The authors wish to acknowledge the competitive faculty-initiated collaboration (FIC) grant from KAUST.

Prをドープしたチタン酸ストロンチウム3粉末の調製<ol><li>のTiO 3粉末のSr 0.95のPr 0.05 10gを調製するために、反応後のSrCO 3粉末（7.53407グラム）、TiO 2のナノ粉末（4.28983グラム）、及びPr 2 O 3焼結塊（0.44299グラム）の化学量論量を量りますX = 0.05のための： </li></ol><img alt="式（1）" fo:content-width="5in" src="/files/ftp_upload/52869/52869eq1.JPG" width="550" /><ol start="2"><li>めのう乳鉢と乳棒を用いて微細な粒子に秤量のPr 2 O 3焼結塊を粉砕。 </li><li>のPr 2 O 3を秤量のSrCO 3粉末とTiO 2ナノ粉末を追加して、視覚的に均質な粉末が得られるまで瑪瑙乳鉢と乳棒を用いて粉砕し、混合を続けます。 </li><li>ガラスジャーに粉砕粉をロードし、目を均一化するために30分間攪拌器を用いて混合しますE混合物。 </li><li>細心の注意を払って清掃し、研磨されたステンレス鋼製の型（直径1インチ）に、得られた混合粉末をロードし、2つのステンレス鋼プランジャの間に挟みます。 </li><li>冷間プレス、約1トンの荷重でプレスを用いた粉末。 </li><li>中空ステンレス製の筒にダイを配置し、プッシュロッドを使用して、上部からプランジャ、ペレットを押すことにより、コールドプレスペレットを取り出します。ダイから冷たいプレスペレット（素地）の吐出時に、静かにスコッチテープの小片でペレットをカバーし、テープをリッピングすることにより薄層を除去することにより、ペレットの周面に汚れをきれいに。 </li><li>アルミナボートやコールドプレスペレットとの間の障壁として市販品を購入したSrTiO 3粉末を充填したアルミナボートに垂直にペレットを配置します。 </li><li> 、チューブ炉内にボートを置いて3時間で1300℃まで加熱し、15のために、この温度で​​それを保ちます時間。焼成が終わったとき、ペレットは炉内を室温に冷却します。この工程は、その後、「焼成工程」と呼びます。 </li><li>めのう乳鉢と乳棒を用いてペレットを粉砕し、さらにタービュレータを使用して混合するためのガラスジャーに得られた粉末をロードします。 </li><li>負荷の約3トンでプレスステンレス製の金型と寒さの中に粉末をロードします。 </li><li> 3時間で1400℃でステップ1.9 1つをより多くの時間を繰り返し、20時間この温度に保ちます。 </li><li>めのう乳鉢と乳棒を用いてペレットを粉砕。 </li><li>繰り返して完成に到達するための固相反応のための1.11、1.12、および1.13 1より多くの時間を繰り返します。 </li></ol>バルク多結晶のPrをドープしたSrTiO 3セラミックスの作製<ol><li> （厚さ2mm、直径12.7ミリメートルディスク用）として調製された粉末1.6グラムを計量。 </li><li>上部と下部のINTEをカバーするために、円形graphoil片を作成グラファイトダイスに挟まれた粉末と黒鉛プランジャのrface。また、グラファイト金型の内壁を覆うように、別の長方形graphoil片を作製。 </li><li>グラファイトダイス（内径12.7ミリメートル）に調製されたままの粉末をロードし、同じサイズの2つの黒鉛プランジャとの間の粉末を挟みます。温度読み取りのためのグラファイトダイの長さの途中で、ダイの外側表面から内側表面の約2mm〜2 mmの穴をドリル。 注：金型外に残っている黒鉛プランジャの長さを調整し、穴が正確な温度測定値を取得するために配置されて挟まれた粉末円筒の中心を合わせます。グラファイトプランジャの顔は細心の注意を払っ個の加工中に平準化する必要があります。任意のずれが放電プラズマ焼結時の焼結ペレットの分解をもたらすことができます。 </li><li>コー​​ルドプレススパークに取り付ける前にプレスを用いて粉末優しく（負荷&lt;200キロ）チャンバ内のプラズマ焼結板。グラファイトプランジャの損傷を防ぐために、上部と下部のプランジャーを押してステージ間の平坦研磨されたステンレス鋼製の支持板を使用してください。 </li><li>グラファイトの一枚をラップ絶縁のために、ダイの周りに感じ、グラファイト糸で固定します。温度読み取りホールがダイ上に配置されているフェルトの長方形部分を切断することにより、グラファイトフェルト上にウィンドウを考案。 </li><li>放電プラズマ焼結室に装填されたグラファイトダイおよびプランジャを配置します。最終的な位置にステージを移動します。 </li><li>フォーカスとダイの温度読み取りホールの温度計の目標円を合わせます。高温計の放射率設定は、黒鉛に設定されていることを確認します。 </li><li>室を閉じて、試料上に7.7 kNの荷重（約60メガパスカル）を置きます。真空およびArで3回チャンバーをパージし、6 Paでの動的真空下室を残します。 </li><li>手動（電流を増加させるか、使用して温度を上昇させますプログラム）。 250分-1使用（に対応する約300〜400℃の分-1）に最適化サンプルのため。これは、放電プラズマ焼結法の最も重要なステップです。 </li><li>手動で電流を調整するか、プログラムを使用して5分​​間1,500℃の温度を保ちます。 5分間の保持期間の終了時に、電流を遮断し、迅速に冷却中にサンプルを割れ避けるために、7.7 kNの荷重を解放します。室内のRTにサンプルが冷まします。 </li><li>グラファイトからバルクペレットを離し冷間プレスを使用して静かに死にます。これは、中空鋼製シリンダーにグラファイトダイスを置き、上からロッドを押す鋼を使用してペレットとグラファイトプランジャを吐出することで行われます。 </li><li>鋭利なカミソリの刃を使用してペレットの上下面だけでなく、周面にgraphoilを削除します。 </li><li>保証するために、それぞれの側から粗いサンドペーパーをダウン0.3〜0.5ミリメートルのための（400グリッド）を使用してサンプルを磨きますgraphoilを完全に除去します。アセトンでサンプルを清掃してください。 </li></ol>電子·バルクセラミックスの熱輸送特性の3キャラクタリゼーション<ol><li>アルキメデス法を用いて、セラミックディスク、ρの密度を決定します。 </li><li>試料の重量を測定し、W の乾燥 、次いで、水に沈めた試料の重量W安定化濃度の測定システムに、 ウェットからアルキメデスの密度を計算します</li></ol><img alt="式（2）" fo:content-width="2.1in" src="/files/ftp_upload/52869/52869eq2.JPG" width="260" /> ρ 水は測定温度での水の密度である。14（ 例えば、1グラムcm -3の300 Kで等しいです） <ol start="2"><li>アルゴンを75ml分-1流下過渡レーザーフラッシュ法を用いて、サンプルDの熱拡散率を測定します。厚さを測定サンプル、Lの、正確に最初のデジタルマイクロメーターを使用して。 異なるサイズおよび形状のサンプル（直径または正方形で例えば円形ディスク12.7ミリメートル10×10ミリメートル2ディスク）パラレル直面し、0.5と5ミリメートルの間の厚さを容易に測定することができます注意してください。 <ol><li>レーザーフラッシュ熱拡散法では、短い（約1秒）のレーザーパルスによって試料の一方の面に照射し、赤外線検出器の反対面の温度上昇を記録します。次に、試料の厚さ及びパーカー式15を用いて、昇温時間プロファイルからレーザーフラッシュインタフェースソフトウェアにより熱拡散率を算出します</li></ol></li></ol><img alt="式3" fo:content-width="1.9in" src="/files/ftp_upload/52869/52869eq3.JPG" width="220" /> Lは、ディスクの厚さであり、t 1/2は、他の複数の最大温度上昇の半分の時間でありますサンプルのIDE。 注：パーカーモデル15は、断熱サンプルと瞬時パルス加熱の理想的な条件を想定し、他のモデルには、熱損失、有限パルス持続時間、不均一なパルス加熱及び不均一などの測定における様々な損失を占めている、長年にわたって提案されています構造。我々は、最も先進的な方法の一つであるパルス補正とコーワンモデル16を使用しています。これは、正面から送信された熱エネルギーの量を最大にし、IR検出器によって観測される信号を最大にするために、試料の表面は高度に放射性でなければならないことに留意すべきです。通常、これは、試料表面にグラファイトの薄いコーティングの適用を必要とします。熱拡散率の測定において2％-5％の不確実性は、ディメンションの決意から生じる、存在している。17 <ol start="3"><li>ダイヤモンドを使用してディスクペレットをカット長方形の棒に見て、2×2×10mm 3で、ホール測定のための高温比熱と薄い長方形のピース、8×5×1mm 3のための導電率とゼーベック係数の測定と同様に正方形ディスク、×4 4×1.5ミリメートル3。 </li><li>平坦かつ鏡面研磨正方形片に試料の比熱C pを 、測定し（4×4×1.5 mm 3で）をアルゴン気流下で示差走査熱量測定（DSC）を用いて、 図18 <ol><li>正確な冷却速度で、試料を500℃に20 K分-1の加熱速度アップに続いて熱平衡に到達させるために10分間等温保持を40℃で5分間K -1までの加熱速度を使用してこれは続きます。 （50ミリリットル分-1示唆されている）をアルゴンの流れの下で測定を行います。 </li></ol></li></ol>注：原因分析のために使用される方法の感度に、熱容量を決定するために、3回の測定を行います<html>既知C Pに（例えば、サファイアのような）標準物質の比熱の（2）の測定、及び試料の比熱の（3）の測定、（1）ベースライン測定は、バックグラウンドを減算することを含みます。サンプルは、測定るつぼ（この作業で使用したAl 2 O 3るつぼでのPt / Rhのパン）の底部との理想的な接触をするために平坦かつ鏡面研磨されていることを確認してください。サンプルを測定するためのDSCステージの正確な構造、他の人にDSC技術の比較、および正確な指示についての詳細は、様々なソースで見つけることができます。19 <ol start="5"><li> 20を 使用してρ、熱拡散率、D、比熱、C P、および密度の測定値からのサンプルの高温の熱伝導率κを計算します</li></ol>/52869/52869eq4.JPG &quot;幅=&quot; 200 &quot;/&gt; <ol start="6"><li>ゴールドプレートサンプルから切断し、2×2×10 mm 3でピース上のプローブの接触点（4接点）は、接触抵抗の問題を緩和します。 <ol><li>唯一の所望の接触領域に金をスパッタするためには、ステンシルとして使用するには、2×2×10ミリメートル3サンプルの周りにスコッチテープを包みます。 2面の非覆われた2×2ミリメートルのままにしておきます。カミソリの刃を使用して、プローブの距離によって分離された線に沿って2×10ミリメートル2面の中央に2非常に小さな穴（直径約1mm）を切り出します。 </li><li>ベンチトップ金スパッタ装置を用い〜200nmの厚さの金膜をスパッタ。21 </li></ol></li><li>温度22,23の関数として試料の電気輸送特性、すなわち電気伝導度とゼーベック係数）を測定します。 <ol><li>四端子法を用いて電気伝導度を測定します。 SAMのゼーベック係数を測定します中央の2つの熱電対、「プローブ」を介して、温度および電圧の測定値を使用して電子のセットアップ。デジタルマイクロスコープを使用して、これら2つのプローブ間の距離を測定します。電気輸送測定の詳細については、他の場所で見つけることができます。22,23 </li></ol></li><li>物性測定システムを使用して、8×5×1mm 3の試料の温度の関数としてのホールキャリア濃度を測定します。24 </li></ol>

<ol>
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M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Thermal Conductivity: Theory, Properties and Applications. , (2004).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> SC7610 Sputter Coater Operating Manual. , (2002).</li><li>Tritt, T. M., Rowe, D. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrical+and+Thermal+Transport+Measurement+Techniques+for+Evaluation+of+the+figure-of-Merit+of+Bulk+Thermoelectric+Materials.">Electrical and Thermal Transport Measurement Techniques for Evaluation of the figure-of-Merit of Bulk Thermoelectric Materials.</a> Thermoelectrics Handbook: Macro to Nano. , 23-1-23-17 (2006).</li><li>Burkov, A. T., Rowe, D. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Measurements+of+Resistivity+and+Thermopower:+Principles+and+Practical+Realization.">Measurements of Resistivity and Thermopower: Principles and Practical Realization.</a> Thermoelectrics Handbook: Macro to Nano. , 22-1 (2006).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Physical Property Measurement System: AC Transport Option User&#8217;s Manual. , (2003).</li><li>Ohta, S., Ohta, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Grain+Size+Dependence+of+Thermoelectric+Performance+of+Nb-doped+SrTiO3.">Grain Size Dependence of Thermoelectric Performance of Nb-doped SrTiO3.</a> Polycrystals. J. Ceram. Soc. Jpn. 114, 102 (2006).</li><li>Wang, N., He, H., Ba, Y., Wan, C., Koumoto, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermoelectric+Properties+of+Nb-doped+SrTiO3+Ceramics+Enhanced+by+Potassium+Titanate+Nanowires+Addition.">Thermoelectric Properties of Nb-doped SrTiO3 Ceramics Enhanced by Potassium Titanate Nanowires Addition.</a> J. Ceram. Soc. Jpn. 118, 1098 (2010).</li><li>Ohta, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Large+Thermoelectric+Performance+of+Heavily+Nb-doped+SrTiO3+Epitaxial+Film+at+High+Temperature.">Large Thermoelectric Performance of Heavily Nb-doped SrTiO3 Epitaxial Film at High Temperature.</a> Appl. Phys. Lett. 87, 092108 (2005).</li><li>Kovalevsky, A., Yaremchenko, A., Populoh, S., Weidenkaff, A., Frade, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Enhancement+of+Thermoelectric+Performance+in+Strontium+Titanate+by+Praseodymium+Substitution.">Enhancement of Thermoelectric Performance in Strontium Titanate by Praseodymium Substitution.</a> J. Appl. Phys. 113, 053704 (2013).</li><li>Kovalevsky, A. V., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Towards+a+High+Thermoelectric+Performance+in+Rare-Earth+Substituted+SrTiO3:+Effects+Provided+by+Strongly-Reducing+Sintering+Conditions.">Towards a High Thermoelectric Performance in Rare-Earth Substituted SrTiO3: Effects Provided by Strongly-Reducing Sintering Conditions.</a> Phys. Chem. 16, 26946 (2014).</li><li>Dawson, J. A., Tanaka, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Local+Structure+and+Energetics+of+Pr-+and+La-Doped+SrTiO3+Grain+Boundaries+and+the+Influence+on+Core–Shell+Structure+Formation.">Local Structure and Energetics of Pr- and La-Doped SrTiO3 Grain Boundaries and the Influence on Core–Shell Structure Formation.</a> J. Phys. Chem. C. 118, 25765-25778 (2014).</li><li>Mehdizadeh Dehkordi, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=New+Insights+on+the+Synthesis+and+Electronic+Transport+in+Bulk+Polycrystalline+Pr-doped+SrTiO3&#8722;&#948;.">New Insights on the Synthesis and Electronic Transport in Bulk Polycrystalline Pr-doped SrTiO3&#8722;&#948;.</a> Appl. Phys. Lett. 117, 055102 (2015).</li></ol>

The authors have nothing to disclose.

このプロトコルでは、改善された成功した電子と熱電特性を示すバルク多結晶のPrドープのSrTiO 3セラミックスを作製するために、合成戦略のステップを提示しています。プロトコルの主なステップは、（i）大気圧下での空気中のドープされたSrTiO 3粉末の固体合成及び（ii）高へのように調製した粉末を緻密化するために、放電プラズマ焼結技術の能力を活用することが含ま?...

酸化物熱電は、電子輸送特性に対する安定性、コストの観点から、高温の熱電アプリケーション向けの有望な候補であることが示されました。 n型酸化物熱電の中で、高度にドープされたチタン酸ストロンチウム（STO）は、その興味深い電子的性質に多くの注目を集めています。しかし、大規模な総熱伝導率（κ〜12 W M -1 K -1 300単結晶のKで）1と低キャリア移動度（μ〜6センチメートル2 V -1秒-1単結晶の300 Kで） 1有害T、電気伝導度σ、ケルビンでの絶対温度を無次元性能指数によって評価される熱電性能、αはゼーベック係数でZT =α2σT/κを、影響し、総熱伝導率をκ。我々は、本明細書の力率などの分子を定義し、PF =α263; T。 （例えば、のSiGe合金など）、他の高温熱電と競合するこの酸化物熱電材料のためには、力率、および/または、格子熱伝導度の低下がより顕著な増加が必要です。 STOの熱電特性を向上させるために実験的研究の大部分は、主に歪み場とフォノンの質量変動散乱を介して熱伝導率の低減に焦点を当てています。これらの試みは、（i）単一またはSrののダブルドーピング2+及び/又はTi 4+サイトを、この方向に対する主な取り組みとして、自然超格子Ruddlesden·ポッパー構造の2,3（ii）の合成さらに、ナノサイズの第二相を添加することによって、絶縁層を介して4のSrO、および（iii）複合エンジニアリング熱伝導率を低減するために5しかし、最近まで、全く強化戦略がsubstantすることが報告されていませんiallyこれらの酸化物熱電力率を増加させます。バルク単及び多結晶STOで報告された最大の力率（PF）の値は、PF &lt;1.0 WのM -1 K -1の上限に限定されています。 合成手法及び処理技術の様々な試みは、上記のアイデアを実現するために使用されてきました。粉末の合成経路は、従来の固相反応を含み、6ゾル-ゲル、7従来の焼結に対し水、8燃焼合成、9、6ホットプレス10と最近放電プラズマ焼結12内に粉末を緻密化するために使用される一般的な技術の一つでありますバルクセラミックス。しかし、同様のドーパント（ 例えば、ラ）とドーピング濃度を、得られたバルクセラミックスは、電子および熱輸送特性の範囲を示します。これは、チタン酸ストロンチウム&lt;強くプロセス依存欠陥化学に大でありますサブ&gt;合成依存特性をもたらす3。熱電輸送を利益のために合成及び処理パラメータを最適化レポートのほんの一握りがあります。それが原因で、非常に小さなフォノンにはSrTiO 3でのフリーパス（300 KにおけるリットルpH約 2 nm）を意味していることを言及する価値がある、11ナノ構造は、主に低減によるバルクSTOセラミックスのTE性能の向上のための実行可能な選択肢ではありません格子熱伝導率の。 最近、我々は、非均一のPrをドープしたSrTiOメリットの熱電図では30％以上の改善を同時に強化熱電力率と減少し、熱伝導率に由来する3セラミックを報告した。この詳細なビデオプロトコルでは12,13、我々が提示し、改良された電子的および熱電特性を示すこれらのPrをドープしたSTOセラミックスの製造のための私たちの合成戦略の手順を説明します。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>SrCO3 Powder, 99.9%</td>
			<td>Sigma Aldrich</td>
			<td>472018</td>
			<td></td>
		</tr>
		<tr>
			<td>TiO2 Nanopowder, 99.5%</td>
			<td>Sigma Aldrich</td>
			<td>718467</td>
			<td></td>
		</tr>
		<tr>
			<td>Pr2O3 Sintered Lumps, 99.9%</td>
			<td>Alfa Aesar</td>
			<td>35663&#160;</td>
			<td></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Name of&#160; Equipment</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Spark Plasma Sintering&#160;</td>
			<td>Dr. Sinter Lab</td>
			<td>SPS-515S</td>
			<td></td>
		</tr>
		<tr>
			<td>Resistivity/Seebeck Coefficient Measurement System</td>
			<td>Ulvac-Riko</td>
			<td>ZEM-2</td>
			<td></td>
		</tr>
		<tr>
			<td>Laser Flash Thermal Diffusivity Measurement System</td>
			<td>Netzsch</td>
			<td>LFA-457 Microflash</td>
			<td></td>
		</tr>
		<tr>
			<td>Differential Scanning Calorimetry (DSC) System</td>
			<td>Netzsch</td>
			<td>404C Pegasus</td>
			<td></td>
		</tr>
		<tr>
			<td>Physical Property Measurement system (PPMS)</td>
			<td>Quantum Design</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Field Emission Scanning Electron Microscope (FE-SEM)</td>
			<td>Hitachi</td>
			<td>SU-6600</td>
			<td></td>
		</tr>
		<tr>
			<td>Energyy-dispersive X-ray Spectroscopy (EDS)</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>X-ray Diffractometer</td>
			<td>Rigaku</td>
			<td>Ultima IV</td>
			<td></td>
		</tr>
		<tr>
			<td>Bench-top Sputter Coater</td>
			<td>Denton Vacuum</td>
			<td>Desk II</td>
			<td></td>
		</tr>
		<tr>
			<td>Diamond&#160; Wheel Saw</td>
			<td>South Bay Technology</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

synthesis of non-uniformly pr-doped srtio3 ceramics and their thermoelectric properties

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma sintering techniques. Polycrystalline ceramics possessing a unique morphology can be achieved by optimizing the process parameters, particularly spark plasma sintering heating rate. The phase and morphology of the synthesized ceramics were investigated in detail using X-ray diffraction, scanning electron microcopy and energy-dispersive X-ray spectroscopy. It was observed that the grains of these bulk Pr-doped SrTiO3 ceramics were enhanced with Pr-rich grain boundaries. Electronic and thermal transport properties were also investigated as a function of temperature and doping concentration. Such a microstructure was found to give rise to improved thermoelectric properties. Specifically, it resulted in a significant improvement in carrier mobility and the thermoelectric power factor. Simultaneously, it also led to a marked reduction in the thermal conductivity. As a result, a significant improvement (> 30%) in the thermoelectric figure of merit was achieved for the whole temperature range over all previously reported maximum values for SrTiO3-based ceramics. This synthesis demonstrates the steps for the preparation of bulk polycrystalline ceramics of non-uniformly Pr-doped SrTiO3.

パターンがたSrTiO 3格子上のPrドープの効果を研究するために調製されたままの粉末及びPr-コンテンツ（ 図1）の関数として対応するバルクセラミックスのために収集したX線回折、チタン酸ストロンチウム中のPrの溶解度3と二次相（複数可）の形成。パターンは反射が空間群（ 図1A）と立方格子にインデックスを付けることができ、すべてのように調?...

Watch this Scientific Journal Video about Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties at JoVE.com

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

A protocol for the synthesis and processing of polycrystalline SrTiO3 ceramics doped non-uniformly with Pr is presented along with the investigation of their thermoelectric properties.

非均一のPrをドープしたチタン酸ストロンチウムの合成<sub&gt; 3</sub&gt;セラミックスとその熱電特性

We demonstrate a novel synthesis strategy for the preparation of Pr-doped SrTiO3 ceramics via a combination of solid state reaction and spark plasma ...

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Chemistry

Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

9.8K ビュー.  Clemson University. A protocol for the synthesis and processing of polycrystalline SrTiO3 ceramics doped non-uniformly with Pr is presented along with the investigation of their thermoelectric properties.

ビデオ: Synthesis of Non-uniformly Pr-doped SrTiO3 Ceramics and Their Thermoelectric Properties

Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. Isonicotinic acid, or its derivatives, are coupled to variable length diaminoalkane chains under an inert atmosphere in anhydrous DMF or DMSO with the use of a weak base, triethylamine, and a coupling agent, 1-propylphosphonic anhydride. The products precipitate from solution upon formation or can be precipitated by the addition of water. If desired, the ligands can be further purified by recrystallization from hot water. Dinuclear platinum complex synthesis using the bispyridine ligands is done in hot water using transplatin. The most informative of the chemical characterization techniques to determine the structure and gross purity of both the bispyridine ligands and the final platinum complexes is 1H NMR with particular analysis of the aromatic region of the spectra (7-9 ppm). The platinum complexes have potential application as anticancer agents and the synthesis method can be modified to produce trinuclear and other multinuclear complexes with different hydrogen bonding functionality in the bridging ligand.

This protocol describes the use of amide coupling reactions of isonicotinic acid and diaminoalkanes to form bridging ligands suitable for use in the synthesis of multinuclear platinum complexes, which combine aspects of the anticancer drugs BBR3464 and picoplatin.

ビスピリジン系リガンドの合成と二核抗癌剤として白金彼らの複合体形成のためのアミドカップリング反応

Amide coupling reactions can be used to synthesize bispyridine-based ligands for use as bridging linkers in multinuclear platinum anticancer drugs. ...

化学

Synthesis and Characterization of Supramolecular Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

超分子コロイドの合成とキャラクタリゼーション

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single molecule level. An electrostatic self-assembly and covalent fixation (ESA-CF) process is used for the synthesis of the cyclic poly(tetrahydrofuran) (poly(THF)). The diffusive motion of individual cyclic polymer chains in a melt state is visualized using single molecule fluorescence imaging by incorporating a fluorophore unit in the cyclic chains. The diffusive motion of the chains is quantitatively characterized by means of a combination of mean-squared displacement (MSD) analysis and a cumulative distribution function (CDF) analysis. The cyclic polymer exhibits multiple-mode diffusion which is distinct from its linear counterpart. The results demonstrate that the diffusional heterogeneity of polymers that is often hidden behind ensemble averaging can be revealed by the efficient synthesis of the cyclic polymers using the ESA-CF process and the quantitative analysis of the diffusive motion at the single molecule level using the MSD and CDF analyses.

A protocol for the synthesis and characterization of diffusive motion of cyclic polymers at the single molecule level is presented.

単一分子レベルでの環状ポリマーの合成と溶融状態におけるそれらの拡散運動のキャラクタリゼーション

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single ...

Synthesis and Characterization of Fe-doped Aluminosilicate Nanotubes with Enhanced Electron Conductive Properties

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe aims at lowering the band gap of imogolite, an insulator with the chemical formula (OH)3Al2O3SiOH, and at modifying its adsorption properties towards azo-dyes, an important class of organic pollutants of both wastewater and groundwater.
Fe-doped nanotubes are obtained in two ways: by direct synthesis, where FeCl3 is added to an aqueous mixture of the Si and Al precursors, and by post-synthesis loading, where preformed nanotubes are put in contact with a FeCl3&#8226;6H2O aqueous solution. In both synthesis methods, isomorphic substitution of Al3+ by Fe3+ occurs, preserving the nanotube structure. Isomorphic substitution is indeed limited to a mass fraction of ~1.0% Fe, since at a higher Fe content (i.e., a mass fraction of 1.4% Fe), Fe2O3 clusters form, especially when the loading procedure is adopted. The physicochemical properties of the materials are studied by means of X-ray powder diffraction (XRD), N2 sorption isotherms at -196 &#176;C, high resolution transmission electron microscopy (HRTEM), diffuse reflectance (DR) UV-Vis spectroscopy, and &#950;-potential measurements. The most relevant result is the possibility to replace Al3+ ions (located on the outer surface of the nanotubes) by post-synthesis loading on preformed imogolite without perturbing the delicate hydrolysis equilibria occurring during nanotube formation. During the loading procedure, an anionic exchange occurs, where Al3+ ions on the outer surface of the nanotubes are replaced by Fe3+ ions. In Fe-doped aluminosilicate nanotubes, isomorphic substitution of Al3+ by Fe3+ is found to affect the band gap of doped imogolite. Nonetheless, Fe3+ sites on the outer surface of nanotubes are able to coordinate organic moieties, like the azo-dye Acid Orange 7, through a ligand-displacement mechanism occurring in an aqueous solution.

Here, we present a protocol to synthesize and characterize Fe-doped aluminosilicate nanotubes. The materials are obtained by either sol-gel synthesis upon addition of FeCl3&#8226;6H2O to the mixture containing the Si and Al precursors or by post-synthesis ionic exchange of preformed aluminosilicate nanotubes.

強化された電子導電特性を持つFeドープアルミノシリケートナノチューブの合成とキャラクタリゼーション

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe ...

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be covalently and site-specifically linked via their end facets, resulting in polymer-like linear or branched chains. The linking procedure begins with a cation-exchange process in which the end facets of the cadmium chalcogenide NCs are first converted to silver chalcogenide. This is followed by the selective removal of ligands at their surface. This results in cadmium chalcogenide NCs with highly reactive silver chalcogenide end facets that spontaneously fuse upon contact with each other, thereby establishing an interparticle facet-to-facet attachment. Through the judicious choice of precursor concentrations, an extensive network of linked NCs can be produced. Structural characterization of the linked NCs is carried out via low- and high-resolution transmission electron microscopy (TEM), as well as energy-dispersive X-ray spectroscopy, which confirm the presence of silver chalcogenide domains between chains of cadmium chalcogenide NCs.

A protocol detailing how shape-anisotropic colloidal cadmium chalcogenide nanocrystals can be covalently linked via their end facets is presented here.

ファセットとファセットの形状異方性のコロイド カドミウム カルコゲナイド系ナノ構造のリンク

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

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 ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a challenge, as it requires asymmetric growth of symmetric crystals. Here, we report a distinctive synthesis of substrate-bound Au nanowires. This template-free synthesis employs thiolated ligands and substrate adsorption to achieve the continuous asymmetric deposition of Au in solution at ambient conditions. The thiolated ligand prevented the Au deposition on the exposed surface of the seeds, so the Au deposition only occurs at the interface between the Au seeds and the substrate. The side of the newly deposited Au nanowires is immediately covered with the thiolated ligand, while the bottom facing the substrate remains ligand-free and active for the next round of Au deposition. We further demonstrate that this Au nanowire growth can be induced on various substrates, and different thiolated ligands can be used to regulate the surface chemistry of the nanowires. The diameter of the nanowires can also be controlled with mixed ligands, in which another &#34;bad&#34; ligand could turn on the lateral growth. With the understanding of the mechanism, Au nanowire-based nanostructures can be designed and synthesized.

We report a solution-based method to synthesize substrate-bound Au nanowires. By tuning the molecular ligands used during the synthesis, the Au nanowires can be grown from various substrates with different surface properties. Au nanowire-based nanostructures can also be synthesized by adjusting the reaction parameters.

アクティブな表面の成長メカニズムを介して基質結合 Au ナノワイヤの作製

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

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 ...

Synthesis of In37P20(O2CR)51 Clusters and Their Conversion to InP Quantum Dots

This text presents a method for the synthesis of In37P20(O2C14H27)51 clusters and their conversion to indium phosphide quantum dots. The In37P20(O2CR)51 clusters have been observed as intermediates in the synthesis of InP quantum dots from molecular precursors (In(O2CR)3, HO2CR, and P(SiMe3)3) and may be isolated as a pure reagent for subsequent study and use as a single-source precursor. These clusters readily convert to crystalline and relatively monodisperse samples of quasi-spherical InP quantum dots when subjected to thermolysis conditions in the absence of additional precursors above 200 &#176;C. The optical properties, morphology, and structure of both the clusters and quantum dots are confirmed using UV-Vis spectroscopy, photoluminescence spectroscopy, transmission electron microscopy, and powder X-ray diffraction. The molecular symmetry of the clusters is additionally confirmed by solution-phase 31P NMR spectroscopy. This protocol demonstrates the preparation and isolation of atomically-precise InP clusters, and their reliable and scalable conversion to InP QDs.

Synthesis of In37P20O2CR51 Clusters and Their Conversion to InP Quantum Dots

A protocol for the synthesis of In37P20(O2C14H27)51 clusters and their conversion to indium phosphide quantum dots is presented.

37P20(o2 CR)51クラスターの合成と InP 量子ドットへの変換

This text presents a method for the synthesis of In37P20(O2C14H27)51 clusters and their conversion to indium phosphide quantum dots. The In37P20(O2CR)51 ...

Design, Synthesis, and Photochemical Properties of Clickable Caged Compounds

Caged compounds enable the photo-mediated manipulation of the cell physiology with high spatiotemporal resolution. However, the limited structural diversity of currently available caging groups and the difficulties in synthetic modification without sacrificing their photolysis efficiencies are obstacles to expanding the repertoire of caged compounds for live cell applications. As the chemical modification of coumarin-type photo-caging groups is a promising approach for the preparation of caged compounds with diverse physical and chemical properties, we report a method for the synthesis of clickable caged compounds that can be modified easily with various functional units via the copper(I)-catalyzed Huisgen cyclization. The modular platform molecule contains a (6-bromo-7-hydroxycoumarin-4-yl)methyl (Bhc) group as a photo-caging group, which exhibits a high photolysis efficiency compared to those of the conventional 2-nitrobenzyls. General procedures for the preparation of clickable caged compounds containing amines, alcohols, and carboxylates are presented. Additional properties such as the water solubility and cell targeting ability can be readily incorporated into clickable caged compounds. Furthermore, the physical and photochemical properties, including the photolysis quantum yield, were measured and were found to be superior to those of the corresponding Bhc caged compounds. The described protocol could therefore be considered a potential solution for the lack of structural diversity in the available caged compounds.

A protocol for the synthesis and measurement of the photochemical properties of modular caged compounds with clickable moieties is presented.

Methods Article

非均一のPrをドープしたチタン酸ストロンチウムの合成