この研究を行ったで、太平洋の北西国立研究所 (なり)、ため、エネルギー省 (DOE) 契約番号の下でバテル記念研究所が運営します。デ-AC05-76RL01830。

ここで示した実験では、無臭、無色、およびこうして人間の感覚によって検出不可能である水素ガスの使用が必要です。水素は引火、やけどほぼ目に見えない青炎しフォームをすることができます酸素の存在下で爆発性混合物。6.9 MPa を超える高圧は、任意のテストに備えて追加爆発の危険を適切に計画する必要がありますを追加します。この蓄えられたエネルギー量は深刻な安全上の問題を表し、したがって適正評価、計画、および安全性に、評価をこれらの危険を軽減することを確認するこのような実験を実行する前に実行する必要があります。ここで示した実験は、34.5 MPa に設定され、適切な換気、バースト ディスクとアメリカ機械学会 (ASME) 認定加圧適切な安全上の注意に従って実行されます。
1. ポリマー シート素材の準備
<ol><li>非研磨スポンジを使用して EDPM ポリマー シート素材に洗剤を適用し、オイルを削除し、タルクの粉末製造と出荷プロセス中に適用される約 3 分のための水の下ですすいでください。</li>
	<li>洗濯の残り水のドライブに約 72 時間、マテリアルの作業温度、EPDM、約 75 ° C の 85% で乾燥炉内のポリマー シートを乾燥させます。</li>
	<li>オーブンの電源を切り、オーブン中室温に冷却する高分子シート ストック材料を許可します。</li>
	<li>ポリマー シートの上部を指している矢印の付いたシート素材の一角をマークします。この矢印はポリマー シートからカットのサンプルがあること一貫して同じ方向を確保するサンプル クーポン生成中にシートの向きを識別するのに役立ちます。</li>
	<li>部屋の温度でポリマー ストック シート、トライボロジー試験前に相対湿度が 25% 近くの湿度制御環境を格納します。</li>
</ol>2 を生成し、サンプル クーポンをマウント
<ol><li>粉を着て手袋を無料、対象クーポン、双方向の矢印がある同じ方向にポリマー シート素材の準備中にマークの矢印付近に矢のポリマー シート素材をマークします。</li>
	<li>2.222 cm 直径の円形死ぬと木槌を使って、矢印マークの周りのサンプル クーポンを根絶します。</li>
	<li>トライボメータその場で、六角のキャップ スクリューと精密試料留め具の一番アクセスし易いコーナーから春削除サンプル クランプを固定する六角キャップ ネジを緩めます。</li>
	<li>試料留め具、サンプルを確認する世話にスライド サンプル クーポンは方向の矢印が上下、トライボメータのバック プレートに近い側であるクランプの背面に向かって顔を指摘しました。</li>
	<li>精密スプリングとサンプルの空の隅に六角のキャップ スクリューをクランプし手に進むは、エラストマー サンプルは元の高さの 10% で圧縮するようフィットするまでクランプの hex キャップネジのすべての 4 つを締めます。0.318 cm サンプル高さを想定して、クランプの 2 つのプレート間 0.287 cm ゲージ ブロックを使用して、10% の圧縮を実現できます。</li>
</ol>3. 準備その場でトライボメータ
<ol><li>場所 2.413 cm ゲージ、トライボメータの壁とドライブのネジのすぐ下のサンプルそりブロックです。データ コレクション ボックスがオフし、時計回りに動き、そりのエッジがトライボメータ壁から 2.413 cm サンプルそりをバックアップするドライブ チェーンを有効にしていることを確認します。</li>
	<li>反対の表面の表面の任意の破片が無料表示されるまで約 30 秒間柔らかい布または糸くずのない紙タオル、アセトンなどの適当な溶剤で表面をカウンターの鋼球を軽く拭きます。</li>
	<li>ブロンズ カウンター表面キャリアとブロンズ重量、カウンター ボールの鍵穴に挿入し、ポリマー サンプルの残りの部分をできるようにサンプルそりに垂直のレール上に 7.5 N の合計荷重スライドさせます。</li>
	<li>自由に浮遊、LVDT シリンダーが腕にかかっていることなど、ブロンズ カウンター表面ホルダーにリニア可変差動トランス (LVDT) 測定アーム六角キーと 2 つの銅ネジを使用して、接続し直します。</li>
	<li>場所の LVDT を保持するクランプを調整したり、ダウンそれの近く、LVDT を測定するようなゼロ点、クランプを締める場所に LVDT をセキュリティで保護します。</li>
	<li>確保、トライボメータと容器の壁との間のギャップに、容器の上部のフランジに管が下がる圧力容器にトライボメータ アセンブリを下げます。</li>
	<li>ラップ シール o リング PTFE テープの 2 つ半層の合計。これは、各ラップと重なる約半分進むラップの o リングの直径を 2 回はやってまで PTFE テープでラップで。O リングの径をラップ重なることがなく最終的な時間。O リングをラップすると、一度は、圧力容器のリップの溝に配置します。</li>
	<li>考慮して配線ラベルは、トライボメータ モーターの 5 電源線、負荷セルの 4 つのデータ線と、LVDT の 5 つのデータ ケーブルを接続し直します。</li>
</ol>4. 圧力容器のシール
<ol><li>下を閉じ、PTFE にそっと上部フランジを下に注意しながら圧力容器上部フランジは o リングをシールをラップしました。</li>
	<li>彼らがタイトな指まで昇順でメーカーが示す上部フランジの番号の穴にボルトを挿入します。</li>
	<li>手動六角キーを使用すると、手にタイトな昇順のフランジ ボルトをトルクし、ボルトを強化されなくことができますまで繰り返します。</li>
	<li>最低 120 Nm と 〜 40 Nm ずつ増えていく昇順 〜 40 Nm 増分の彼らがカンカンまで 280 ボルト、トルクをトルクレンチを使用して Nm。</li>
</ol>5. 圧力容器の充填
<ol><li>今では圧力容器が密閉されているガス器具をオートクレーブ蓋に接続し、容器の酸素に配管酸素センサーを用いた 10 ppm を下回るまで約 1 h のアルゴンのガスを低圧 (~0.55 MPa) と圧力容器をフラッシュ圧力容器の出力。</li>
	<li>ゆっくりと (< 0.25 MPa ・ s) 6.9 MPa まで水素ガスの容器をフラッシュし、ゆっくりと大気圧ガスを発散します。フラッシュ プロセスをさらに 2 回繰り返します。</li>
	<li>ゆっくりと圧力容器をフラッシュした後 (< 0.25 MPa ・ s) 水素ガス 13.75 MPa までの圧力容器を記入し、容器内のガスの温度は部屋の温度にあるように 10 分の残りの部分に容器を許可します。</li>
	<li>20.7 mpa 容器記入し、別の 10 分を待ちます。</li>
	<li>ターゲット 27.6 まで容器をもたらす MPa と閉じるすべてのバルブをオフします。</li>
	<li>完全な浸透を可能にするのに実験を開始する前に、水素ガスで少なくとも 12 時間浸漬する高分子サンプルを許可します。</li>
</ol>6. 実験の実行
<ol><li>圧力容器を終了するすべてのパススルー ワイヤ トライボメータ コントロール ボックスに関連付けられたラベル付き配線ハーネスに正しく接続されていると、トライボメータ入れますダブル チェック。</li>
	<li>トライボメータでは、ソフトウェアは、実験時間を 0.140 cm のパスの長さを 0.1 cm/s の速度で 1 時間に設定します。これは約 3.5 m の距離に対応します。</li>
	<li>風袋、ロードセル、LVDT が 0 mm に近いことトライボメータ ソフトウェアの適切な深さを報告していることを確認.</li>
	<li>実験を開始します。</li>
</ol>7. 後の実験
<ol><li>約 0.35 MPa/s、圧力容器の温度は 0 ° C 下で落ちないことを確認で水素ガスの圧力容器をゆっくりと発散実験が完了すると、</li>
	<li>最後に、容器内の残りの水素がないことを確認する 10 分間大気圧アルゴン ガス圧力容器ボリュームをフラッシュします。</li>
</ol>

<ol>
	<li>Schlapbach, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Technology:+Hydrogen-fuelled+vehicles.">Technology: Hydrogen-fuelled vehicles.</a> Nature. 460 (7257), 809-811 (2009).</li><li>Jones, R., Thomas, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Materials for the Hydrogen Economy. , (2007).</li><li>Barth, R., Simons, K. L., San Marchi, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Polymers for Hydrogen Infrastructure and Vehicle Fuel Systems: Applications, Properties, and Gap Analysis. , 23-34 (2013).</li><li>Marchi, C., Somerday, B. P., Ref, M. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Technical Reference on Hydrogen Compatibility of Materials. , (2008).</li><li>Welch, 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=.">.</a> Challenges in developing hydrogen direct injection technology for internal combustion engines. , (2008).</li><li>Fukai, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> The Metal-Hydrogen System. , (2005).</li><li>Lu, G., Kaxiras, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrogen+embrittlement+of+aluminum:+The+crucial+role+of+vacancies.">Hydrogen embrittlement of aluminum: The crucial role of vacancies.</a> Phys. Rev. Lett. 94 (15), 155501 (2005).</li><li>Zhao, Z., Carpenter, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Annealing+enhanced+hydrogen+absorption+in+nanocrystalline+Pd&#8725;AuPd&#8725;Au+sensing+films.">Annealing enhanced hydrogen absorption in nanocrystalline Pd&#8725;AuPd&#8725;Au sensing films.</a> J. Appl. Phys. 97 (12), 124301 (2005).</li><li>Alvine, K. J., 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=High-pressure+hydrogen+materials+compatibility+of+piezoelectric+films.">High-pressure hydrogen materials compatibility of piezoelectric films.</a> Appl. Phys. Lett. 97 (22), 221911 (2010).</li><li>Alvine, K. J., 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=Hydrogen+species+motion+in+piezoelectrics:+A+quasi-elastic+neutron+scattering+study.">Hydrogen species motion in piezoelectrics: A quasi-elastic neutron scattering study.</a> J. Appl. Phys. 111 (5), 53505 (2012).</li><li>Aggarwal, 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=Effect+of+hydrogen+on+Pb(Zr,Ti)O3Pb(Zr,Ti)O3-based+ferroelectric+capacitors.">Effect of hydrogen on Pb(Zr,Ti)O3Pb(Zr,Ti)O3-based ferroelectric capacitors.</a> Appl. Phys. Lett. 73 (14), (1998).</li><li>Ikarashi, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Analytical+transmission+electron+microscopy+of+hydrogen-induced+degradation+in+ferroelectric+Pb(Zr,+Ti)O3Pb(Zr,+Ti)O3+on+a+Pt+electrod.">Analytical transmission electron microscopy of hydrogen-induced degradation in ferroelectric Pb(Zr, Ti)O3Pb(Zr, Ti)O3 on a Pt electrod.</a> Appl. Phys. Lett. 73 (14), (1998).</li><li>Castagnet, S., Grandidier, J., Comyn, M., Beno&#305;, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrogen+influence+on+the+tensile+properties+of+mono+and+multi-layer+polymers+for+gas+distribution.">Hydrogen influence on the tensile properties of mono and multi-layer polymers for gas distribution.</a> Int. J. Hydrog. Energy. 35, 7633-7640 (2010).</li><li>Theiler, G., Gradt, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tribological+characteristics+of+polyimide+composites+in+Hydrogen+environment.">Tribological characteristics of polyimide composites in Hydrogen environment.</a> Tribol. Int. 92, 162-171 (2015).</li><li>Sawae, Y., 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=Friction+and+wear+of+bronze+filled+PTFE+and+graphite+filled+PTFE+in+40+MPA+hydrogen+gas.">Friction and wear of bronze filled PTFE and graphite filled PTFE in 40 MPA hydrogen gas.</a> Proceed. , 249-251 (2011).</li><li>Fujiwara, H., Ono, H., Nishimura, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Degradation+behavior+of+acrylonitrile+butadiene+rubber+after+cyclic+high-pressure+hydrogen+exposure.">Degradation behavior of acrylonitrile butadiene rubber after cyclic high-pressure hydrogen exposure.</a> Int. J. Hydrogen Energy. 40 (4), 2025-2034 (2015).</li><li>Zhang, L., 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=Influence+of+low+temperature+prestrain+on+hydrogen+gas+embrittlement+of+metastable+austenitic+stainless+steels.">Influence of low temperature prestrain on hydrogen gas embrittlement of metastable austenitic stainless steels.</a> Int. J. Hydrogen Energy. 38 (25), 11181-11187 (2013).</li><li>Weber, S., Theisen, W., Mart&#305;, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+a+stable+high-aluminum+austenitic+stainless+steel+for+hydrogen+applications.">Development of a stable high-aluminum austenitic stainless steel for hydrogen applications.</a> Int. J. Hydrogen Energy. 38 (14), 5989-6001 (2013).</li><li>Papavinasam, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Corrosion control in the oil and gas industry. , (2013).</li><li>Yamamoto, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrogen+Embrittlement+of+Nuclear+Power+Plant+Materials.">Hydrogen Embrittlement of Nuclear Power Plant Materials.</a> Mat. Trans. 45 (8), 2647-2649 (2004).</li><li>Rymuza, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tribology+of+polymers.">Tribology of polymers.</a> Arch. Civ. Mech. Eng. 7 (4), 177-184 (2007).</li><li>Mckeen, L. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> 1 Introduction to Fatigue and Tribology of Plastics and Elastomers. , (2010).</li><li>Lorge, O., Briscoe, B. J., Dang, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gas+induced+damage+in+poly(vinylidene+fluoride)+exposed+to+decompression.">Gas induced damage in poly(vinylidene fluoride) exposed to decompression.</a> Polymer. 40, 2981-2991 (1999).</li><li>Sawae, Y., Yamaguchi, A., Nakashima, K., Murakami, T., Sugimura, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effects+of+Hydrogen+Atmosphere+on+Wear+Behavior+of+PTFE+Sliding+Against+Austenitic+Stainless+Steel.">Effects of Hydrogen Atmosphere on Wear Behavior of PTFE Sliding Against Austenitic Stainless Steel.</a> Proceed. , 1-3 (2008).</li><li>Sawae, Y., Nakashima, K., Doi, S., Murakami, T., Sugimura, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effects+of+high+pressure+hydrogen+on+wear+of+PTFE+and+PTFE+composite.">Effects of high pressure hydrogen on wear of PTFE and PTFE composite.</a> Proceed. , 233-235 (2010).</li><li>Duranty, E., 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=An+in+situ+tribometer+for+measuring+friction+and+wear+of+polymers+in+a+high+pressure+hydrogen+environment.">An in situ tribometer for measuring friction and wear of polymers in a high pressure hydrogen environment.</a> Rev. Sci. Instrum. 88 (9), (2017).</li></ol>

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高分子材料のトライボロジー試験のため現在元場テクニックには、される前に減圧される高圧水素にさらされるサンプルが必要商業トライボメータを使用してテストします。15,24,25このプロトコルのテスト方法は、高圧環境でその場でポリマー サンプルのトライボロジー特性のテストを許可するように設計さ...

近年、可能性ゼロ排出ガスとして水素の大きな関心や車、定置型電源のゼロに近い排出量の燃料をされています。室温で低密度のガスとして水素が存在するので、ほとんどのアプリケーションは燃料の圧縮水素のいくつかのフォームを使用します。1,2の圧縮を使用して潜在的な欠点は、高圧水素ガスは、インフラストラクチャ2,3,4と車載5内で見つかった多くの材料との互換性、互換性の問題が繰り返される圧力および温度と組み合わせてサイクリングします。純粋な水素環境は特定の鋼を含む金属の部品が損傷、腫れ、水素化物の形成を含むさまざまなメカニズムを通じてチタン表面とふくれ、脆化。2,6,7,ジルコン酸チタン酸鉛 (PZT) 圧電セラミックスの使用など8非金属部品も鉛の移行と表面ふくれなど水素非互換性効果による劣化を受けやすい証明しました。9,10,11,12水素照射による損傷のこれらの例は既に研究されている中、水素環境内の高分子のコンポーネントとの互換性が関心になるばかり。13,14,15,16主成分ポリマーは通常の障壁またはシールとして、核の構造の整合性とオイルとガスのアプリケーションを提供する金属のコンポーネントの結果です。17,18,19,20その結果、ポリテトラフルオロ エチレン (PTFE) などのコンポーネント内で高分子材料の摩擦・摩耗特性シートとバルブ トリル ブタジエンのゴム (NBR) O リングになる重要な要因で機能する能力で。
水素インフラの場合は、貯蔵タンク、コンプレッサー、バルブなどのコンポーネントは、金属表面と接触している高分子材料を含まれています。高分子と金属表面間の摩擦の相互作用は、各表面の摩耗の結果します。摩擦と相互作用する 2 つの表面の摩耗の関係の科学はトライボロジーと呼ばれます。低弾性率と金属よりも強度を持っている傾向があるポリマー、高分子材料のトライボロジー特性は金属材料から大きく異なるため。その結果、高分子表面は、金属表面との摩擦接触後以上の摩耗や損傷を展示する傾向があります。21,22水素インフラストラクチャ アプリケーション、高速圧力と温度サイクルが高分子と金属表面の相互作用の繰り返しの原因は、摩擦の可能性が高まるとポリマー成分に着用します。元場非トライボ損傷を引き起こす可能性があります減圧後ポリマー サンプルの可能な爆発性減圧のためこの損傷の定量化は難しい。23また、多くのポリマー製品含める多くのフィラーと水素化、元場これらの摩耗の解析をさらに複雑な中に水素ガスとの対話を通じて否定的マグネシウム酸化物 (MgO) などの添加物材料。24,25
減圧元場摩擦摩耗による損傷発生高分子材料への損傷間の差別化の複雑さのため直接非金属材料原の摩擦特性を調査する必要があります。水素配信インフラストラクチャ内に存在する可能性のある高圧水素環境で。このプロトコルでは、テストを示す摩擦を定量化し、専用の in situトライボメータを利用した高圧水素雰囲気下における高分子材料の性質を着用する方法論を開発しました。26本代表のデータ取得の in situトライボメータとエチレン プロピレンのジエンの単量体 (EPDM) ゴム、一般的なポリマー シールおよびバリア材を使用します。EPDM 素材 0.3175 cm 厚さで 60.96 cm 正方形シートで購入したデータは、以下のプロトコルを使用して生成された代表と 60A 硬さの評価を持っているベンダーによって報告されました。

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			<td height="79" style="height:79px;width:201px;">EPDM Polymer Stock Sheet</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">8525T68</td>
			<td style="width:156px;">24&#34; x 24&#34;, 1/8&#34; Thick</td>
		</tr>
		<tr height="49">
			<td height="49" style="height:49px;width:201px;">Pressure Vessel, Autoclave</td>
			<td style="width:123px;">Fluitron Inc.</td>
			<td style="width:117px;">8308-1788-U</td>
			<td style="width:156px;">5&#34; diameter, 1&#39; height</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:201px;">High Purity Hydrogen Gas</td>
			<td style="width:123px;">Praxair</td>
			<td style="width:117px;">HY4.5</td>
			<td style="width:156px;">Grade 4.5, 5ppm O2, 5 ppm H20</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:201px;">O2 Sensor</td>
			<td style="width:123px;">Advanced Micro Instruments</td>
			<td style="width:117px;">T2</td>
			<td style="width:156px;">0-5ppm min. range, 10,0000ppm max.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:201px;">Pre-purified Argon Gas</td>
			<td style="width:123px;">Oxarc</td>
			<td style="width:117px;">LCCO-HP818</td>
			<td style="width:156px;">High-purity, 99.998%</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Liquid Dishwashing Detergent</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">98365T89</td>
			<td style="width:156px;">32 oz pour bottle, lemon scented</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Mildew Resistant Sponge</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">7309T1</td>
			<td style="width:156px;">6&#34; long x 3 -1/2&#34; Wide x 1&#34; High, yellow</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">PTFE Pipe Thread Sealant Tape</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">4591K12</td>
			<td style="width:156px;">1/2&#34; wide, white color</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:201px;">Gas Tube Fittings</td>
			<td style="width:123px;">Swagelok</td>
			<td style="width:117px;">SS-400-1-4</td>
			<td style="width:156px;">1/4&#34; OD, stainless steel, male NPT threading</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Hammer Driven Die</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">3427A22</td>
			<td style="width:156px;">7/8&#34; Hammer driven hole punch</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Linear Variable Differential Transformer</td>
			<td style="width:123px;">Omega</td>
			<td style="width:117px;">LD320-2.5&#160;</td>
			<td style="width:156px;">2.5mm, AC output, guided w/spring</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">Autoclave O-ring Seal</td>
			<td style="width:123px;">Fluitron Inc.</td>
			<td style="width:117px;">A-4511</td>
			<td style="width:156px;">Hastelloy C-276, 5-3/4&#34; OD x 5&#34; ID x 3/8&#34;</td>
		</tr>
		<tr height="105">
			<td height="105" style="height:105px;width:201px;">Torque Wrench</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">85555A422</td>
			<td style="width:156px;">Adjustable Torque-Limiting Wrench, Quick-Release, 1/2&#34; Square Drive, 50-250 ft.-lbs. Torque</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:201px;">Mallet</td>
			<td style="width:123px;">McMaster-Carr</td>
			<td style="width:117px;">5939A11</td>
			<td style="width:156px;">Hard and Extra-Hard Rubber Hammer, 2-1/4 lbs.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:201px;">iLoad Mini Capacitive Load Sensor</td>
			<td style="width:123px;">Loadstar Sensors</td>
			<td style="width:117px;">MFM-050-050-S*C03</td>
			<td style="width:156px;">50 lb, U Calibration, 0.5% Accuracy, Steel</td>
		</tr>
	</tbody>
</table>

in situ high pressure hydrogen tribological testing of common polymer materials used in the hydrogen delivery infrastructure

高圧水素ガスは、コンプレッサー、バルブ、ホース、およびアクチュエータの金属部品に悪影響を与える知られています。しかし、比較的少しはまたこれらのコンポーネント内で見つかったポリマー シールとバリア材料の高圧水素の影響について知られています。多くの研究は、高圧水素と水素燃料の輸送インフラのコンポーネントは、一般的なポリマー材料の互換性を判断するために必要です。その結果、摩擦などの物理特性の変化を考慮し、ポリマーは、高圧水素にさらされている間その場で着用することが重要です。このプロトコルで摩擦試験方法とカスタムその場でピンのフラット直線往復を使用して 28 MPa 高圧水素環境におけるエチレン プロピレン ジエンの単量体 (EPDM) エラストマー試料の性質を着用トライボメータ。この試験は代表的な結果表示これは EPDM サンプル クーポンと鋼の反対の表面との間の摩擦係数が高圧水素で同様に測定した摩擦係数と比較すると増加することを示す周囲の空気。

紹介する方法を使用して、高圧水素環境中弾性サンプルの運動摩擦・摩耗率の係数を測定できます。図 1に示す代表的なデータは、高圧水素環境で大きな力が EPDM ポリマー サンプル スチール カウンター表面の下を移動する必要であることを示します。関係を使用して FNと EPDM のサンプル間の摩擦力 FK摩擦係数 μ、強制的に通常?...

Watch this Scientific Journal Video about In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure at JoVE.com

In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

水素インフラ サービスで使用される高分子のトライボロジー特性を定量化するためのテスト方法を示したし、一般的なエラストマーの特徴的な結果について述べる。

その場で高圧水素トライボロジー水素配信インフラストラクチャで使用される一般的なポリマー材料の試験

High pressure hydrogen gas is known to adversely affect metallic components of compressors, valves, hoses, and actuators. However, relatively little is ...

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Research

JoVE Journal

Engineering

In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

7.5K ビュー.  Pacific Northwest National Laboratory. 水素インフラ サービスで使用される高分子のトライボロジー特性を定量化するためのテスト方法を示したし、一般的なエラストマーの特徴的な結果について述べる。

ビデオ: In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

エクストリーム圧力と温度での合成とMicrodiffraction

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

工学

Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and non-destructively reveals the hydrogen density distribution at surfaces, at interfaces, and in the volume of solid materials with high depth resolution. The technique applies a 15N ion beam of 6.385 MeV provided by an electrostatic accelerator and specifically detects the 1H isotope in depths up to about 2 &#956;m from the target surface. Surface H coverages are measured with a sensitivity in the order of ~1013 cm-2 (~1% of a typical atomic monolayer density) and H volume concentrations with a detection limit of ~1018 cm-3 (~100 at. ppm). The near-surface depth resolution is 2-5 nm for surface-normal 15N ion incidence onto the target and can be enhanced to values below 1 nm for very flat targets by adopting a surface-grazing incidence geometry. The method is versatile and readily applied to any high vacuum compatible homogeneous material with a smooth surface (no pores). Electrically conductive targets usually tolerate the ion beam irradiation with negligible degradation. Hydrogen quantitation and correct depth analysis require knowledge of the elementary composition (besides hydrogen) and mass density of the target material. Especially in combination with ultra-high vacuum methods for in-situ target preparation and characterization, 1H(15N,&#945;&#947;)12C NRA is ideally suited for hydrogen analysis at atomically controlled surfaces and nanostructured interfaces. We exemplarily demonstrate here the application of 15N NRA at the MALT Tandem accelerator facility of the University of Tokyo to (1) quantitatively measure the surface coverage and the bulk concentration of hydrogen in the near-surface region of a H2 exposed Pd(110) single crystal, and (2) to determine the depth location and layer density of hydrogen near the interfaces of thin SiO2 films on Si(100).

We illustrate the application of 1H(15N,&#945;&#947;)12C resonant nuclear reaction analysis (NRA) to quantitatively evaluate the density of hydrogen atoms on the surface, in the volume, and at an interfacial layer of solid materials. The near-surface hydrogen depth profiling of a Pd(110) single crystal and of SiO2/Si(100) stacks is described.

核反応分析と深さ方向分析を通じて表面・界面層とバルク材料中の水素濃度の定量

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and ...

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices have used devices prepared by spin coating, a process that is not amenable to large-scale fabrication. This mismatch in device fabrication makes it difficult to translate quantitative results obtained in the laboratory to the commercial level, making optimization difficult. Using a mini-slot die coater, this mismatch can be resolved by translating the commercial process to the laboratory and characterizing the structure formation in the active layer of the device in real time and in situ as films are coated onto a substrate. The evolution of the morphology was characterized under different conditions, allowing us to propose a mechanism by which the structures form and grow. This mini-slot die coater offers a simple, convenient, material efficient route by which the morphology in the active layer can be optimized under industrially relevant conditions. The goal of this protocol is to show experimental details of how a solar cell device is fabricated using a mini-slot die coater and technical details of running in situ structure characterization using the mini-slot die coater.

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Here, we present a protocol to fabricate organic thin film solar cells using a mini-slot die coater and related in-line structure characterizations using synchrotron scattering techniques.

バルクヘテロ接合太陽電池の印刷作製と<em&gt;その場で</em&gt;形態キャラクタリゼーション

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices ...

Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with one twist grain boundary. This apparatus utilizes high uniaxial pressure and a pulsed direct current for rapid consolidation of material. Diffusion bonding of strontium titanate bicrystals without fracture, in a spark plasma sintering apparatus, is possible at high pressures due to the unusual temperature dependent plasticity behavior of strontium titanate. We demonstrate a method for the successful formation of bicrystals at accelerated time scales and lower temperatures in a spark plasma sintering apparatus compared to bicrystals formed by conventional diffusion bonding parameters. Bond quality was verified by scanning electron microscopy. A clean and atomically abrupt interface containing no secondary phases was observed using transmission electron microscopy techniques. Local changes in bonding across the boundary was characterized by simultaneous scanning transmission electron microscopy and spatially resolved electron energy-loss spectroscopy.

A viable technique for the formation of strontium titanate bicrystals at high pressure and fast heating rate via the spark plasma sintering apparatus is developed.

チタン酸ストロンチウム双結晶の形成に用いられるプラズマ焼結装置をスパーク

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with ...

Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, interface precipitation, and mini-emulsion. In all methods, well-defined, micrometer-sized spheres are obtained from a self-assembling process in solution. The vapor diffusion method can result in spheres with the highest sphericity and surface smoothness, yet the types of the polymers able to form these spheres are limited. On the other hand, in the mini-emulsion method, microspheres can be made from various types of polymers, even from highly crystalline polymers with coplanar, &#960;-conjugated backbones. The photoluminescent (PL) properties from single isolated microspheres are unusual: the PL is confined inside the spheres, propagates at the circumference of the spheres via the total internal reflection at the polymer/air interface, and self-interferes to show sharp and periodic resonant PL lines. These resonating modes are so-called "whispering gallery modes" (WGMs). This work demonstrates how to measure WGM PL from single isolated spheres using the micro-photoluminescence (&#181;-PL) technique. In this technique, a focused laser beam irradiates a single microsphere, and the luminescence is detected by a spectrometer. A micromanipulation technique is then used to connect the microspheres one by one and to demonstrate the intersphere PL propagation and color conversion from coupled microspheres upon excitation at the perimeter of one sphere and detection of PL from the other microsphere. These techniques, &#181;-PL and micromanipulation, are useful for experiments on micro-optic application using polymer materials.

Protocols for the synthesis of microspheres from polymers, the manipulation of microspheres, and micro-photoluminescence measurements are presented.

光共振器およびレーザ応用のためのポリマーマイクロスフェアの作製

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

その場でテスト用 LiPON ベース固体リチウム イオン Nanobatteries の集束イオンビーム ビーム加工

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Detecting the Water-soluble Chloride Distribution of Cement Paste in a High-precision Way

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a high-precision chloride profile. Firstly, paste specimens are molded, cured, and exposed to cyclic wet-dry conditions. Then, powder samples at different specimen depths are grinded when the exposure age is reached. Finally, the water-soluble chloride content is detected using a silver nitrate titration method, and chloride profiles are plotted. The key to improving the accuracy of the chloride distribution along the depth is to exclude the error in the powderization, which is the most critical step for testing the distribution of chloride. Based on the above concept, the grinding method in this protocol can be used to grind powder samples automatically layer by layer from the surface inward, and it should be noted that a very thin grinding thickness (less than 0.5 mm) with a minimum error less than 0.04 mm can be obtained. The chloride profile obtained by this method better reflects the chloride distribution in specimens, which helps researchers to capture the distribution features that are often overlooked. Furthermore, this method can be applied to studies in the field of cement-based materials, which require high chloride distribution accuracy.

A protocol for obtaining a water-soluble chloride profile by using a high precision milling method is presented.

セメント ペーストの水溶性塩化物の分布を高精度に検出

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a ...

Ultrasonic Fatigue Testing in the Tension-Compression Mode

Ultrasonic fatigue testing is one of a few methods which allow investigating fatigue properties in the ultra-high cycle region. The method is based on exposing the specimen to longitudinal vibrations on its resonance frequency close to 20 kHz. With use of this method, it is possible to significantly decrease the time required for the test, when compared to conventional testing devices usually working at frequencies under 200 Hz. It is also used to simulate loading of material during operation in high speed conditions, such as those experienced by components of jet engines or car turbo pumps. It is necessary to operate only in the high and ultra-high cycle region, due to the possibility of extremely high deformation rates, which can have a significant influence on the test results. Specimen shape and dimensions have to be carefully selected and calculated to fulfill the resonance condition of the ultrasonic system; thus, it is not possible to test the full components or specimens of arbitrary shape. Before each test, it is necessary to harmonize the specimen with the frequency of the ultrasonic system to compensate for deviations of the real shape from the ideal one. It is not possible to run a test until a total fracture of the specimen, since the test is automatically terminated after initiation and propagation of the crack to a certain length, when the stiffness of the system changes enough to shift the system out of the resonance frequency. This manuscript describes the process of evaluation of materials' fatigue properties at high-frequency ultrasonic fatigue loading with use of mechanical resonance at a frequency close to 20 kHz. The protocol includes a detailed description of all steps required for a correct test, including specimen design, stress calculation, harmonizing with the resonance frequency, performing the test, and final static fracture.

A protocol for ultrasonic fatigue testing in the high and ultra-high cycle region in axial tension-compression loading mode.

超音波疲労引張圧縮モードでのテスト

Ultrasonic fatigue testing is one of a few methods which allow investigating fatigue properties in the ultra-high cycle region. The method is based on ...

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57Fe isotope, namely M&#246;ssbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. M&#246;ssbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Here, we present a protocol to describe ex situ and in situ investigations of structural transformations in metallic glasses. We employed nuclear-based analytical methods which inspect hyperfine interactions. We demonstrate the applicability of M&#246;ssbauer spectrometry and nuclear forward scattering of synchrotron radiation during temperature-driven experiments.

Ex その場その場で調査構造変換の方法: 金属ガラスの結晶化の事例

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic ...

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone (ITZ)

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect of aggregate surface morphology on the formation of ITZ. First, a model concrete sample is prepared with a spherical ceramic particle in roughly the central part of the cement matrix, acting as a coarse aggregate used in common concrete/mortar. After curing until the designed age, the sample is scanned by X-ray computed tomography to determine the relative location of the ceramic particle inside the cement matrix. Three locations of the ITZ are chosen: above the aggregate, on the side of the aggregate, and below the aggregate. After a series of treatments, the samples are scanned with a SEM-BSE detector. The resultant images were further processed using a digital image processing method (DIP) to obtain quantitative characteristics of the ITZ. The surface morphology is characterized at the pixel level based on the digital image. Thereafter, K-means clustering method is used to illustrate the effect of surface roughness on ITZ formation.

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ

Hereby, we proposed a protocol to illustrate the effect of aggregate surface morphology on the ITZ microstructure. The SEM-BSE image were quantitatively analyzed to obtain ITZ's porosity gradient via digital image processing and a K-means clustering algorithm was further employed to establish a relationship between porosity gradient and surface roughness.

界面遷移帯における凝集表面形態の測定(ITZ)

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect ...