This work is a part of the STW project "Integral solution for sustainable construction (IS2C, Fleur van Rossem for her support during the chip fabrication, Justyna Wiedemair for the chip design and Allison Bidulock for her support during the manuscript preparation.

1.チップ製造注：チップは、Ag / AgClの作用電極（WE）、銀/塩化銀擬似参照電極（擬似RE）とガラスチップ上に白金対向電極から構成されています。銀金属16を処理し 、標準的なクリーンルームを使用して、ガラスチップ上に堆積されます。次いで、それを表面上に塩化銀層を形成するために30秒間の0.1MのFeCl 3溶液中に塩素化されています。銀/塩化銀WE（面積= 9.812 平方ミリメートル）は 、図1に示すように、銀/塩化銀疑似REに囲まれ、中央部に位置しています。 <ol><li>平面銀電極を形成するために、ガラス上に金属銀を析出。次のようにクリーンルームでのステップバイステップのチップ製造を与えられます： <ol><li>リソグラフィー<ol><li>ウェハ洗浄のために、濃に最初のガラスウェハを浸します。表面をきれいにするために任意の有機汚染物を除去した後、1 M KOHにするHNO 3風呂。 </li><li> （厚さ200nm）にポジ型レジスト写真を適用しますスピンコーティングによりウエハ、15分間95℃でレジストをプリベーク。 </li><li>ガラスマスクを介して、5秒間UV光にウェハを公開します。 </li><li>現像液中​​のフォトレジストを開発します。これは、電極が堆積され、残りの領域をレジスト未露光によってカバーされるガラスの面積を公開します。 </li></ol></li><li>ガラスエッチング<ol><li>ガラスの露出領域をエッチングするためにKOHの浴に開発ガラスウェーハを浸します。 </li></ol></li><li>金属蒸着（スパッタリング） <ol><li>露出したガラスエリアでの預金銀金属。 <ol><li>第一のガラスのための接着層として20nmのチタン（スパッタリングによって）チタン（Ti）層を堆積させます。 </li><li>次いで、銀とTiとの間の拡散バリアとして（スパッタリングによって）70n​​mのパラジウム（Pd）層を堆積させます。 </li><li>最後に、銀金属の500 nmのを堆積させます。これは、堆積された金属の厚さです。作用電極の面積を4mm 2です。 </li><li> Rを削除しますアセトン浴中でリフトオフ法によりレジストをemaining。 </li></ol></li><li>シングルチップサイズにウェハをDICE。チップは現在、オンチップのAg / AgCl電極を形成するために塩素化される準備ができています。 </li></ol></li></ol></li><li> 図1に示すように、社内で設計されたポリテトラフルオロエチレンチップホルダにチップを置きます。ホルダーは、プッシュピン（またはバネ式のピン）を介して容易に電気的接続を提供し、電気化学セルが含まれています。 </li><li>チップ上のAg / AgCl電極を形成する銀電極を塩化物にします。そのために、30秒間、細胞中の0.1MのFeCl 3溶液を注ぎます。または電極のシルバー色まで暗い灰色がかったなり。短い浸漬時間は、Ag / AgClでの析出につながることができ、一方、より長い浸漬は重要ではありません。 </li><li>残りのFeCl 3【選択チップをきれいにするために脱イオン水でチップをすすぐ今クロノ測定に使用する準備が整いました。 </li></ol>2.電解準備注：電解質は、0.5M KNO 3における塩化カリウムの異なる濃度で調製しました。 <ol><li> 50のKCl電解質原液（溶液50ml中のKClの0.186グラム）の50ミリリットルを準備します。 </li><li>同じ溶液中0.5 M KNO 3バックグラウンド電解質を形成するために、KNO 3の2.52グラムを追加します。 </li><li>脱イオン水50mlにKNO 3の2.52グラムを追加し、他の言葉ではM. 0.5にゼロとKNO 3に塩化物の出発濃度を保管してください。 </li><li>以下の手順に示すように、体系的に、電解質（1ミリモルから6ミリメートル）の塩化物イオン濃度を増加させるための50mMのKClを加えます。 <ol><li> 1 mMの[CL]を取得するために、0.5M KNO 3の4.9ミリリットルに50mMのKClを100μlのを追加します。 </li><li> 2 mMの[CL]を取得するステップ2.4​​.1の溶液に50mMのKCl溶液の104μLを加えます。 </li><li> sの中に50mMのKCl溶液の108.41μLを追加3 mMの[CL]を取得するためのステップ2.4​​.2のolution。 </li><li> 4 mMの[CL]を取得するステップ2.4​​.3の溶液に50mMのKCl溶液の113.19μLを加えます。 </li><li> 5 mMの[CL]を取得するステップ2.4​​.4の溶液に50mMのKCl溶液の118.2μLを加えます。 </li><li> 6 mMの[CL]を取得するステップ2.4​​.5の溶液に50mMのKCl溶液の123.3μLを加えます。 </li></ol></li></ol> 3.実験のセットアップ注：測定は、ポテンショスタット（生物学的科学器具、フランス）を用いて行きました。 <ol><li>チップホルダにチップを置き、ポテンショスタットの対応する端子に接続します。 </li><li> Ag / AgCl電極をポテンショスタットの作用電極端子を接続します。 </li><li>別のAg / AgCl電極をポテンショスタットの参照電極端子を接続します。 </li><li>白金電極にポテンショスタットの対向電極端子を接続します。 </li><li>カンプを配置周囲の騒音を避けるために、ファラデーケージ内LETE実験のセットアップ。 </li></ol> 4.機器の操作設定注：電気化学セルの動作パラメータは、ポテンシオスタットのユーザインタフェースを介して制御されます。印加電流パルス中のAg / AgClをWEの電位応答は、塩化物イオンの異なる濃度について測定されます。 <ol><li>ポテンショスタットのプログラムでは、技術のクロノを開き、動作パラメータを設定します。 <ol><li>要件に応じて次のパラメータを設定します。 <ol><li>電流（I S） </li><li>印加電流（T 秒 ）の時間</li></ol></li><li>ポテンショスタットプログラムで再生ボタンをクリックすることで、この技術を起動します。 注：ポテンショスタットプログラムが適用される電流パルスの下で時間の関数としての潜在的な応答が表示されます。 </li></ol></li></ol> 5.測定とデータAnalysiの<ol><li>電解液中のClイオン濃度対遷移時間の検量線を描画します。 <ol><li>系統的に、塩化カリウム電解液中のCl濃度を変更します。 <ol><li>電気化学セル中の0.5M KNO 3バックグラウンド電解質と1のKClの5ミリリットルで測定を開始します。 </li><li>ポテンショスタットを使用してクロノ実験を開始し、10ミリアンペア/ cm -2で10秒間の電流を印加し、データを格納します。 </li><li>系統的に1 mMの刻みで6 mmの濃度を変更し、測定を繰り返します。 </li></ol></li><li> a.mptファイルとして測定されたデータを格納し、データ処理プログラムのデータファイルを分析します。 <ol><li>電位応答の一次導関数を計算し、一次微分のピークを計算するために社内開発されたデータ処理プログラムを使用してデータを分析します。一次導関数のピークは、遷移時間です。 注：完全なタラをデータ処理プログラムのINGはのアッバスら、2014補足情報に記載されています。 </li></ol></li><li> 1時間ごとの間隔で測定を3回繰り返します。 </li><li>データ処理プログラムですべてのデータファイルを開き、各測定のための遷移時間を計算します。遷移時間計算の詳細手順は以下のとおりであります： <ol><li>クロノ計測のデータファイルから取得した対時間の電位差をプロットします。 </li><li>電位応答の一次導関数を計算します。 </li><li>一次導関数の最大値と、それの時間を示します。一次導関数の最大値の時間は、遷移時間です。 </li></ol></li><li>検量線は、CLイオン濃度に対する遷移時間の平方根をプロット。 </li><li>測定したデータに沿って砂の式25に基づく理論曲線をプロットします。拡散coefficを逆算データプロットからient。 <ol><li>遷移時間との間で測定されたデータプロットで[CL]ライン上の任意の点を取ると、遷移時間の値と[CL]を記録します。砂の方程式は以下のように与えられます。 τ=（FC * / 2J（1-T のCl - ））2Dπ トランスポート番号であり、Dは拡散係数である-ここで、C *は、バルクのClイオン濃度であり、Fはファラデー定数、Jは電流密度、T Clです 。ネグレクトトンのCl -それは、より高いバックグラウンド電解質濃度のためにゼロに近づくので。 </li><li>拡散係数の砂方程式で唯一残っている変数。遷移時間、塩化物イオン濃度および拡散係数の値を取得砂式の印加電流値を置きます。 </li></ol></li></ol></li><li>ドリフト測定<ol><li>中のKClの1 mMと5ミリリットルを注ぎます電気化学セル。 </li><li>ポテンショスタットでは、現在適用されているが、午前10時-2、時間は10秒となるように設定します。 </li><li>測定間の3時間の間隔で3つの測定毎日で2週間のための潜在的な応答を測定します。 </li><li>電解質、 すなわち、1のKCl、測定を行う前に、毎日更新します。 </li><li>測定値の2週間にわたって遷移時間をプロットします。一日あたりの遷移時間の変化は、遷移時間応答のドリフトです。 </li></ol></li><li>遷移時間測定の擬似参照電極の影響 注：このような銀/塩化銀線、白金線と鋼線のような様々な擬似参照は、遷移時間を測定するために試験されます。 <ol><li>電気化学セルでのKCl電解質の4 mMのを注ぎます。 </li><li>擬似参照電極として銀/塩化銀を使用し、ポテンシオスタットの参照電極端子に接続します。陽極電流パルスのCl＆＃へ713;イオンは、Ag / AgClの作用電極の近くに空乏化されます。 </li><li> 10秒間15アム-2の電流密度を印加することにより、クロノ測定を行います。 </li><li>擬似参照電極として白金で測定を繰り返し、データを記録します。 </li><li>擬似参照電極としての鋼棒を用いた測定を繰り返し、データを記録します。 </li><li>使用される様々な擬似参照電極のための測定された遷移時間をプロットします。 </li><li> KCl 5mMのと測定の完全なセットを繰り返し、様々な擬似参照電極を使用して遷移時間をプロットします。 </li></ol></li></ol>

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The authors have nothing to disclose.

遷移時間は変曲の瞬間です。それは、基準電位、すなわち、参照電極の理論的に独立しています。したがって、任意の金属線は、遷移時間測定のための擬似参照電極として用いることができます。コンクリート中の塩化物イオンの既存の電位差測定とは対照的に、この方法は、長期的かつキャリブレーションのない測定を可能にします。さらに感度及び濃度の検出範囲は、印加される?...

Ag / AgCl電極の遷移時間測定に基づいて、塩化物イオンセンサが提供されます。目的は、電解液中の塩化物イオンの長時間連続監視中に固有のドリフトを回避することです。 Ag / AgCl電極の動的な測定手法であるクロノポテンシオメトリー測定は、この目的のために使用されます。ここでのAg / AgCl電極の電位の変化の割合は、刺激（定電流パルス）の間に測定されます。このアプローチの利点は、次のような現場アプリケーション、従って長期（数年）のためのClイオン濃度の検出を可能にする、液体接合参照電極を逃亡し、代わりに、擬似参照電極としての金属製のワイヤを使用し、 で実証されていますコンクリート構造物内部の測定。 コンクリート構造物中の塩化物イオンが劣化1,2の主要な原因の1つです。これは、補強鋼aで孔食開始します構造3の最終的な失敗でND結果。そのため、コンクリート中のClイオンを測定することは、構造4,5の寿命やメンテナンスサイクルを予測することは避けられません。異なる感知原理は、電気化学的な6,7、光学8,9電磁10,11として、コンクリート中の塩化物イオンの測定のために報告されています。しかし、かさばるセットアップを持っている光学、電磁方法、スタンドアロンシステムとして統合し、選択性12の問題を持ってすることは困難です。電気化学的手法では、銀/塩化銀電極の電位差測定は、技術のアプローチ6,7,13の状態です。有望な結果にもかかわらず、このアプローチは、欠陥のあるデータ14,15における基準電位と拡散電位降下結果のドリフトので、実験室規模の測定に限定されています。動的電気化学測定（DEM）に基づいて、遷移時間のアプローチは、潜在的に問題を軽減することができ16ドリフト 。 DEMでは、適用される刺激に対するシステムの応答は、17から19を測定しました。そのようなシステムの例は、クロノポテンショメトリーです。ここで適用される電流パルスは、電極表面近くにイオンを枯渇させる刺激として使用され、対応する電位応答が測定されます。 Ag / AgCl電極で陽極電流がファラデー反応を開始銀（Ag + CL <img alt="図1" src="/files/ftp_upload/53312/arrow.jpg" /> AgCl + e）は、電極表面近くのClイオンの枯渇をもたらします。電位変化は、印加される電流の関数であり、電解質12,20で（選択）イオンの濃度です。現時点では、これらのイオンは、変曲点21を与え 、完全に電極表面近傍に急速に電位上昇の変化率を枯渇させます。電位 - 時間応答曲線（クロノポテンショグラム）上の変曲点は、​​遷移時間を示すから決定することができます電位応答22の一次導関数の最大値。遷移時間は、イオン濃度の特徴です。このアプローチは、異なるイオン濃度17および電解質23,24のpHを決定するために使用されています。 （電流が印加される）作用電極としてのAg / AgCl電極の場合に枯渇イオンは、塩化物イオン17あろう。したがって、その遷移時間を測定し、その濃度を決定します。

<table border="0" cellpadding="0" cellspacing="0" width="1009">
	<tbody>
		<tr height="25">
			<td height="25" style="height:25px;width:373px;">Platinum wire (&#8805;99.99% trace metals)</td>
			<td style="width:292px;">Sigma Aldrich, the Netherlands</td>
			<td style="width:172px;">EP1330-1EA</td>
			<td style="width:172px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Potassium chloride (BioXtra, &#8805;99.0%)</td>
			<td>Sigma Aldrich, the Netherlands</td>
			<td>P9333-500G</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Potassium hydroxide (90% pure reagent grade)</td>
			<td>Sigma Aldrich, the Netherlands</td>
			<td>484016-1KG</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Ferric chloride&#160;</td>
			<td>Sigma Aldrich, the Netherlands</td>
			<td>451649-1G</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">potassium nitrate (&#62; 99% reagent grade)&#160;</td>
			<td>Sigma Aldrich, the Netherlands</td>
			<td>P6083-500G</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Ag/AgCl liquid junction reference electrode&#160;</td>
			<td>BASi, USA</td>
			<td>model MF-2079</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">VSP potentiostat</td>
			<td>Biologic Science Instruments, France</td>
			<td>VSP 300</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Steel wire</td>
			<td>Microlab TU Delft</td>
			<td></td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Silver wire&#160;</td>
			<td>Sigma Aldrich, the Netherlands</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

dynamic electrochemical measurement of chloride ions

This protocol describes the dynamic measurement of chloride ions using the transition time of a silver silver chloride (Ag/AgCl) electrode. Silver silver chloride electrode is used extensively for potentiometric measurement of chloride ions concentration in electrolyte. In this measurement, long-term and continuous monitoring is limited due to the inherent drift and the requirement of a stable reference electrode. We utilized the chronopotentiometric approach to minimize drift and avoid the use of a conventional reference electrode. A galvanostatic pulse is applied to an Ag/AgCl electrode which initiates a faradic reaction depleting the Cl&#713; ions near the electrode surface. The transition time, which is the time to completely deplete the ions near the electrode surface, is a function of the ion concentration, given by the Nernst equation. The square root of the transition time is in linear relation to the chloride ion concentration. Drift of the response over two weeks is negligible (59 &#181;M/day) when measuring 1 mM [Cl&#713;]using a current pulse of 10 Am-2. This is a dynamic measurement where the moment of transition time determines the response and thus is independent of the absolute potential. Any metal wire can be used as a pseudo-reference electrode, making this approach feasible for long-term measurement inside concrete structures.

Ag / AgCl電極は、標準的なクリーンルームのプロセスを用いてガラスチップ（ 図1.）上に製造されます。クロノポテンシオメトリー測定セットアップ（ 図2）を使用し、応答をポテンシオスタットを用いて測定しました。遷移時間でのClイオン濃度の影響を観察するために、0.5 M KNO 3バックグラウンド中のClイオンの4、5及び6ミリモルを?...

Watch this Scientific Journal Video about Dynamic Electrochemical Measurement of Chloride Ions at JoVE.com

Dynamic Electrochemical Measurement of Chloride Ions

Dynamic measurement of chloride ions is presented. Transition time of an Ag/AgCl electrode, during a chronopotentiometric technique, can give the concentration of chloride ions in electrolyte. This method does not require a stable conventional reference electrode.

塩化物イオンの動的電気化学測定

This protocol describes the dynamic measurement of chloride ions using the transition time of a silver silver chloride (Ag/AgCl) electrode. Silver silver ...

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11.3K ビュー.  University of Twente. Dynamic measurement of chloride ions is presented. Transition time of an Ag/AgCl electrode, during a chronopotentiometric technique, can give the concentration of chloride ions in electrolyte. This method does not require a stable conventional reference electrode.

ビデオ: Dynamic Electrochemical Measurement of Chloride Ions

Activating Molecules, Ions, and Solid Particles with Acoustic Cavitation

The chemical and physical effects of ultrasound arise not from a direct interaction of molecules with sound waves, but rather from the acoustic cavitation: the nucleation, growth, and implosive collapse of microbubbles in liquids submitted to power ultrasound. The violent implosion of bubbles leads to the formation of chemically reactive species and to the emission of light, named sonoluminescence. In this manuscript, we describe the techniques allowing study of extreme intrabubble conditions and chemical reactivity of acoustic cavitation in solutions. The analysis of sonoluminescence spectra of water sparged with noble gases provides evidence for nonequilibrium plasma formation. The photons and the "hot" particles generated by cavitation bubbles enable to excite the non-volatile species in solutions increasing their chemical reactivity. For example the mechanism of ultrabright sonoluminescence of uranyl ions in acidic solutions varies with uranium concentration: sonophotoluminescence dominates in diluted solutions, and collisional excitation contributes at higher uranium concentration. Secondary sonochemical products may arise from chemically active species that are formed inside the bubble, but then diffuse into the liquid phase and react with solution precursors to form a variety of products. For instance, the sonochemical reduction of Pt(IV) in pure water provides an innovative synthetic route for monodispersed nanoparticles of metallic platinum without any templates or capping agents. Many studies reveal the advantages of ultrasound to activate the divided solids. In general, the mechanical effects of ultrasound strongly contribute in heterogeneous systems in addition to chemical effects. In particular, the sonolysis of PuO2 powder in pure water yields stable colloids of plutonium due to both effects.

Acoustic cavitation in liquids submitted to power ultrasound creates transient extreme conditions inside the collapsing bubbles, which are the origin of unusual chemical reactivity and light emission, known as sonoluminescence. In the presence of noble gases, nonequilibrium plasma is formed. The "hot" particles and the photons generated by collapsing bubbles are able to excite species in solution.

分子、イオン、および音響キャビテーションと固体粒子を活性化

The chemical and physical effects of ultrasound arise not from a direct interaction of molecules with sound waves, but rather from the acoustic ...

化学

Measurement of Particle Size Distribution in Turbid Solutions by Dynamic Light Scattering Microscopy

A protocol for measuring polydispersity of concentrated polymer solutions using dynamic light scattering is described. Dynamic light scattering is a technique used to measure the size distribution of polymer solutions or colloidal particles. Although this technique is widely used for the assessment of polymer solutions, it is difficult to measure the particle size in concentrated solutions due to the multiple scattering effect or strong light absorption. Therefore, the concentrated solutions should be diluted before measurement. Implementation of the confocal optical component in a dynamic light scattering microscope1 helps to overcome this barrier. Using such a microscopic system, both transparent and turbid systems can be analyzed under the same experimental setup without a dilution. As a representative example, a size distribution measurement of a temperature-responsive polymer solution was performed. The sizes of the polymer chains in an aqueous solution were several tens of nanometers at a temperature below the lower critical solution temperature (LCST). In contrast, the sizes increased to more than 1.0 &#181;m when above the LCST. This result is consistent with the observation that the solution turned turbid above the LCST.

A protocol for the direct measurement of particle size distribution in concentrated solutions using dynamic light scattering microscopy is presented.

動的光散乱顕微鏡による濁りソリューションにおける粒度分布の測定

A protocol for measuring polydispersity of concentrated polymer solutions using dynamic light scattering is described. Dynamic light scattering is a ...

Fabrication and Testing of Photonic Thermometers

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being leveraged for developing sophisticated photonic sensors. Silicon photonic sensors seek to exploit the strong confinement of light in nano-waveguides to transduce changes in physical state to changes in resonance frequency. In the case of thermometry, the thermo-optic coefficient, i.e., changes in refractive index due to temperature, causes the resonant frequency of the photonic device such as a Bragg grating to drift with temperature. We are developing a suite of photonic devices that leverage recent advances in telecom compatible light sources to fabricate cost-effective photonic temperature sensors, which can be deployed in a wide variety of settings ranging from controlled laboratory conditions, to the noisy environment of a factory floor or a residence. In this manuscript, we detail our protocol for the fabrication and testing of photonic thermometers.

We describe the process of fabrication and testing of photonic thermometers.

光温度計の作製と試験

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

電気化学インピー ダンス分光電気化学定数推定法のためのツールとして

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Preparation of Stable Bicyclic Aziridinium Ions and Their Ring-Opening for the Synthesis of Azaheterocycles

Bicyclic aziridinium ions were generated by the removal of an appropriate leaving group through internal nucleophilic attack by nitrogen atom in the aziridine ring. The utility of bicyclic aziridinium ions, specifically 1-azoniabicyclo[3.1.0]hexane and 1-azoniabicyclo[4.1.0]heptane tosylate highlighted in the aziridine ring openings by the nucleophile with the release of the ring strain to yield the corresponding ring-expanded azaheterocycles such as pyrrolidine, piperidine and azepane with diverse substituents on the ring in regio- and stereospecific manner. Herein, we report a simple and convenient method for the preparation of the stable 1-azabicyclo[4.1.0]heptane tosylate followed by selective ring opening via a nucleophilic attack either at the bridge or at the bridgehead carbon to yield piperidine and azepane rings, respectively. This synthetic strategy allowed us to prepare biologically active natural products containing piperidine and azepane motif including sedamine, allosedamine, fagomine and balanol in highly efficient manner.

Bicyclic aziridinium ions such as 1-azoniabicyclo[4.1.0]heptane tosylate were generated from 2-[4-tolenesulfonyloxybutyl]aziridine, which was utilized for the preparation of substituted piperidines and azepanes via regio- and stereospecific ring-expansion with various nucleophiles. This highly efficient protocol allowed us to prepare diverse azaheterocycles including natural products such as fagomine, febrifugine analogue and balanol.

安定した二環性 Aziridinium イオンと開環の Azaheterocycles の合成のための準備

Bicyclic aziridinium ions were generated by the removal of an appropriate leaving group through internal nucleophilic attack by nitrogen atom in the ...

Disentangling High Strength Copolymer Aramid Fibers to Enable the Determination of Their Mechanical Properties

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to diversify the fiber choices in the United States body armor market, copolymer fibers based on the combination of 5-amino-2-(p-aminophenyl) benzimidazole (PBIA) and the more conventional PPTA were introduced. Little is known regarding the long-term stability of these fibers, but as condensation polymers, they are expected to have potential sensitivity to moisture and humidity. Therefore, characterizing the strength of the materials and understanding their vulnerability to environmental conditions is important for evaluating their use lifetime in safety applications. Ballistic resistance and other critical structural properties of these fibers are predicated on their strength. To accurately determine the strength of the individual fibers, it is necessary to disentangle them from the yarn without introducing any damage. Three aramid-based copolymer fibers were selected for the study. The fibers were washed with acetone followed by methanol to remove an organic coating that held the individual fibers in each yarn bundle together. This coating makes it difficult to separate single fibers from the yarn bundle for mechanical testing without damaging the fibers and affecting their strength. After washing, fourier transform infrared (FTIR) spectroscopy was performed on both washed and unwashed samples and the results were compared. This experiment has shown that there are no significant variations in the spectra of poly(p-phenylene-benzimidazole-terephthalamide-co-p-phenylene terephthalamide) (PBIA-co-PPTA1) and PBIA-co-PPTA3 after washing, and only a small variation in intensity for PBIA. This indicates that the acetone and methanol rinses are not adversely affecting the fibers and causing chemical degradation. Additionally, single fiber tensile testing was performed on the washed fibers to characterize their initial tensile strength and strain to failure, and compare those to other reported values. Iterative procedural development was necessary to find a successful method for performing tensile testing on these fibers.

The primary goal of the study is to develop a protocol to prepare consistent specimens for accurate mechanical testing of high strength copolymer aramid fibers, by removing a coating and disentangling the individual fiber strands without introducing significant chemical or physical degradation.

その力学的特性の測定を可能にする高強度共重合体のアラミド繊維を disentangling

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to ...

Electrochemical Roughening of Thin-Film Platinum Macro and Microelectrodes

This protocol demonstrates a method for electrochemical roughening of thin-film platinum electrodes without preferential dissolution at grain boundaries of the metal. Using this method, a crack free, thin-film macroelectrode surface with up to 40 times increase in active surface area was obtained. The roughening is easy to do in a standard electrochemical characterization laboratory and incudes the application of voltage pulses followed by extended application of a reductive voltage in a perchloric acid solution. The protocol includes the chemical and electrochemical preparation of both a macroscale (1.2 mm diameter) and microscale (20 &#181;m diameter) platinum disc electrode surface, roughening the electrode surface and characterizing the effects of surface roughening on electrode active surface area. This electrochemical characterization includes cyclic voltammetry and impedance spectroscopy and is demonstrated for both the macroelectrodes and the microelectrodes. Roughening increases electrode active surface area, decreases electrode impedance, increases platinum charge injection limits to those of titanium nitride electrodes of same geometry and improves substrates for adhesion of electrochemically deposited films.

This protocol demonstrates a method for electrochemical roughening of thin-film platinum electrodes without preferential dissolution at grain boundaries. The electrochemical techniques of cyclic voltammetry and impedance spectroscopy are demonstrated to characterize these electrode surfaces.

薄膜白金マクロ及びマイクロ電極の電気化学粗化

This protocol demonstrates a method for electrochemical roughening of thin-film platinum electrodes without preferential dissolution at grain boundaries ...

Asymmetric Thermoelectrochemical Cell for Harvesting Low-grade Heat under Isothermal Operation

Low-grade heat is abundantly available in the environment as waste heat. The efficient conversion of low-grade heat into electricity is very difficult. We developed an asymmetric thermoelectrochemical cell (aTEC) for heat-to-electricity conversion under isothermal operation in the charging and discharging processes without exploiting the thermal gradient or the thermal cycle. The aTEC is composed of a graphene oxide (GO) cathode, a polyaniline (PANI) anode, and 1M KCl as the electrolyte. The cell generates a voltage due to the pseudocapacitive reaction of GO when heating from room temperature (RT) to a high temperature (TH, ~40-90 &#176;C), and then current is successively produced by oxidizing PANI when an external electrical load is connected. The aTEC demonstrates a remarkable temperature coefficient of 4.1 mV/K and a high heat-to-electricity conversion efficiency of 3.32%, working at a TH = 70 &#176;C with a Carnot efficiency of 25.3%, unveiling a new promising thermoelectrochemical technology for low-grade heat recovery.

Low-grade heat is abundant, but its efficient recovery is still a great challenge. We report an asymmetric thermoelectrochemical cell using graphene oxide as a cathode and polyaniline as an anode with KCl as the electrolyte. This cell works under isothermal heating, exhibiting a high heat-to-electricity conversion efficiency in low-temperature regions.

等温運転下で低品位熱を収穫するための非対称熱電気化学セル

Low-grade heat is abundantly available in the environment as waste heat. The efficient conversion of low-grade heat into electricity is very difficult. We ...

Fabrication of Thin Film Silver/Silver Chloride Electrodes with Finely Controlled Single Layer Silver Chloride

This paper aims to present a protocol to form smooth and well-controlled films of silver/silver chloride (Ag/AgCl) with designated coverage on top of thin film silver electrodes. Thin film silver electrodes sized 80 &#181;m x 80 &#181;m and 160 &#181;m x 160 &#181;m were sputtered on quartz wafers with a chromium/gold (Cr/Au) layer for adhesion. After passivation, polishing and cathodic cleaning processes, the electrodes underwent galvanostatic oxidation with consideration of Faraday&#39;s Law of Electrolysis to form smooth layers of AgCl with a designated degree of coverage on top of the silver electrode. This protocol is validated by inspection of scanning electron microscope (SEM) images of the surface of the fabricated Ag/AgCl thin film electrodes, which highlights the functionality and performance of the protocol. Sub-optimally fabricated electrodes are fabricated as well for comparison. This protocol can be widely used to fabricate Ag/AgCl electrodes with specific impedance requirements (e.g., probing electrodes for impedance sensing applications like impedance flow cytometry and interdigitated electrode arrays).

This paper aims to present a method to form smooth and well-controlled films of silver chloride (AgCl) with designated coverage on top of thin film silver electrodes.

細かく制御された単層塩化銀を用いた薄膜銀/塩化銀電極の製造

This paper aims to present a protocol to form smooth and well-controlled films of silver/silver chloride (Ag/AgCl) with designated coverage on top of thin ...

Probing Surface Electrochemical Activity of Nanomaterials using a Hybrid Atomic Force Microscope-Scanning Electrochemical Microscope (AFM-SECM)

Scanning electrochemical microscopy (SECM) is used to measure the local electrochemical behavior of liquid/solid, liquid/gas and liquid/liquid interfaces. Atomic force microscopy (AFM) is a versatile tool to characterize micro- and nanostructure in terms of topography and mechanical properties. However, conventional SECM or AFM provides limited laterally resolved information on electrical or electrochemical properties at nanoscale. For instance, the activity of a nanomaterial surface at crystal facet levels is difficult to resolve by conventional electrochemistry methods. This paper reports the application of a combination of AFM and SECM, namely, AFM-SECM, to probe nanoscale surface electrochemical activity while acquiring high-resolution topographical data. Such measurements are critical to understanding the relationship between nanostructure and reaction activity, which is relevant to a wide range of applications in material science, life science and chemical processes. The versatility of the combined AFM-SECM is demonstrated by mapping topographical and electrochemical properties of faceted nanoparticles (NPs) and nanobubbles (NBs), respectively. Compared to previously reported SECM imaging of nanostructures, this AFM-SECM enables quantitative assessment of local surface activity or reactivity with higher resolution of surface mapping.

Probing Surface Electrochemical Activity of Nanomaterials using a Hybrid Atomic Force Microscope-Scanning Electrochemical Microscope AFM-SECM

Atomic force microscopy (AFM) combined with scanning electrochemical microscopy (SECM), namely, AFM-SECM, can be used to simultaneously acquire high-resolution topographical and electrochemical information on material surfaces at nanoscale. Such information is critical to understanding heterogeneous properties (e.g., reactivity, defects, and reaction sites) on local surfaces of nanomaterials, electrodes and biomaterials.

ハイブリッド原子間力顕微鏡走査型電気化学顕微鏡(AFM-SECM)を用いたナノ材料の表面電気化学的活性の調査

Scanning electrochemical microscopy (SECM) is used to measure the local electrochemical behavior of liquid/solid, liquid/gas and liquid/liquid interfaces. ...