溶融塩合成

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared according to the methodology developed by surface organometallic chemistry (SOMC). In this framework, catalytic cycles can be determined by isolating crucial intermediates. All air-sensitive materials are handled under inert atmosphere (using gloveboxes or a Schlenk line) or high vacuum lines (HVLs, &#60;10-5 mbar). The preparation of SiO2-700 (silica dehydroxylated at 700 &#176;C) and subsequent applications (the grafting of complexes and catalytic runs) requires the use of HVLs and double-Schlenk techniques. Several well-known characterization methods are used, such as Fourier-transform infrared spectroscopy (FTIR), elemental microanalysis, solid-state nuclear magnetic resonance spectroscopy (SSNMR), and state-of-the-art dynamic nuclear polarization surface enhanced NMR spectroscopy (DNP-SENS). FTIR and elemental microanalysis permit scientists to establish the grafting and its stoichiometry. 1H and 13C SSNMR allows the structural determination of the hydrocarbon ligands coordination sphere. DNP SENS is an emerging powerful technique in solid characterization for the detection of poorly sensitive nuclei (15N, in our case). SiO2-700 is treated with about one equivalent of the metal precursor compared to the amount of surface silanol (0.30 mmol&#183;g-1) in pentane at room temperature. Then, volatiles are removed, and the powder samples are dried under dynamic high vacuum to afford the desired materials [(&#8801;Si-O-)Hf(&#951;2&#960;-MeNCH2)(&#951;1-NMe2)(&#951;1-HNMe2)]. After a thermal treatment under high vacuum, the grafted complex is converted into metal imido silica complex [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)]. [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] effectively promotes the metathesis of imines, using the combination of two imine substrates, N-(4-phenylbenzylidene)benzylamine, or N-(4-fluorobenzylidene)-4-fluoroaniline, with N-benzylidenetert-butylamine as substrates. A significantly lower conversion is observed with the blank runs; thus, the presence of the imido group in [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is correlated to the catalytic performance.

A new group IV metal catalyst for imine metathesis is prepared by grafting amine metal complex onto dehydroxylated silica. Surface metal fragments are characterized using FT-IR, elemental microanalysis, and solid-state NMR spectroscopy. Further dynamic nuclear polarization surface enhanced NMR spectroscopy experiments complement the determination of the coordination sphere.

表面有機金属化学の方法論を用いてシリカ支持触媒によるイミンメタセシス

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...

Metal Oxide Heterojunction for Photocatalytic Activities

There is a significant global demand for improvements in synthesis techniques and their optimal characteristics, especially for industrial-scale applications. Sol-gel-based solution combustion synthesis (SG-SCS) is a simple method to produce ordered porous materials. In this regard, Pearson&#39;s hard and soft acids and bases theory assists in selecting host-dopant reactivity to form a proper heterojunction.
The formation of a heterojunction also changes the essential properties of the materials, improving photocatalysis via charge transfer or synergistic activities. A calcination temperature of 500 &#176;C is ideal for this process based on the results of the stability assessment via a differential thermogravimetry ratio analysis (DTG).
The nanoscale dimensions of the nanoparticles (NPs) and nanocomposites (NCs) generated were validated using X-ray diffraction and high-resolution transmission electron microscopy (HRTEM). Furthermore, the scanning electron microscopy micrographs and BET analyses confirmed the porosity nature of the materials. HRTEM, X-ray photoelectron spectroscopy, and energy-dispersive X-ray investigations established the materials composition. The study found that NCs degraded the acid orange 8 (AO8) color more efficiently than bare ZnO.

The development of a heterojunction boosts the photocatalytic activities of solution combustion synthesis, which is a time-/energy-efficient process. Advanced analytical characterization techniques were used in this protocol to evaluate the materials&#39; characteristics, and nanocomposites demonstrated improved acid orange-8 dye degradation.

There is a significant global demand for improvements in synthesis techniques and their optimal characteristics, especially for industrial-scale ...

Synthesis of Single-Crystalline Core-Shell Metal-Organic Frameworks

Because of their designability and unprecedented synergistic effects, core-shell metal-organic frameworks (MOFs) have been actively examined recently. However, the synthesis of single-crystalline core-shell MOFs is very challenging, and thus a limited number of examples have been reported. Here, we suggest a method of synthesizing single-crystalline HKUST-1@MOF-5 core-shells, which is HKUST-1 at the center of MOF-5. Through the computational algorithm, this pair of MOFs was predicted to have the matched lattice parameters and chemical connection points at the interface. To construct the core-shell structure, we prepared the octahedral- and cubic-shaped HKUST-1 crystals as a core MOF, in which the (111) and (001) facets were mainly exposed, respectively. Via the sequential reaction, the MOF-5 shell was well-grown on the exposed surface, showing a seamless connect interface, which resulted in the successful synthesis of single-crystalline HKUST-1@MOF-5. Their pure phase formation was proved by optical microscopic images and powder X-ray diffraction (PXRD) patterns. This method presents the potential of and insights into the single-crystalline core-shell synthesis with different kinds of MOFs.

Here, we demonstrate a protocol for the two-step synthesis of single-crystalline core-shells using a non-isostructural metal-organic framework (MOF) pair, HKUST-1 and MOF-5, which have well-matched crystal lattices.

単結晶コアシェル金属有機構造体の合成

Because of their designability and unprecedented synergistic effects, core-shell metal-organic frameworks (MOFs) have been actively examined recently. ...

トリアゾールおよびテトラゾール官能化Zr-MOFの合成と特性評価

Synthesis of Triazole and Tetrazole-Functionalized Zr-Based Metal-Organic Frameworks Through Post-Synthetic Ligand Exchange

Metal-organic frameworks (MOFs) are a class of porous materials that are formed through coordination bonds between metal clusters and organic ligands. Given their coordinative nature, the organic ligands and strut framework can be readily removed from the MOF and/or exchanged with other coordinative molecules. By introducing target ligands to MOF-containing solutions, functionalized MOFs can be obtained with new chemical tags via a process called post-synthetic ligand exchange (PSE). PSE is a straightforward and practical approach that enables the preparation of a wide range of MOFs with new chemical tags via a solid-solution equilibrium process. Furthermore, PSE can be performed at room temperature, allowing the incorporation of thermally unstable ligands into MOFs. In this work, we demonstrate the practicality of PSE by using heterocyclic triazole- and tetrazole-containing ligands to functionalize a Zr-based MOF (UiO-66; UiO = University of Oslo). After digestion, the functionalized MOFs are characterized via various techniques, including powder X-ray diffraction and nuclear magnetic resonance spectroscopy.

著者スポットライト:Functionalizing Metal-Organic Frameworks: Advancements, Challenges, and the Power of Post-Synthetic Ligand Exchange 

Post-synthetic ligand exchange (PSE) is a versatile and powerful tool for installing functional groups into metal-organic frameworks (MOFs). Exposing MOFs to solutions containing triazole- and tetrazole-functionalized ligands can incorporate these heterocyclic moieties into Zr-MOFs through PSE processes.

合成後配位子交換によるトリアゾールおよびテトラゾール官能化Zr系金属有機構造体の合成

Metal-organic frameworks (MOFs) are a class of porous materials that are formed through coordination bonds between metal clusters and organic ligands. ...

ミル-96、UiO-66-NH₂原子層のソルボサーマル合成繊維のマット上金属酸化皮膜に堆積

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