The authors gratefully acknowledge financial support from the Belgian Federal government (Belspo through the IAP VI/27 and IAP-7/05 programs), the European Union's Seventh Framework Programme (FP7/2007-2013 under grant agreement no. 310651 SACS), the Flemish government in the form of long-term structural funding "Methusalem" grant METH/08/04 CASAS, the "Strategisch Initiatief Materialen" SoPPoM program, and the Fund for Scientific Research Flanders (FWO) grant G.0349.12. W.B. gratefully acknowledge the chemistry department of the KU Leuven for a FLOF-scholarship. The authors thank UOP Antwerp for the kind donation of zeolite samples and the mechanical workshop of the KU Leuven for helping with the design and construction of the heating/vacuum cell used in this study.

注意：このレポートで使用される化学物質および試薬は、適切な安全保護（白衣、手袋、安全ゴーグル、ヒュームフード）を使用して、注意して取り扱われました。本研究では、微多孔性無機材料（1から5ミクロンの範囲のサイズを有するゼオライト）の操作を扱うので、特別な注意が適切な防じん（防塵マスク）の使用を対象としました。我々は、適切な操作および/または廃棄物処理のために使用する前に、この作業に用いられる化学物質および試薬の関連材料の安全性データ（MSDS）の相談をお勧めします。 1.ゼオライトの前処理<ol><li>熱前処理 注：銀クラスター形成や発光を妨げる可能性があり、このような有機不純物などの不純物を、除去するために、使用前にゼオライト材料を事前に扱います。 <ol><li>商業LTA（NA）ゼオライトの10グラムを計量し、デポ（商業LTAゼオライトは、カウンターバランスそのフレームワーク中のイオンとしてナトリウムが含まれています）磁器トレイ上に均一に座ります。 </li><li>ゼオライト構造の損傷を避けるために80°Cと110°Cで1時間の間隔で5℃/分の温度傾斜を用いて、450℃のマッフル炉中で一晩ゼオライト粉末を加熱します。 </li><li>オーブンからゼオライト材料を取り外し、それは周囲条件下で室温まで冷却しましょう。 </li></ol></li><li>ゼオライト粒子のサイズ選択 注：これは、均質なフィルムを作成するために必要な出発ゼオライト材料のより均一な粒度分布を生成します。このステップは、多くの場合、工業的に製造さゼオライト中に存在している大規模な非晶質粒子を除去します。 <ol><li>商業LTA（NA）を10gを秤量し、脱イオン水1L中に懸濁します。 </li><li>積極的に手で10分ごとにサスペンションを振っ、1時間サスペンションを超音波処理。 </li><li> 30分間Atterbergシリンダ（1 L）中懸濁液を注ぎます。サイズは10ミクロン未満の粒子懸濁液中に残っているが、より大きな粒子が沈殿します。 </li><li>サスペンションをデカントし、ブフナー漏斗を用いて濾過することにより粉末を回収します。脱イオン水で回収した粉末を3回洗浄します。 </li><li>熱ステップ1.1.2で説明したように粉末を扱います。 </li></ol></li></ol>発光LTA（ナ）-Agゼオライト複合材料の作製<ol><li>発光銀の合成は、参考資料として[LTA（ナ）-Ag] LTAゼオライトを交換しました<ol><li> 250ミリリットル高密度ポリプロピレン（HDPE）ボトルに脱イオン水200ミリリットル中の硝酸銀の74.8ミリグラムを溶解させます。 </li><li>前処理LTA（NA）試料1gを秤量し、硝酸銀溶液中に懸濁します。 </li><li>室温で転倒型シェーカーオーブンに一晩攪拌HDPEフラスコを残します。 </li><li>ブフナー漏斗を用いて懸濁液を濾過し、脱イオン水でゼオライト粉末を3回洗浄します。 </li><li> 45時マッフル炉中で回収した粉末を加熱ステップ1.1.2に記載したのと同じ手順を用いて、0℃、。 </li><li>サンプルを冷却し、制御された湿度（相対湿度98％）でデシケーターに入れてください。デシケーター内部の飽和硫酸カリウム溶液を配置することによって相対湿度を制御します。15 </li><li>分光蛍光光度計ならびにそれらの外部量子効率を用いて、（異なる波長で）サンプルの励起および発光スペクトルを測定します。 <ol><li> 1ミリメートルパス石英キュベットにサンプルを配置することによって、2次元励起 - 発​​光プロットを測定します。 5nmのステップおよび0.1秒の滞留時間を用いて800 nmの励起波長、最大上に30nm出発発光スペクトルを収集します。 </li><li>ランプ強度と生データへの放出経路の波長依存性の検出のための機器のソフトウェアを使用して修正を適用します。さらに、2次元プロットで二次ピークを避けるために、ロングパスフィルターを使用しています。 </li><li>量子efficiを実行しますその後encyの分光蛍光光度計に取り付けられた積分球を使用して測定。16録音ゼオライトサンプルと励起波長として260nmのを使用してのBaSO 4参照の両方のための600 nmの240 nmでの放射スキャン、および機器のソフトウェアを使用して量子効率を計算します。 </li></ol></li></ol></li></ol>発光[LTA（李）-Ag]ゼオライト複合材料の調製<ol><li>部分的に交換されたリチウムLTAゼオライトの合成[LTA（李）] 注：手順は八尋と共同研究者の報告書から適応された部分的に交換LTA（Li）とゼオライトの製造に続いて17。 <ol><li> 2.5 Lの脱イオン水に17.2グラムの硝酸リチウムを溶解させます。 </li><li> 1LのHDPEフラスコに硝酸リチウム溶液0.5 Lを注ぎます。 </li><li>前処理LTA（NA）ゼオライトを3gを秤量し、硝酸リチウム溶液を含むHDPEフラスコ中に懸濁します。 </li><li>エンド-Oを用いてフラスコを撹拌室温で一晩版エンドシェーカーオーブン。 </li><li>ブフナー漏斗を用いて懸濁液を濾過し、脱イオン水を用いて回収した粉末を3回洗浄します。 </li><li>リチウム交換を行います<ol><li>濾過工程（3.1.5）から回収した粉末を含む1LのHDPEフラスコに新鮮な硝酸リチウム溶液（3.1.1）の0.5 Lを追加します。 </li><li>繰り返しは、3.1.4と3.1.5を繰り返します。 </li><li>繰り返しは、3.1.6.1と3.1.6.2別の4回繰り返します。 </li></ol></li><li>ゼオライト粉末を回収し、一晩80°Cと110°Cで1時間の間隔で5℃/分の温度傾斜を用いて、450℃のマッフル炉中で加熱します。 </li></ol></li><li>発光の合成[LTA（李）-Ag]ゼオライト<ol><li> 250ミリリットルHDPEボトルを使用して、脱イオン水200ミリリットルで74.8 mgの硝酸銀を溶解させます。 </li><li>部分的に交換されたリチウムLTAゼオライト[LTA（李）]の1グラムを計量し、硝酸銀溶液（3.2.1）にそれを中断。 </li><li> HDPE FLを攪拌室温で一晩転倒型振とうオーブンを使用してお願いします。 </li><li>ブフナー漏斗を用いて懸濁液を濾過し、脱イオン水を用いて回収したゼオライト粉末を3回洗浄します。 </li><li>一晩80℃〜110℃で1時間の間隔で5℃/分の温度勾配を使用して、450℃のマッフル炉中で粉末を熱処理します。 </li><li>内部飽和硫酸カリウム溶液（98％相対湿度）を含むデシケータを用いて制御された湿度条件下でサンプルを冷却15 </li><li>ステップ2.1.7に記載の手順に従って、サンプルの励起および発光スペクトルならびにそれらの外部量子効率を測定します。 </li><li> 、1簡単に言えば。異なる温度で、試料中の水分含有量を決定するために、熱重量分析（TGA）を行い、白金試料ホルダーにとして、調製した試料の30〜50ミリグラムを配置し、TGAデバイスにロードします。 50からの重量損失を測定します°C、600°Cまで窒素流（90 ml /分）下に5℃/分の加熱速度を使用して。 </li></ol></li></ol>湿度検出アプリケーションのためのLTA（李）-Ag /ポリエチレンイミン（PEI）複合蒸着膜の4製作注：このレポートで使用される堆積手順が変更され、基準18から適応されました。 <ol><li> LTA（李）-Agコロイド懸濁液の準備。 <ol><li>脱イオン水で100mlに商用50重量％PEI溶液1mlを希釈します。 </li><li>発光LTA（李）-Ag材料250mgの重量を量ります。 </li><li> 125ミリリットルのHDPEボトルで一緒にゼオライトとPEI溶液を混合し、積極的にサスペンションを振ります。 </li><li>均一な懸濁液を得るために、室温で一晩40 kHzの超音波洗浄器でボトルを置きます。 </li><li>スプレーボトルにLTA（李）-Ag / PEI懸濁液を注ぎます。 </li></ol></li><li>センサーPROTのための石英板上にLTA（李）-Ag / PEI膜の堆積otypeの生産。 <ol><li>前の成膜に、連続的に脱イオン水及びアセトンでそれをすすぐことによって石英板を清掃してください。 1時間80℃のオーブンできれいなプレートを乾燥させます。 </li><li>アルミニウム箔のクリーンシートに水平石英板を配置し、約20cmの距離から三回（3秒毎に）噴霧することにより、一方の側にコートに石英板をスプレー。 50℃で30分間乾燥炉内部のコーティングされたプレートを置きます。 </li><li>フィルムが均一になるまで繰り返しステップは、別の4回4.2.2。 </li></ol></li><li>センサーのプロトタイプの水和/脱水。 <ol><li>社内加熱/真空セルのサンプルコンパートメントにコーティングされた石英板を配置します。5 </li><li>コーティングされたプレートの上にゴムリングとの組み合わせできれいな石英板を配置することによって、細胞の試料室を閉じ、 図2に示すように、テフロンストッパーとネジを使用してセルを密封します。 </li><li>高真空を適用し、私たちサンプルを脱水するために、細胞を一晩に、10 -3ミリバール未満の圧力をる。 </li><li>視覚的にUVランプを使用して堆積膜（可視光領域）の発光色の変化を監視します。 </li><li> UVランプを用いて膜の再水和の際に、可視領域の発光色の変化を監視するために試料室を開きました。 </li><li> LTA（李）-Ag / PEIフィルムの可逆性をテストするために、ステップ4.3.2から4.3.5に始まるサイクルを複数回繰り返します。 </li></ol></li></ol>

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The authors have nothing to disclose.

A simple device to demonstrate the proof of concept of using LTA(Li)-Ag as a luminescence based humidity sensor was produced by spray coating the LTA(Li)-Ag powder suspended in a PEI solution onto a quartz plate. The PEI solution produces a polymer layer with homogenous thickness when the water is evaporated. The polymer-zeolite composite layer displays similar luminescent properties as that of the zeolite in powder form. The PEI/LTA(Li)-Ag zeolite composite displays the expected water-responsive luminescent properties, whose emission color changes upon variations in the water content present in the composite at relatively low humidity scale. 
Replacing Na with Li ions in LTA zeolites (calculated exchange rate 33%) has a notable impact on the self-assembly and stabilization of luminescent silver clusters in the LTA(Li) scaffolds leading to unique optical properties. The EQE of LTA(Li)-Ag as compared to LTA(Na)-Ag samples is enhanced by more than one order of magnitude. Moreover, the emission colors displayed by the LTA(Li)-Ag samples have a water-dependence, providing a potential application of the samples as luminescence based humidity sensors. 
We have thus demonstrated an easy method to fabricate a luminescent film-like humidity sensor through which changes in hydration levels can be visually monitored simply by using a UV lamp. The availability of the raw materials, the direct visualization of the color changes correlated with humidity content, the photo-stability of the films, and the relative ease of fabricating cost-effective devices make these luminescent materials potential candidates to compete with state-of-the-art humidity sensors based upon electrical responses. The procedure described in this report could also be applied and extended to different substrates, at different micro and macro scales, to make the sensor more flexible. Additionally, several critical steps during the fabrication of Ag-zeolites, which play an important role in determining the final optical properties of such materials, were discussed in this protocol. For instance, the pre-cleaning of the raw zeolite material leads to the removal of optical and chemical impurities, as well as to homogenous zeolite crystal size distribution. This is crucial for the incorporation of zeolites into functional devices. One limitation of the present methodology is the restriction on the use of thin film sensors beyond 75 &#176;C. This is mainly due to the decomposition of the PEI polymer, rather than to the degradation of the LTA(Li)-Ag zeolites, which can withstand up to 500 &#176;C. The use of heat-resistant polymers, such as polyvinyl alcohol, could expand the temperature range up to 200 &#176;C. We expect that further investigations will be directed to the development of methodologies for the synthesis of nanostructured Ag-zeolite composites with (multi)functional properties and finally to the design of advanced sensor prototypes.

閉じ込められたゼオライトマトリックス中に自己組織化によって形成された小サブナノメートルoligoatomic銀クラスターは、独自の光学特性を示す。1-5このような銀-ゼオライト複合材料は、高い化学的及び光安定性を有します。しかしながら、それらの光ルミネセンス特性は銀クラスターのローカル環境に大きく依存しています。銀ゼオライト複合体に光学的特徴に影響を与える環境条件に内因性および外因性の特性に分けることができます。固有特性は、ゼオライトトポロジー、カウンターバランスするイオンの種類、および銀の負荷に関連している。1一方、外因性の性質は、そのような中で吸着物や水分子の存在などの合成後の変化に関連していますゼオライトの空洞。3,4後者の特性は、銀ゼオライトに与えるには、光学的に、このようなゼオライト足場6-8内の水分の変動のような外部刺激に応答する能力を合成します</suP&gt;または決定されたガスの存在。したがって、水蒸気およびガスセンサーとしてのそれらの使用が提案されている。9,10 最近の研究では、湿気に銀ゼオライトの光学応答が唯一の彼らの放射の吸収または消光の変化にも、それらの含水量に対して異なる発光色の外観に相関されていないことを実証している。5安定化部分的にLiがLTAゼオライトは、それぞれ、脱水および水和試料中の緑/黄色発光する青色から動的な色の変化に反映された相対湿度の低いスケールで変化する水分応答性材料の形成につながっ交換で銀クラスターの。したがって、発光ベース湿度センサとして、これらの材料を使用することが提案されました。今日まで、このような電解質、セラミック、ポリマー、およびナノ構造複合材料などの材料の異なるタイプの湿度Bにおける監視変更が提案されています電気的および光学的応答に関するASED。11,12この詳細なプロトコルでは、我々は、湿度センサとしてLTA（李）-Agゼオライトの応用のために、さらにプロトタイプの開発に、概念実証を実証することを目指しています。 LTA（李）-Agゼオライトの汎用性のために、異なる基板に組み込まれるように、彼らの潜在的な拡張性と費用対効果の製造は、プロトタイプの設計を容易にする可能性があります。13このようなセンサは、のように、異なる産業分野での適用可能性を持つことができます農業だけでなく、自動車、製紙産業。14

<table><tbody><tr><td>LTA(Na) zeolite</td><td>UOP</td><td>Molsiv adsorbent 4A</td><td></td></tr><tr><td>Silver nitrate</td><td>Sigma Aldrich</td><td>209139</td><td>&amp;ge;99.0%</td></tr><tr><td>Lithium nitrate</td><td>Sigma Aldrich</td><td>62574</td><td>&amp;ge;99.0%, calc. on dry substances</td></tr><tr><td>Polyethyleneimine solution</td><td>Sigma Aldrich</td><td>3880</td><td>~50% H&lt;sub&gt;2&lt;/sub&gt;O</td></tr><tr><td>Scanning electron microscope (SEM)</td><td>JEOL</td><td>JSM-6010LV</td><td></td></tr><tr><td>Thermogravimetric analyzer</td><td>TA instruments</td><td>Q500</td><td></td></tr><tr><td>Spectrofluorimeter</td><td>Edinburgh instruments</td><td>FLS980-s</td><td></td></tr><tr><td>Integrating sphere</td><td>Labsphere</td><td>4P-GPS-033-SL</td><td></td></tr></tbody></table>

nanostructured ag-zeolite composites as luminescence-based humidity sensors

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high external quantum efficiencies (EQE) and spans the whole visible spectrum. It has been recently reported that the UV excited luminescence of partially Li-exchanged sodium Linde type A zeolites [LTA(Na)] containing luminescent silver clusters can be controlled by adjusting the water content of the zeolite. These samples showed a dynamic change in their emission color from blue to green and yellow upon an increase of the hydration level of the zeolite, showing the great potential that these materials can have as luminescence-based humidity sensors at the macro and micro scale. Here, we describe the detailed procedure to fabricate a humidity sensor prototype using silver-exchanged zeolite composites. The sensor is produced by suspending the luminescent Ag-zeolites in an aqueous solution of polyethylenimine (PEI) to subsequently deposit a film of the material onto a quartz plate. The coated plate is subjected to several hydration/dehydration cycles to show the functionality of the sensing film.

LTA-銀ゼオライトのSEM顕微鏡写真は、陽イオン交換および熱処理工程の後に記録しました。続いてフォトルミネセンス、二次元（2D）の励起/放射プロットは、水和LTA（NA）-Ag及びLTA（リー）-Agゼオライト（ 図1）の両方を測定しました。 Agは、その化学組成を決定するために、ゼオライトを交換の元素分析は、XPSにより行いました。解析はLTA（NA）とLTA（Li）とゼオライトに銀交換はそれぞれ19.6重量％および21.5重量％の銀重量パーセントと非常に近いことを示しています。重量百分率の差は、Li原子の低い原子量に帰することができます。さらに、元素分析は、リチウム交換後のナトリウムの33％が置換されることが示されました。陽イオン交換およびサンプル上で実行される後続の熱処理工程は、SEMによって示されるように、LTA結晶の構造に影響を与えていないように見えます。また、より大きな銀の形成のnゼオライト結晶の表面上anoparticlesが可視化されていませんでした。発光特性は、主にその水和状態で両方のLTA（李）-AgとLTA（NA）-Agサンプル間で異なります。カウンターバランス陽イオンとしてゼオライト骨格にリチウムを組み込むことにより、励磁最大でブルーシフトは、LTA（NA）-AgとLTA（李）-Agため、それぞれ、波長370nmから260nmのが原因で発生します。これとは対照的に発光極大は、システムにリチウムを添加することにより、565 nmの550から小さな赤方偏移を受けます。これらのサンプルの間の最大の違いは、それらの外部量子効率（EQE）で観察されます。 （260 nmで励起したとき）LTAのためのEQE（李）-Agゼオライトが62％に達したのに対し、LTA（ナ）-Agゼオライトは、その最大励起（370 nm）ので約4％のEQEを有しています。これは、254nmの紫外線照射下で明るい黄色の発光粉末になります。 LTA（リー）-Ag試料の発光特性はまた、水の含有量に依存していますシステム。これは、TGAおよび温度に依存する発光実験の組み合わせによって示された、TGAは、ゼオライトの水和レベルまで温度を相関させます。さらに、温度は、社内加熱セルを使用して、LTA（李）-Agサンプル（ 図2）によって表示される発光色に間接的に関係しました。緑色から青色に黄色の発光色がシフトし、LTA（李）-Ag系から水を除去します。 EQEは着実に21％（脱水状態）に62％（含水状態）から降下します。 なぜならLTA（リー）-Agの水応答性挙動を、この材料はPEI溶液中に粉末を懸濁し、続いて、石英板上に複合材料をスプレーコーティングすることにより、発光ベースの湿度センサのプロトタイプを作製しました。 （昼光とUV照射下）の写真やスプレー塗装LTA（李）-Ag / PEIフィルムのSEM顕微鏡写真を図3に表示されている。我々は、USIによってことを観察しました<html> NGこのコーティング手順、発光面でのポリマー - ゼオライト複合体の比較的均一な層が得られました。 SEM顕微鏡写真は、ゼオライト結晶をコーティング手順によって変更されないことを示しています。社内加熱/真空セルを使用して、それはまた、ポリマー - ゼオライトフィルムは、粉末形態でゼオライトで観察された水の応答特性を保持することが示されました。 <img alt="図1" src="/files/ftp_upload/54674/54674fig1.jpg" /> 図1：SEM 写真と銀の発光特性は、LTAゼオライトのSEM顕微鏡写真およびLTA（ナ）-Ag（b）およびLTA（李）-Ag（C、D）の2次元励起発光プロットを交換しました。 2D励起 - 発​​光プロットにおける挿入図は、異なる励起波長（254、300、366および450 nm）の下でのサンプルのシミュレートされた発光色を表示します。<html> OAD / 54674 / 54674fig1large.jpg &quot;ターゲット=&quot; _空白 &quot;&gt;この図の拡大版をご覧になるにはこちらをクリックしてください。 <img alt="図2" src="/files/ftp_upload/54674/54674fig2.jpg" /> 図2：LTA（ 李）-Agの発光特性上の水和レベルの効果。 。。LTA（Li）との260 nmの励起時LTA（李）-Agサンプルc）の正規化された発光スペクトル（）のために、この研究b）の TGAプロットで採用、社内加熱/真空セルのa）の模式図- Agのサンプルは、異なる温度で測定した。d）のスキームの水含有量に関して実際のサンプルの発光色の変化を表示する。 <a href="http://ecsource.jove.com/files/ftp_upload/54674/54674fig2large.jpg" target="_blank">この図の拡大版をご覧になるにはこちらをクリックしてください。</a> ftp_upload / 54674 / 54674fig3.jpg &quot;/&gt; 図3：LTA（ 李）-Ag / PEI複合に基づいて発光湿度センサ。 a）は、昼光照明の下でコーティングされたプレートの写真。 （B、C）石英表面上のLTA（李）-Ag結晶の分布を示す堆積膜のそれぞれ脱水および水和コーティングされたプレートの写真254 nmのUV光照射下、。d）の SEM写真。挿入図は、元のSEM写真の選択した領域を拡大して表示されます。水和、脱水PEI / LTAのe）の排出量の最大値（Li）と-Agゼオライト複合、励起波長として260nmのを使用して、10の水和/脱水サイクル中。f）の PEI / LTA（李）10水和/脱水サイクル後-Agゼオライト複合体の発光極大プロファイルの挙動を示すプロット。 <a href="http://ecsource.jove.com/files/ftp_upload/54674/54674fig3large.jpg" target="_blank">viにはこちらをクリックしてください</a>この図の拡大版をEW。

Watch this Scientific Journal Video about Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors at JoVE.com

Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors

A protocol for the synthesis of moisture-responsive luminescent Ag-zeolite composites is described in this report.

発光ベースの湿度センサなどのナノ構造のAg-ゼオライト複合

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high ...

nanostructured-ag-zeolite-composites-as-luminescence-based-humidity

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

10.1K ビュー.  KU Leuven. A protocol for the synthesis of moisture-responsive luminescent Ag-zeolite composites is described in this report.

ビデオ: Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and reduction half reactions, and fast electron (hole) diffusion and charge separation. Nanowires present suitable architectures to meet these requirements. Axially segmented Ag|ZnO and radially segmented (coaxial) TiO2-Ag nanowires with a diameter of 200 nm and a length of 6-20 &#181;m were made by templated electrodeposition within the pores of polycarbonate track-etched (PCTE) or anodized aluminum oxide (AAO) membranes, respectively. In the photocatalytic experiments, the ZnO and TiO2 phases acted as photoanodes, and Ag as cathode. No external circuit is needed to connect both electrodes, which is a key advantage over conventional photo-electrochemical cells. For making segmented Ag|ZnO nanowires, the Ag salt electrolyte was replaced after formation of the Ag segment to form a ZnO segment attached to the Ag segment. For making coaxial TiO2-Ag nanowires, a TiO2 gel was first formed by the electrochemically induced sol-gel method. Drying and thermal annealing of the as-formed TiO2 gel resulted in the formation of crystalline TiO2 nanotubes. A subsequent Ag electrodeposition step inside the TiO2 nanotubes resulted in formation of coaxial TiO2-Ag nanowires. Due to the combination of an n-type semiconductor (ZnO or TiO2) and a metal (Ag) within the same nanowire, a Schottky barrier was created at the interface between the phases. To demonstrate the photocatalytic activity of these nanowires, the Ag|ZnO nanowires were used in a photocatalytic experiment in which H2 gas was detected upon UV illumination of the nanowires dispersed in a methanol/water mixture. After 17 min&#160;of illumination, approximately 0.2 vol% H2 gas was detected from a suspension of ~0.1 g of Ag|ZnO nanowires in a 50 ml 80 vol% aqueous methanol solution.

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Procedures are outlined to prepare segmented and coaxial nanowires via templated electrodeposition in nanopores. As examples, segmented nanowires consisting of Ag and ZnO segments, and coaxial nanowires consisting of a TiO2 shell and a Ag core were made. The nanowires were used in photocatalytic hydrogen formation experiments.

ZnOと同軸のTiO |光触媒活性セグメント化銀の調製および使用<sub&gt; 2</subテンプレート化電製&gt; - 銀ナノワイヤー

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and ...

工学

Synthesis of Zeolites Using the ADOR (Assembly-Disassembly-Organization-Reassembly) Route

Zeolites are an important class of materials that have wide ranging applications such as heterogeneous catalysts and adsorbents which are dependent on their framework topology. For new applications or improvements to existing ones, new zeolites with novel pore systems are desirable. We demonstrate a method for the synthesis of novel zeolites using the ADOR route. ADOR is an acronym for Assembly, Disassembly, Organization and Reassembly. This synthetic route takes advantage of the assembly of a relatively poorly stable that which can be selectively disassembled into a layered material. The resulting layered intermediate can then be organized in different manners by careful chemical manipulation and then reassembled into zeolites with new topologies. By carefully controlling the organization step of the synthetic pathway, new zeolites with never before seen topologies are capable of being synthesized. The structures of these new zeolites are confirmed using powder X-ray diffraction and further characterized by nitrogen adsorption and scanning electron microscopy. This new synthetic pathway for zeolites demonstrates its capability to produce novel frameworks that have never been prepared by traditional zeolite synthesis techniques.

Synthesis of Zeolites Using the ADOR Assembly-Disassembly-Organization-Reassembly Route

A protocol for the preparation of novel zeolites by the ADOR (Assembly-Disassembly-Organization-Reassembly) synthetic route is presented.

ADOR（組立・解体・組織・再組み立て）ルートを使用したゼオライトの合成

Zeolites are an important class of materials that have wide ranging applications such as heterogeneous catalysts and adsorbents which are dependent on ...

化学

Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobalt metals.

Because of the importance and extensive use of palladium, gold and cobalt metals in high-technology equipment, their recovery and recycling constitute an important industrial challenge. The metal recovery system described herein is a simple, low-cost means for the effective detection, removal, and recovery of these metals from the urban mine.

検出とパラジウムの回収は、都市鉱山からの金やコバルト金属は、ナノスケールワゴンホイール形の細孔を有する指定小説センサ/吸着剤を使用しました

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in ...

Iridium Oxide-reduced Graphene Oxide Nanohybrid Thin Film Modified Screen-printed Electrodes as Disposable Electrochemical Paper Microfluidic pH Sensors

A facile, controllable, inexpensive and green electrochemical synthesis of IrO2-graphene nanohybrid thin films is developed to fabricate an easy-to-use integrated paper microfluidic electrochemical pH sensor for resource-limited settings. Taking advantages from both pH meters and strips, the pH sensing platform is composed of hydrophobic barrier-patterned paper micropad (&#181;PAD) using polydimethylsiloxane (PDMS), screen-printed electrode (SPE) modified with IrO2-graphene films and molded acrylonitrile butadiene styrene (ABS) plastic holder. Repetitive cathodic potential cycling was employed for graphene oxide (GO) reduction which can completely remove electrochemically unstable oxygenated groups and generate a 2D defect-free homogeneous graphene thin film with excellent stability and electronic properties. A uniform and smooth IrO2 film in nanoscale grain size is anodically electrodeposited onto the graphene film, without any observable cracks. The resulting IrO2-RGO electrode showed slightly super-Nernstian responses from pH 2-12 in Britton-Robinson (B-R) buffers with good linearity, small hysteresis, low response time and reproducibility in different buffers, as well as low sensitivities to different interfering ionic species and dissolved oxygen. A simple portable digital pH meter is fabricated, whose signal is measured with a multimeter, using high input-impedance operational amplifier and consumer batteries. The pH values measured with the portable electrochemical paper-microfluidic pH sensors were consistent with those measured using a commercial laboratory pH meter with a glass electrode.

The study demonstrates the growth of iridium oxide-reduced graphene oxide (IrO2-RGO) nanohybrid thin films on irregular and rough screen-printed carbon substrate through a green electrochemical synthesis, and their implementation as a pH sensor with a patterned paper-fluidic platform.

使い捨て電気化学紙のマイクロ流体のpHセンサーとしてイリジウム酸化還元グラフェン酸化物ナノハイブリッド薄膜変更されたスクリーン印刷電極

A facile, controllable, inexpensive and green electrochemical synthesis of IrO2-graphene nanohybrid thin films is developed to fabricate an easy-to-use ...

Adsorption Device Based on a Langatate Crystal Microbalance for High Temperature High Pressure Gas Adsorption in Zeolite H-ZSM-5

We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate crystal microbalance, LCM) and its use for gas adsorption measurements in zeolite H-ZSM-5. Prior to the adsorption measurements, zeolite H-ZSM-5 crystals were synthesized on the gold electrode in the center of the LCM, without covering the connection points of the gold electrodes to the oscillator, by the steam-assisted crystallization (SAC) method, so that the zeolite crystals remain attached to the oscillating microbalance while keeping good electroconductivity of the LCM during the adsorption measurements. Compared to a conventional quartz crystal microbalance (QCM) which is limited to temperatures below 80 &#176;C, the LCM can realize the adsorption measurements in principle at temperatures as high as 200-300 &#176;C (i.e., at or close to the reaction temperature of the target application of one-stage DME synthesis from the synthesis gas), owing to the absence of crystalline-phase transitions up to its melting point (1,470 &#176;C). The system was applied to investigate the adsorption of CO2, H2O, methanol and dimethyl ether (DME), each in the gas phase, on zeolite H-ZSM-5 in the temperature and pressure range of 50-150 &#176;C and 0-18 bar, respectively. The results showed that the adsorption isotherms of these gases in H-ZSM-5 can be well fitted by Langmuir-type adsorption isotherms. Furthermore, the determined adsorption parameters, i.e., adsorption capacities, adsorption enthalpies, and adsorption entropies, compare well to literature data. In this work, the results for CO2 are shown as an example.

A protocol for high-temperature and high-pressure gas adsorption measurements on zeolite H-ZSM-5 using an adsorption measurement device based on a langatate crystal microbalance is presented. Prior to the adsorption measurements, the synthesis of zeolite H-ZSM-5 on the langatate crystal microbalance sensor by the steam-assisted crystallization (SAC) method is demonstrated.

ゼオライトH-ZSM-5で高温・高圧のガス吸着用のLangatateクリスタルマイクロバランスに基づいて吸着装置

We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate ...

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 ...

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, ...

Resource Recycling of Red Soil to Synthesize Fe2O3/FAU-type Zeolite Composite Material for Heavy Metal Removal

Heavy metal-polluted water is of great concern to human health and the eco-environment. In situ water remediation techniques enabled by highly efficient adsorption materials are of great importance in these circumstances. Among all the materials used in water remediation, iron-based nanomaterials and porous materials are of great interest, benefiting from their rich redox reactivity and adsorption function. Here, we developed a facile protocol to directly convert the widely spread red soil in south China to fabricate the Fe2O3/faujasite (FAU)-type zeolite composite material. 
The detailed synthesis procedure and synthesis parameters, such as reaction temperature, reaction time, and the Si/Al ratio in the raw materials, have been carefully tuned. The as-synthesized composite materials show good adsorption capacity for typical heavy metal(loid) ions. With 0.001 g/mL Fe2O3/FAU-type zeolite composite material added to different heavy metal(loid)-polluted aqueous solutions (single type of heavy metal(loid) concentration: 1,000 mg/L [ppm]), the adsorption capacity was shown to be 172, 45, 170, 40, 429, 693, 94, and 133 mg/g for Cu (II), Cr (III), Cr (VI), As (III), Cd (II), Pb (II), Zn (II), and Ni (II) removal, respectively, which can be further expanded for heavy metal-polluted water and soil remediation.

Resource Recycling of Red Soil to Synthesize Fe2O3/FAU-type Zeolite Composite Material for Heavy Metal Removal

This article presents a novel and convenient route to synthesize Fe2O3/faujasite (FAU)-type zeolite composite material from red soil. The detailed synthesis parameters have been finely tuned. The obtained composite material can be used for efficient heavy metal-contaminated water remediation, indicating its potential applications in environmental engineering.

重金属除去用Fe2O3/FAU型ゼオライト複合材料合成のための赤土の資源循環

Heavy metal-polluted water is of great concern to human health and the eco-environment. In situ water remediation techniques enabled by highly efficient ...

環境学

Luminescence Lifetime Imaging of O2 with a Frequency-Domain-Based Camera System

We describe a method to image dissolved oxygen (O2), in 2D at high spatial (&#60; 50-100 &#181;m) and temporal (&#60; 10 s) resolution. The method employs O2 sensitive luminescent sensor foils (planar optodes) in combination with a specialized camera system for imaging luminescence lifetime in the frequency-domain. Planar optodes are prepared by dissolving the O2-sensitive indicator dye in a polymer and spreading the mixture on a solid support in a defined thickness via knife coating. After evaporation of the solvent, the planar optode is placed in close contact with the sample of interest - here demonstrated with the roots of the aquatic plant Littorella uniflora. The O2 concentration-dependent change in the luminescence lifetime of the indicator dye within the planar optode is imaged via the backside of the transparent carrier foil and aquarium wall using a special camera. This camera measures the luminescence lifetime (&#181;s) via a shift in phase angle between a modulated excitation signal and emission signal. This method is superior to luminescence intensity imaging methods, as the signal is independent of the dye concentration or intensity of the excitation source, and solely relies on the luminescence decay time, which is an intrinsically referenced parameter. Consequently, an additional reference dye or other means of referencing are not needed. We demonstrate the use of the system for macroscopic O2 imaging of plant rhizospheres, but the camera system can also easily be coupled to a microscope.

Luminescence Lifetime Imaging of O2 with a Frequency-Domain-Based Camera System

We describe the use of a novel, frequency-domain luminescence lifetime camera for mapping 2D O2 distributions with optical sensor foils. The camera system and image analysis procedures are described along with the preparation, calibration and application of sensor foils for visualizing the O2 microenvironment in the rhizosphere of aquatic plants.

周波数領域ベースのカメラシステムを用いたO2の発光寿命イメージング

We describe a method to image dissolved oxygen (O2), in 2D at high spatial (&#60; 50-100 &#181;m) and temporal (&#60; 10 s) resolution. The method employs ...

Encapsulating Cytochrome c in Silica Aerogel Nanoarchitectures without Metal Nanoparticles while Retaining Gas-phase Bioactivity

Applications such as sensors, batteries, and fuel cells have been improved through the use of highly porous aerogels when functional compounds are encapsulated within the aerogels. However, few reports on encapsulating proteins within sol&#8211;gels that are processed to form aerogels exist. A procedure for encapsulating cytochrome c (cyt. c) in silica (SiO2) sol-gels that are supercritically processed to form bioaerogels with gas-phase activity for nitric oxide (NO) is presented. Cyt. c is added to a mixed silica sol under controlled protein concentration and buffer strength conditions. The sol mixture is then gelled and the liquid filling the gel pores is replaced through a series of solvent exchanges with liquid carbon dioxide. The carbon dioxide is brought to its critical point and vented off to form dry aerogels with cyt. c encapsulated inside. These bioaerogels are characterized with UV-visible spectroscopy and circular dichroism spectroscopy and can be used to detect the presence of gas-phase nitric oxide. The success of this procedure depends on regulating the cyt. c concentration and the buffer concentration and does not require other components such as metal nanoparticles. It may be possible to encapsulate other proteins using a similar approach making this procedure important for potential future bioanalytical device development.

Encapsulating Cytochrome c in Silica Aerogel Nanoarchitectures without Metal Nanoparticles while Retaining Gas-phase Bioactivity

This procedure describes how to encapsulate cytochrome c (cyt. c) in silica (SiO2) sol-gels, process these gels to form bioaerogels, and use these bioaerogels to rapidly recognize nitric oxide (NO) through a gas-phase reaction. This type of protocol may aid in the future development of biosensors or other bioanalytical devices.

発光ベースの湿度センサなどのナノ構造のAg-ゼオライト複合

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ZnOと同軸のTiO |光触媒活性セグメント化銀の調製および使用

ADOR（組立・解体・組織・再組み立て）ルートを使用したゼオライトの合成

検出とパラジウムの回収は、都市鉱山からの金やコバルト金属は、ナノスケールワゴンホイール形の細孔を有する指定小説センサ/吸着剤を使用しました

使い捨て電気化学紙のマイクロ流体のpHセンサーとしてイリジウム酸化還元グラフェン酸化物ナノハイブリッド薄膜変更されたスクリーン印刷電極

ゼオライトH-ZSM-5で高温・高圧のガス吸着用のLangatateクリスタルマイクロバランスに基づいて吸着装置

たTiO

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

重金属除去用_Fe2O3/FAU型ゼオライト複合材料合成のための赤土の資源循環

周波数領域ベースのカメラシステムを用いた_O2の発光寿命イメージング

シトクロムをカプセル化