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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著者が明らかに何もありません。

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 border="0" cellpadding="0" cellspacing="0" width="625">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">trimethylaluminum</td>
			<td style="width:123px;">Strem Chemicals</td>
			<td style="width:119px;">93-1360</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">home-built ALD reactor</td>
			<td style="width:123px;">N/A</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">nitrogen cylinder</td>
			<td style="width:123px;">Arc3</td>
			<td style="width:119px;">UN1066</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">trimesic acid</td>
			<td style="width:123px;">Sigma-Aldrich</td>
			<td style="width:119px;">482749-500G</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">ethanol</td>
			<td style="width:123px;">Koptec</td>
			<td style="width:119px;">V1001</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">teflon lined autoclave</td>
			<td style="width:123px;">PARR Instrument Company</td>
			<td style="width:119px;">4760-1211</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">isotemp furnace</td>
			<td style="width:123px;">Fisher Scientific</td>
			<td style="width:119px;">F47925</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Zirconium (IV) chloride</td>
			<td style="width:123px;">Alfa Aesar</td>
			<td style="width:119px;">12104</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">2-aminoterephthalic acid</td>
			<td style="width:123px;">Acros Organics</td>
			<td style="width:119px;">278031000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">N,N-dimethylformamide</td>
			<td style="width:123px;">Fisher Scientific</td>
			<td style="width:119px;">D119-4</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Hydrochloric Acid</td>
			<td style="width:123px;">Fisher Scientific</td>
			<td style="width:119px;">A481-212</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Polypropylene fiber mats</td>
			<td style="width:123px;">N/A</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Polyamide fiber mats</td>
			<td style="width:123px;">N/A</td>
			<td style="width:119px;"></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

Research

JoVE Journal

Chemistry

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

11.3K 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

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 ...

化学

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

リン酸化ペプチドの強化充実のためのマクロポーラスポリマーモノリスの高度に多孔性配位高分子コーティングの製造

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

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 ...

Improved Heterojunction Quality in Cu2O-based Solar Cells Through the Optimization of Atmospheric Pressure Spatial Atomic Layer Deposited Zn1-xMgxO

Atmospheric pressure spatial atomic layer deposition (AP-SALD) was used to deposit n-type ZnO and Zn1-xMgxO thin films onto p-type thermally oxidized Cu2O substrates outside vacuum at low temperature. The performance of photovoltaic devices featuring atmospherically fabricated ZnO/Cu2O heterojunction was dependent on the conditions of AP-SALD film deposition, namely, the substrate temperature and deposition time, as well as on the Cu2O substrate exposure to oxidizing agents prior to and during the ZnO deposition. Superficial Cu2O to CuO oxidation was identified as a limiting factor to heterojunction quality due to recombination at the ZnO/Cu2O interface. Optimization of AP-SALD conditions as well as keeping Cu2O away from air and moisture in order to minimize Cu2O surface oxidation led to improved device performance. A three-fold increase in the open-circuit voltage (up to 0.65 V) and a two-fold increase in the short-circuit current density produced solar cells with a record 2.2% power conversion efficiency (PCE). This PCE is the highest reported for a Zn1-xMgxO/Cu2O heterojunction formed outside vacuum, which highlights atmospheric pressure spatial ALD as a promising technique for inexpensive and scalable fabrication of Cu2O-based photovoltaics.

Improved Heterojunction Quality in Cu2O-based Solar Cells Through the Optimization of Atmospheric Pressure Spatial Atomic Layer Deposited Zn1-xMgxO

Here we present a protocol for synthesizing Zn1-xMgxO/Cu2O heterojunctions in open-air at low temperature via atmospheric pressure spatial atomic layer deposition (AP-SALD) of Zn1-xMgxO on cuprous oxide. Such high quality conformal metal oxides can be grown on a variety of substrates including plastics by this cheap and scalable method.

銅で改善されたヘテロ接合品質<sub&gt; 2</sub析出した大気圧空間原子層の最適化により&gt; O系太陽電池<br /&gt; Znの<sub&gt; 1-xの</sub&gt; Mgの<sub&gt; X</sub&gt; O

Atmospheric pressure spatial atomic layer deposition (AP-SALD) was used to deposit n-type ZnO and Zn1-xMgxO thin films onto p-type thermally oxidized Cu2O ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide (CdSe@CdS) nanorod photocatalysts. Seeded rods are grown using a colloidal hot-injection method and then moved to an aqueous medium by ligand exchange. CdSe@CdS nanorods, an iridium precursor and other salts are mixed and illuminated. The deposition process is initiated by absorption of photons by the semiconductor particle, which results with formation of charge carriers that are used to promote redox reactions. To insure photochemical oxidative growth we used an electron scavenger. The photogenerated holes oxidize the iridium precursor, apparently in a mediated oxidative pathway. This results in the growth of high quality crystalline iridium oxide particles, ranging from 0.5 nm to about 3 nm, along the surface of the rod. Iridium oxide grown on CdSe@CdS heterostructures was studied by a variety of characterization methods, in order to evaluate its characteristics and quality. We explored means for control over particle size, crystallinity, deposition location on the CdS rod, and composition. Illumination time and excitation wavelength were found to be key parameters for such control. The influence of different growth conditions and the characterization of these heterostructures are described alongside a detailed description of their synthesis. Of significance is the fact that the addition of iridium oxide afforded the rods astounding photochemical stability under prolonged illumination in pure water (alleviating the requirement for hole scavengers).

A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

CdSeの@のCdSナノロッド上にイリジウム酸化物ナノ粒子の光化学酸化成長

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and conformality by taking advantage of self-limiting reactions between vapor-phase precursors and the growing film. Perovskite oxides present potential for next-generation electronic materials, but to-date have mostly been deposited by physical methods. This work outlines a method for depositing SrTiO3 (STO) on germanium using ALD. Germanium has higher carrier mobilities than silicon and therefore offers an alternative semiconductor material with faster device operation. This method takes advantage of the instability of germanium's native oxide by using thermal deoxidation to clean and reconstruct the Ge (001) surface to the 2&#215;1 structure. 2-nm thick, amorphous STO is then deposited by ALD. The STO film is annealed under ultra-high vacuum and crystallizes on the reconstructed Ge surface. Reflection high-energy electron diffraction (RHEED) is used during this annealing step to monitor the STO crystallization. The thin, crystalline layer of STO acts as a template for subsequent growth of STO that is crystalline as-grown, as confirmed by RHEED. In situ X-ray photoelectron spectroscopy is used to verify film stoichiometry before and after the annealing step, as well as after subsequent STO growth. This procedure provides framework for additional perovskite oxides to be deposited on semiconductors via chemical methods in addition to the integration of more sophisticated heterostructures already achievable by physical methods.

This work details the procedures for the growth and characterization of crystalline SrTiO3 directly on germanium substrates by atomic layer deposition. The procedure illustrates the ability of an all-chemical growth method to integrate oxides monolithically onto semiconductors for metal-oxide semiconductor devices.

原子層堆積法を介してゲルマニウム上のペロブスカイト型チタン酸ストロンチウムのエピタキシャル成長

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

Aerosol-assisted Chemical Vapor Deposition of Metal Oxide Structures: Zinc Oxide Rods

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, their high cost production and/or incompatibility with microfabrication technologies, due to the use of pre-deposited catalyst-seeds and/or high processing temperatures exceeding 900 &#176;C, represent a drawback for a widespread use of these methods. Here, however, we report the synthesis of ZnO rods via a non-catalyzed vapor-solid mechanism enabled by using an aerosol-assisted chemical vapor deposition (CVD) method at 400 &#176;C with zinc chloride (ZnCl2) as the precursor and ethanol as the carrier solvent. This method provides both single-step formation of ZnO rods and the possibility of their direct integration with various substrate types, including silicon, silicon-based micromachined platforms, quartz, or high heat resistant polymers. This potentially facilitates the use of this method at a large-scale, due to its compatibility with state-of-the-art microfabrication processes for device manufacture. This report also describes the properties of these structures (e.g., morphology, crystalline phase, optical band gap, chemical composition, electrical resistance) and validates its gas sensing functionality towards carbon monoxide.

Columnar zinc oxide structures in the form of rods are synthesized via aerosol-assisted chemical vapor deposition without the use of pre-deposited catalyst-seed particles. This method is scalable and compatible with various substrates based on either silicon, quartz or polymers.

エアロゾルによる金属酸化物の構造の化学蒸着: 酸化亜鉛棒

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, ...

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity and convenient colorimetric readout. However, high densities of nanoparticles are typically needed for detection. The available synthesis-based enhancement protocols are either limited to gold and silver nanoparticles or rely on precise enzymatic control and optimization. Here, we present a protocol to enhance the colorimetric readout of gold, silver, silica, and iron oxide nanoprobes. It was observed that the colorimetric signal can be improved by up to a 10000-fold factor. The basis for such signal enhancement strategies is the chemical reduction of Au3+ to Au0. There are several chemical reactions that enable the reduction of Au3+ to Au0. In the protocol, Good&#39;s buffers and H2O2 are used and it is possible to favor the deposition of Au0 onto the surface of existing nanoprobes, in detriment of the formation of new gold nanoparticles. The protocol consists of the incubation of the microarray with a solution consisting of chloroauric acid and H2O2 in 2-(N-morpholino)ethanesulfonic acid pH 6 buffer following the nanoprobe-based detection assay. The enhancement solution can be applied to paper and glass-based sensors. Moreover, it can be used in commercially available immunoassays as demonstrated by the application of the method to a commercial allergen microarray. The signal development requires less than 5 min of incubation with the enhancement solution and the readout can be assessed by naked eye or low-end image acquisition devices such as a table-top scanner or a digital camera.

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

In this work, a protocol for signal enhancement of nanoprobe-based biosensing is presented. The protocol is based on the reduction of chloroauric acid onto the surface of existing nanoprobes that consist of gold, silver, silica or iron-oxide nanoparticles.

原金ナノ粒子合成による急速なナノプローブ信号強調

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity ...

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. ...

Niobium Oxide Films Deposited by Reactive Sputtering: Effect of Oxygen Flow Rate

Reactive sputtering is a versatile technique used to form compact films with excellent homogeneity. In addition, it allows easy control over deposition parameters such as gas flow rate that results in changes on composition and thus in the film required properties. In this report, reactive sputtering is used to deposit niobium oxide films. A niobium target is used as metal source and different oxygen flow rates to deposit niobium oxide films. The oxygen flow rate was changed from 3 to 10 sccm. The films deposited under low oxygen flow rates show higher electrical conductivity and provide better perovskite solar cells when used as electron transport layer.

Here, we present a protocol for niobium oxide films deposition by reactive sputtering with different oxygen flow rates for use as an electron transport layer in perovskite solar cells.

反応性スパッタリングによって堆積した酸化ニオブ膜:酸素流量の影響

Reactive sputtering is a versatile technique used to form compact films with excellent homogeneity. In addition, it allows easy control over deposition ...