Biz elektrokimyasal deneyler ve enstrümantasyon (LSC ve JTH) desteğiyle için Kimya Virginia Askeri Enstitüsü (VMI) Bölümü kabul. Fakültesi Dekanı VMI Ofisi vallahi yayınları ile ilgili üretim ücretleri destekledi. Biz UNC EFRC kabul: Güneş yakıtlar Merkezi&#39;ni, bileşik sentezi ve karakterizasyonu malzeme desteği için Enerji, Bilim Ofisi, Ödül Numarası DE-SC0001011 altında Temel Enerji Bilimler Dairesi, ABD Bakanlığı tarafından finanse Enerji Frontier Araştırma Merkezi (DPH ).

1. Sentez 1 Göre: - (Şekil 4;, 5,5&#39;-dvbpy-bipiridin-divinil-2,2&#39; 5,5&#39; olan -terpiridin, 2 &#39;&#39; &#39;6&#39; PhTpy 4&#39;-fenil-2,2 olan) 1 sentez prosedür önceden sıraladı. 18 2. Bir elektrolit solüsyonu içinde 1 1.3 mM Monomer çözeltisi hazırlayın <ol><li> , Asetonitril, MeCN tetra-n-butilamonyum heksaflorofosfat bir 0.1 M stok elektrolit solüsyonu, TBAPF 6 hazırlayın. <ol><li> 3 A moleküler elekler ya da K 2 CO 3 aktive üzerinde tesadüfi H2O kaldırmak için 24 saat boyunca, MeCN yerleştirin </li><li> Ölçülü balona kurutulmuş bir 25.00 ml alev TBAPF 6 (0.969 g, 2.50 mmol) yerleştirin. </li><li> 3 parçacık kurutulmuş MeCN moleküler elek veya K 2 CO Filtre ve TBAPF içeren 25.00 ml ölçülü balona getirmek <suhacim b&gt; 6. </li></ol></li><li> 1 (0.0049 g, 5.2 x 10 -6 mol) ve kuru 4 gramlık bir şişe veya bir 10 ml&#39;lik yuvarlak tabanlı bir şişeye yerleştirilir ve MeCN içinde 0.1 M TBAPF 6 stok çözeltisi 4.00 mi ekleyin. </li><li> Orta gözenekli cam hamuru ile ayrılmış her bölmesi ile, 3 bölmeli hücrenin merkezi bölmeye 1 kırmızı-turuncu renkli elektrolitik çözeltisi 3,5-4,0 ml aktarın. </li><li> Hızlı bir şekilde dış bölümlerine sızıntının önlenmesi için MeCN kalan kuru 0.1M TBAPF 6 bazı merkezi bölme stok çözeltisi olarak, eşit bir yüksekliğe 3 bölmeli hücrenin dış bölmeyi doldurmak. Not: farklı bölümlerinde solüsyonlar yavaş &#39;yavaş karıştırılması ve çözücü yükseklikleri aynı değilse önemli ölçüde ana bölme konsantrasyonu değişecektir çünkü saat için önemli bir faktördür. </li></ol> 3 mm çaplı cam 3. Electropolymerize 1y Carbon Elektrot veya 1,0 cm 2 FTO Elektrot <ol><li> Azot / argon gaz alma tüpleri ve elektrotlar için septa hazırlayın. <ol><li> Yarıktan ince politetraflüoroetilen, PTFE, tüp 3 lastik septum her bir yarık kesin ve kılavuz. </li><li> Bölmeler biri ile Ag / iyodinin 3 referans elektrot kayıcı dış bölmelerin birinde referans elektrotu / PTFE tüp / septum yerleştirin ve septum ile bölme mühür. </li><li> Dış bölmeden birinde farklı bir septum yer aracılığıyla platin tel / PTFE tüp / septum platin tel / gazlı bez karşı elektrot Kılavuzu ve septum ile bölmesini kapatın. Yarık tel bükme önlemek için yeterince sert yeterince büyük veya tel değilse, septum ile platin tel karşı elektrot rehberlik geniş bir delik iğne kullanın. </li><li> Kalan septum ile taze cilalı 3 mm camsı karbon elektrodu Kılavuzu ve elektrot süspansiyon haline olduğunu yerleştirmekNDED bir FTO, sürgü için çözelti ya da, içinde, septum üzerinden bir Krokodilli bağlı bir kılavuz tel, daha sonra Krokodilli FTO kaydırma kelepçesi ve batmış sürgünün iletken yan karşı elektrot dik olduğundan emin olmak . <ol><li> Camsı karbon elektrot takmadan önce: pad dik elektrodu tutarken bir ıslatılmış parlatma pedi üzerine alümina (0.5 mikron) koyarak lehçe camsı karbon, daha sonra, bir figür-8 hareket için 30 saniye içinde elektrot hareket - parlatmak için elektrodun tüm tarafların eşit - ve bir MeCN fışkırtma şişe durulama ardından H 2 O su fışkırtma şişesi ile kalan alümina durulayın. </li><li> FTO, slayt sıkma önce: sürgünün 10 x 10 mm&#39;lik bölümünün maruz kaldığı bir şekilde bir 30 x 10 mm FTO, sürgünün orta kısmı etrafında olarak iletken olmayan kapton bant birkaç kat sarın. </li><li> Bir Posit FTO slayt / yerleştirerek tutarak FTO slayt UV-Vis spektrumu toplayıntutarlılığını sağlamak için önceden belirlenmiş olan spektrometrenin ışın yolu iyon. </li></ol></li></ol></li><li> 3-bölmesi elektrokimyasal hücrede çözümler De-havalandırmak. <ol><li> Azot / argon kaynağı Tygon hortumunun bir ucunu ve MeCN içeren bir gaz yıkayıcı diğer ucunu. </li><li> , Tygon boru başka bir parça kesin MeCN azot / argon yıkanmış akan bir ucunu ve bir 4 yollu splitter diğer ucunu. </li><li> 4 yollu splitter kalan 3 bağlantıları PTFE tüpleri bağlayın. </li><li> Bölmelerin her biri içinde çözeltiler halinde PTFE tüpleri daldırın ve bir çözelti hızlı bir köpürme başlar nitrojen / argon akışını açın. </li><li> Daha sonra, sadece çözeltinin yüzey üzerinde PTFE tüpleri çekme sistemi ve çözelti önlemek için bir inert gaz pozitif bir basınç sağlamak amacıyla / argon ile azot akışı bırakarak, 5-10 dakika için bir çözüm-havalandırma de devam convection kabarcıkların neden olduğu. </li></ol></li><li> Elektrokimyasal deneyler yapın. <ol><li> 3-bölmesi hücrede uygun elektrotlara potansiyostatla elektrotları bağlayın. </li><li> Bir dönüşümlü voltametri gerçekleştirin, CV, aşağıdaki parametrelerle deney: anahtarlama potansiyeller = 0 V ve -1,81 V; tarama / süpürme oranı = 100 mV / sn; döngüleri = 5 sayısı. </li><li> Geçmiş Deney tamamlandığında polimerizasyon çözeltisi çalışan (cam, karbon veya FTO) elektrot kaldırma ve yavaşça bir pipet ya da herhangi bir diğer monomer çözeltisinin ayrılması için bir fışkırtma şişe MeCN ile elektrodun yüzeyi yıkayın. </li></ol></li></ol> 4. Yüzey Kapsama Belirlenmesi <ol><li> Bir karşı elektrot ve bir referans elektrodu (electropolymerizatio kullanılan, tercihen, aynı referans elektrot ihtiva eden bir elektrokimyasal pile, 0.1 M TBAPF 6 / MeCN taze hazırlanmış bir çözelti içinde durulandı çalışma elektrodun). </li><li> Bir dönüşümlü voltametri gerçekleştirin, CV, aşağıdaki parametrelerle deney: anahtarlama potansiyeller = 0 ve 1,5 V; tarama / süpürme oranı = 100 mV / sn; döngü sayısı 15 =. </li><li> Adsorbe Elektropolimer Ru (III / II) çift için anodik ve katodik piklerin altında ücret entegre anodik ve katodik piklerin altında ücret ortalama ve Denklem 1 yüzey kapsama belirlemek kullanarak. </li><li> FTO slayt için: yerinde / ışın yolu renkli filmin geçtiği gibi UV-Vis numune tutucu önünde önceden belirlenmiş pozisyonda FTO slayt tutun. FTO slayt ıslak veya kuru olabilir ama boş spektrumları altında toplanmıştır aynı koşullar altında karşılaştırmalar yapabilirsiniz. </li><li> Söz konusu sürgü için toplanmıştır FTO spektrumu edilen frekans spektrumunu çıkarma önce filmin kendisi için bir emme spektrumu elde etmek için film-on-FTO tayfından Elektropolimerizasyon için. </li></ol>

<ol>
	<li>Abru&#241;a, H. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Coordination+chemistry+in+two+dimensions:+chemically+modified+electrodes.">Coordination chemistry in two dimensions: chemically modified electrodes.</a> Coordination Chemistry Reviews. 86, 135-189 (1988).</li><li>Waltman, R. J., Bargon, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrically+conducting+polymers:+a+review+of+the+electropolymerization+reaction,+of+the+effects+of+chemical+structure+on+polymer+film+properties,+and+of+applications+towards+technology.">Electrically conducting polymers: a review of the electropolymerization reaction, of the effects of chemical structure on polymer film properties, and of applications towards technology.</a> Canadian Journal of Chemistry. 64, 76-95 (1986).</li><li>Zhong, Y. -. W., Yao, C. -. J., Nie, H. -. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electropolymerized+films+of+vinyl-substituted+polypyridine+complexes:+Synthesis,+characterization,+and+applications.">Electropolymerized films of vinyl-substituted polypyridine complexes: Synthesis, characterization, and applications.</a> Coordination Chemistry Reviews. 257, 1357-1372 (2013).</li><li>Bard, A. J., Faulkner, L. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electrochemical Methods Fundamentals and Applications. , (1980).</li><li>Ramos Sende, J. 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=Electrocatalysis+of+CO2+Reduction+in+Aqueous+Media+at+Electrodes+Modified+with+Electropolymerized+Films+of+Vinylterpyridine+Complexes+of+Transition+Metals.">Electrocatalysis of CO2 Reduction in Aqueous Media at Electrodes Modified with Electropolymerized Films of Vinylterpyridine Complexes of Transition Metals.</a> Inorganic Chemistry. 34, 3339-3348 (1995).</li><li>Cosnier, S., Deronzier, A., Moutet, J. -. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+coating+of+a+platinum+electrode+by+a+poly(pyrrole)+film+containing+the+fac-Re(2,2'-bipyridine)(CO)3Cl+system+application+to+electrocatalytic+reduction+of+CO2.">Electrochemical coating of a platinum electrode by a poly(pyrrole) film containing the fac-Re(2,2'-bipyridine)(CO)3Cl system application to electrocatalytic reduction of CO2.</a> Journal of Electroanalytical Chemistry and Interfacial Electrochemistry. 207, 315-321 (1986).</li><li>Cosnier, S., Deronzier, A., Moutet, J. -. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrocatalytic+reduction+of+CO2+on+electrodes+modified+by+fac-Re(2,2'-bipyridine)(CO)3Cl+complexes+bonded+to+polypyrrole+films.">Electrocatalytic reduction of CO2 on electrodes modified by fac-Re(2,2'-bipyridine)(CO)3Cl complexes bonded to polypyrrole films.</a> Journal of Molecular Catalysis. 45, 381-391 (1988).</li><li>Toole, T. R., 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=Electrocatalytic+reduction+of+CO2+at+a+chemically+modified+electrode.">Electrocatalytic reduction of CO2 at a chemically modified electrode.</a> Journal of the Chemical Society, Chemical Communications. 20, 1416-1417 (1985).</li><li>Cheung, K. -. C., 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=Ruthenium+Terpyridine+Complexes+Containing+a+Pyrrole-Tagged+2,2&#8242;-Dipyridylamine+Ligand&#8212;Synthesis.">Ruthenium Terpyridine Complexes Containing a Pyrrole-Tagged 2,2&#8242;-Dipyridylamine Ligand&#8212;Synthesis.</a> Crystal Structure, and Electrochemistry. Inorganic Chemistry. 51, 6468-6475 (2012).</li><li>Ashford, D. 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=Water+Oxidation+by+an+Electropolymerized+Catalyst+on+Derivatized+Mesoporous+Metal+Oxide+Electrodes.">Water Oxidation by an Electropolymerized Catalyst on Derivatized Mesoporous Metal Oxide Electrodes.</a> Journal of the American Chemical Society. 136, 6578-6581 (2014).</li><li>Abru&#241;a, H. D., Denisevich, P., Umana, M., Meyer, T. J., Murray, R. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rectifying+interfaces+using+two-layer+films+of+electrochemically+polymerized+vinylpyridine+and+vinylbipyridine+complexes+of+ruthenium+and+iron+on+electrodes.">Rectifying interfaces using two-layer films of electrochemically polymerized vinylpyridine and vinylbipyridine complexes of ruthenium and iron on electrodes.</a> Journal of the American Chemical Society. 103, 1-5 (1981).</li><li>Gould, S., Gray, K. H., Linton, R. W., Meyer, T. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microstructures+in+thin+polymeric+films.+Photochemically+produced+molecular+voids.">Microstructures in thin polymeric films. Photochemically produced molecular voids.</a> Inorganic Chemistry. 31, 5521-5525 (1992).</li><li>Devenney, M., 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=Excited+State+Interactions+in+Electropolymerized+Thin+Films+of+Ru(II).">Excited State Interactions in Electropolymerized Thin Films of Ru(II).</a> Os(II), and Zn(II) Polypyridyl Complexes. The Journal of Physical Chemistry A. 101, 4535-4540 (1997).</li><li>Moss, J. 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=Sensitization+and+Stabilization+of+TiO2+Photoanodes+with+Electropolymerized+Overlayer+Films+of+Ruthenium+and+Zinc+Polypyridyl+Complexes:+A+Stable+Aqueous+Photoelectrochemical+Cell.">Sensitization and Stabilization of TiO2 Photoanodes with Electropolymerized Overlayer Films of Ruthenium and Zinc Polypyridyl Complexes: A Stable Aqueous Photoelectrochemical Cell.</a> Inorganic Chemistry. 43, 1784-1792 (2004).</li><li>Yang, J., Sykora, M., Meyer, T. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electropolymerization of Vinylbipyridine Complexes of Ruthenium(II) and Osmium(II) in SiO2 Sol&#8722;Gel Films. Inorganic Chemistry. 44, 3396-3404 (2005).</li><li>Nie, H. -. J., Shao, J. -. Y., Wu, J., Yao, J., Zhong, Y. -. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+Reductive+Electropolymerization+of+Metal+Complexes+with+5,5&#8242;-Divinyl-2,2&#8242;-Bipyridine.">Synthesis and Reductive Electropolymerization of Metal Complexes with 5,5&#8242;-Divinyl-2,2&#8242;-Bipyridine.</a> Organometallics. 31, 6952-6959 (2012).</li><li>Yao, C. -. J., Zhong, Y. -. W., Nie, H. -. J., Abru&#241;a, H. D., Yao, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Near-IR+Electrochromism+in+Electropolymerized+Films+of+a+Biscyclometalated+Ruthenium+Complex+Bridged+by+1,2,4,5-Tetra(2-pyridyl)benzene.">Near-IR Electrochromism in Electropolymerized Films of a Biscyclometalated Ruthenium Complex Bridged by 1,2,4,5-Tetra(2-pyridyl)benzene.</a> Journal of the American Chemical Society. 133, 20720-20723 (2011).</li><li>Harrison, D. P., 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=Coordination+Chemistry+of+Single-Site+Catalyst+Precursors+in+Reductively+Electropolymerized+Vinylbipyridine+Films.">Coordination Chemistry of Single-Site Catalyst Precursors in Reductively Electropolymerized Vinylbipyridine Films.</a> Inorganic Chemistry. 52, 4747-4749 (2013).</li><li>Calvert, J. M., 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=Synthetic+and+mechanistic+investigations+of+the+reductive+electrochemical+polymerization+of+vinyl-containing+complexes+of+iron(II),+ruthenium(II),+and+osmium(II).">Synthetic and mechanistic investigations of the reductive electrochemical polymerization of vinyl-containing complexes of iron(II), ruthenium(II), and osmium(II).</a> Inorganic Chemistry. 22, 2151-2162 (1983).</li><li>Moss, J. A., Argazzi, R., Bignozzi, C. A., Meyer, T. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electropolymerization+of+Molecular+Assemblies.">Electropolymerization of Molecular Assemblies.</a> Inorganic Chemistry. 36, 762-763 (1997).</li><li>Deronzier, A., Eloy, D., Jardon, P., Martre, A., Moutet, J. -. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electroreductive+coating+of+electrodes+from+soluble+polypyrrole-ruthenium+(II)+complexes:+ion+modulation+effects+on+their+electroactivity.">Electroreductive coating of electrodes from soluble polypyrrole-ruthenium (II) complexes: ion modulation effects on their electroactivity.</a> Journal of Electroanalytical Chemistry. 453, 179-185 (1998).</li><li>Mola, 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=Ru-Hbpp-Based+Water-Oxidation+Catalysts+Anchored+on+Conducting+Solid+Supports.">Ru-Hbpp-Based Water-Oxidation Catalysts Anchored on Conducting Solid Supports.</a> Angewandte Chemie International Edition. 47, 5830-5832 (2008).</li><li>Deronzier, A., Moutet, J. -. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polypyrrole+films+containing+metal+complexes:+syntheses+and+applications.">Polypyrrole films containing metal complexes: syntheses and applications.</a> Coordination Chemistry Reviews. 147, 339-371 (1996).</li><li>Sabouraud, G., Sadki, S., Brodie, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+mechanisms+of+pyrrole+electropolymerization.">The mechanisms of pyrrole electropolymerization.</a> Chemical Society Review. 29, 283-293 (2000).</li><li>Denisevich, P., Abru&#241;a, H. D., Leidner, C. R., Meyer, T. J., Murray, R. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electropolymerization+of+vinylpyridine+and+vinylbipyridine+complexes+of+iron+and+ruthenium:+homopolymers,+copolymers,+reactive+polymers.">Electropolymerization of vinylpyridine and vinylbipyridine complexes of iron and ruthenium: homopolymers, copolymers, reactive polymers.</a> Inorganic Chemistry. 21, 2153-2161 (1982).</li><li>Younathan, J. N., Wood, K. S., Meyer, T. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrocatalytic+reduction+of+nitrite+and+nitrosyl+by+iron(III)+protoporphyrin+IX+dimethyl+ester+immobilized+in+an+electropolymerized+film.">Electrocatalytic reduction of nitrite and nitrosyl by iron(III) protoporphyrin IX dimethyl ester immobilized in an electropolymerized film.</a> Inorganic Chemistry. 31, 3280-3285 (1992).</li><li>Ikeda, T., Schmehl, R., Denisevich, P., Willman, K., Murray, R. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Permeation+of+electroactive+solutes+through+ultrathin+polymeric+films+on+electrode+surfaces.">Permeation of electroactive solutes through ultrathin polymeric films on electrode surfaces.</a> Journal of the American Chemical Society. 104, 2683-2691 (1982).</li><li>Concepcion, J. 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=Making+Oxygen+with+Ruthenium+Complexes.">Making Oxygen with Ruthenium Complexes.</a> Accounts of Chemical Research. 42, 1954-1965 (2009).</li><li>Chen, Z., Concepcion, J. J., Jurss, J. W., Meyer, T. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-Site,+Catalytic+Water+Oxidation+on+Oxide+Surfaces.">Single-Site, Catalytic Water Oxidation on Oxide Surfaces.</a> Journal of the American Chemical Society. 131, 15580-15581 (2009).</li><li>Lapides, A. M., 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=Stabilization+of+a+Ruthenium(II)+Polypyridyl+Dye+on+Nanocrystalline+TiO2+by+an+Electropolymerized+Overlayer.">Stabilization of a Ruthenium(II) Polypyridyl Dye on Nanocrystalline TiO2 by an Electropolymerized Overlayer.</a> Journal of the American Chemical Society. 135, 15450-15458 (2013).</li><li>Paulson, S. C., Sapp, S. A., Elliott, C. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+and+Spectroelectrochemical+Investigations+into+the+Nature+of+Charge-Trapping+in+Electrochemically-Generated+Homopolymer+Films+of+Tris(4-vinyl-4&#8216;-methyl-2,2&#8216;-bipyridine)ruthenium(II).">Electrochemical and Spectroelectrochemical Investigations into the Nature of Charge-Trapping in Electrochemically-Generated Homopolymer Films of Tris(4-vinyl-4&#8216;-methyl-2,2&#8216;-bipyridine)ruthenium(II).</a> The Journal of Physical Chemistry B. 105, 8718-8724 (2001).</li><li>Laviron, E., Roullier, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=General+expression+of+the+linear+potential+sweep+voltammogram+for+a+surface+redox+reaction+with+interactions+between+the+adsorbed+molecules:+Applications+to+modified+electrodes.">General expression of the linear potential sweep voltammogram for a surface redox reaction with interactions between the adsorbed molecules: Applications to modified electrodes.</a> J. Electroanal. Chem. Interfacial Electrochem. 115, 65-74 (1980).</li><li>Laviron, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=General+expression+of+the+linear+potential+sweep+voltammogram+in+the+case+of+diffusionless+electrochemical+systems.">General expression of the linear potential sweep voltammogram in the case of diffusionless electrochemical systems.</a> J. Electroanal. Chem. 101, 19-28 (1979).</li><li>Ratcliff, E. L., Jenkins, J. L., Nebesny, K., Armstrong, N. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposited,+&#34;Textured&#34;+Poly(3-hexyl-thiophene)+(e-P3HT)+Films+for+Photovoltaic+Applications.">Electrodeposited, &#34;Textured&#34; Poly(3-hexyl-thiophene) (e-P3HT) Films for Photovoltaic Applications.</a> Chemistry of Materials. 20, 5796-5806 (2008).</li></ol>

No conflicts of interest declared.

Elektropolimerizasyon diğer tekniklere yaygın değildir kontrol değişkenler geniş bir ürün yelpazesi sunmaktadır. Gibi reaktif (monomer) konsantrasyonu, sıcaklık, solvent gibi standart reaksiyon değişkenleri ek olarak, elektrokimyasal ilave elektrokimyasal yöntemlerin ortak elektrokimyasal deney parametreleri ile kontrol edilebilir. CV tarama oranları, anahtarlama potansiyeller ve döngü sayısı Elektropolimerlerin birikimi etkiler. Örneğin, ligand azaltma dalgaları aracılığıyla döngü s...

Elektropolimerizasyon doğrudan bir elektrod yüzeyinde monomer ön-polimerizasyonunu başlatmak için uygulanan bir potansiyel kullanır ve Elektrokataliz fotokimyasal ince elektro-aktif ve / veya elektrot ve yarı iletken yüzeyler üzerinde aktif polypyridyl filmler. 1-4 üretmek için kullanılabilir olan bir polimerleştirme tekniği 5-10 elektron transferi, 11, 12 fotokimyasal, 13-16 elektrokromizm, 17 ve koordinasyon kimyası 18 elektrokimyasal filmlerde incelenmiştir. Bu teknik ilk olarak vinil 3, 5, 7, 8, 11-15, 19, 20 ve pirol 6, 9 elektrokimyasal bir Meyer-Murray işbirliği Kuzey Carolina Üniversitesi&#39;nde geliştirilen, 21-24 beni derivesubstratlar iletken çeşitli Tal kompleksleri. 1 metal kompleksleri ile koordine olduğunda, Elektropolimerler ürettiler ortak piridil göre ligandların bir dizi sunulur Şekil. Pirol-fonksiyonlu ligandlar, elektrokimyasal (Şekil 2), oksidatif elektrokimyasal sonuçlanan pirol kısımların oksidasyonu ile başlatılır ise indirgeyici elektrokimyasal olarak, vinil ihtiva eden bileşiklerin elektrokimyasal, vinil gruplarına konjuge piridil ligandların indirgendikten sonra meydana gelir. Elektrokimyasal teknoloji doğrudan herhangi bir elektroda hemen hemen herhangi bir geçiş metali kompleksi birleştirilmesi için genel bir yöntem sağlamak amacı ile geliştirilmiştir. Yöntemin çok yönlülük Elektropolimer modifiye elektrotlar sayısız incelemelere kapıyı açar. Elektrotuna doğrudan bağ içeren diğer bağlanma stratejileri, aksine, elektrokimyasal zarf sunarelektrot yüzeyi ön-modifikasyon gerektiren değil antage. . Bu nedenle, bağımsız bir yüzey bileşimi ya da morfolojisi 4, 10, 25, iletken alt-tabakaların herhangi bir sayıda uygulanabilir, 26 Bu çok yönlülük, polimer uzunluğu büyüdükçe gibi fiziksel özelliklerini değiştirmek için bir sonucudur; monomerler, elektrolitik çözelti içinde çözünür olan, ancak polimerizasyon meydana gelir ve çapraz bağlama elektrot yüzeyi meydana gelir filmi, çökeltme ve fiziksel adsorpsiyon (Şekil 3) rigidifies. 27 Yaygın güneş yakıtlar araştırmada kullanılan yüksek pH&#39;larda, kararsızdır oksit su içinde yüzeyler veya fosfonat-türevli kompleksleri üzerinde kararsız oksit yüzeyine bağlı karboksilat, karşılaştırıldığında, bu ara yüzey, elektrot polimer film yapıları stabilite yararı teklif Büyük bir pH aralığında (0-14) üzerinde organik çözücüler ve su dahil medyanın çeşitli.28-30 Elektropolimerizasyon ayrıca alt-tek tabaka karboksilat veya fosfonat-türetilmiş kompleksleri-arayüz yapıları tek tabaka yüzey sigortaların sınırlı ise onlarca veya benzerleri tek tabaka yüzlerce, açıkça yüzey sigortaların büyük aralıkları, filmler yatırabilirsiniz. Vinil ya da pirrol içeren piridil ve polypyridyl bileşikler herhangi bir sayıda polimerizasyon kapasitesine sahip olmakla birlikte, [Ru II (PhTpy) (5,5&#39;-dvbpy) (MeCN)] (PF6) 2, (1; PhTpy 4&#39;-fenil -2,2 &#39;: 6&#39;, 2 &quot;&#39;- -terpiridin, 5,5&#39;-dvbpy is-divinil-2,2&#39; 5,5&#39;-bipiridin; Şekil 4) indirgeyici elektrokimyasal olarak göstermek için bir model kompleksi olarak kullanılacaktır camsı karbon ve fluor-takviyeli kalay oksit, FTO, bu raporda elektrotlar. 1 nedeniyle metal-li potansiyel elektrokatalitik uygulamalar sahip modern Elektropolimer öncünün bir örneğidir veGand yük transferi, MLCT, ışık tayfının görünür bölgede yatan emme spektrumu, UV-Vis spektroskopisi. 18, 30, 1 için burada sunulan bazı sonuçlar zaten biraz değiştirilmiş formda yayınlanmış olduğunu unutmayın. 18 ile araştırılabilir

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reductive electropolymerization of a vinyl-containing poly-pyridyl complex on glassy carbon and fluorine-doped tin oxide electrodes

Kontrol elektrot yüzey modifikasyonu alanları güneş yakıt uygulamaları ile, özellikle de bir dizi önemlidir. Elektrokimyasal Helmholtz tabakasında alt tabakalar polimerizasyonunu başlatmak için uygulanan bir potansiyeli kullanarak bir elektrot yüzeyinde bir polimerik film electrodeposits bir yüzey değiştirme yöntemidir. Bu kullanışlı tekniği ilk 1980&#39;lerin başında Chapel Hill&#39;deki North Carolina Üniversitesi&#39;nde Murray-Meyer işbirliği ile kurulan ve monomerik madde gibi inorganik kompleksleri içeren filmlerin çok sayıda fiziksel fenomenleri incelemek için kullanılmıştır. Burada, cam, karbon ve flüor karışımlı kalay oksit kaplama elektrotlar üzerine vinil içerikli poli-piridil kompleksinin indirgeyici elektrokimyasal olarak gerçekleştirerek, bir inorganik kompleks ile kaplama elektrotları için bir prosedür vurgulamaktadır. Elektrokimyasal hücre konfigürasyonları ve sorun giderme prosedürleri Öneriler dahildir. Değil, e rağmenxplicitly burada açıklanan, pirol-ihtiva eden bileşiklerin, oksidatif elektrokimyasal vinil bazlı indirgeyici elektrokimyasal benzer prosedürler takip eder, ancak çok daha az duyarlıdır oksijen ve su bulunmaktadır.

Reçete CV deney (Protokol Metin ADIM 3.3.2) ilerleme gözlemleyerek zaman Elektropolimer büyüme en kolay tanınır. 5 Bir 0.071 cm 2 (3 mm çapında) üzerine Elektropolimer büyüme, 1 ile camsı karbon elektrot örneğidir Şekil. Deneyin birinci döngüsü voltogramda yaklaşık 1 ve 2. bağ merkezli indirgeme dalgaları ile birbirini takip eden devrelerine içindeki konsantrasyonu (Şekil 5, siyah iz), ancak bir rutenyum ç?...

Watch this Scientific Journal Video about Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes at JoVE.com

Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization.

Camsı karbon ve flüor katkılı kalay oksit elektrotlar üzerinde vinil içerikli poli-piridil Kompleksinin indirgeyici elektrokimyasal

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is ...

reductive-electropolymerization-vinyl-containing-poly-pyridyl-complex

Research

JoVE Journal

Chemistry

11.7K Görüntüleme.  Virginia Military Institute. A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization. 

Video: Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

Improved In-gel Reductive &#946;-Elimination for Comprehensive O-linked and Sulfo-glycomics by Mass Spectrometry

Separation of proteins by SDS-PAGE followed by in-gel proteolytic digestion of resolved protein bands has produced high-resolution proteomic analysis of biological samples. Similar approaches, that would allow in-depth analysis of the glycans carried by glycoproteins resolved by SDS-PAGE, require special considerations in order to maximize recovery and sensitivity when using mass spectrometry (MS) as the detection method. A major hurdle to be overcome in achieving high-quality data is the removal of gel-derived contaminants that interfere with MS analysis. The sample workflow presented here is robust, efficient, and eliminates the need for in-line HPLC clean-up prior to MS. Gel pieces containing target proteins are washed in acetonitrile, water, and ethyl acetate to remove contaminants, including polymeric acrylamide fragments. O-linked glycans are released from target proteins by in-gel reductive &#946;-elimination and recovered through robust, simple clean-up procedures. An advantage of this workflow is that it improves sensitivity for detecting and characterizing sulfated glycans. These procedures produce an efficient separation of sulfated permethylated glycans from non-sulfated (sialylated and neutral) permethylated glycans by a rapid phase-partition prior to MS analysis, and thereby enhance glycomic and sulfoglycomic analyses of glycoproteins resolved by SDS-PAGE.

Improved In-gel Reductive &amp;#946;-Elimination for Comprehensive O-linked and Sulfo-glycomics by Mass Spectrometry

In order to comprehensively explore the diversity of O-linked glycans, a new procedure for in-gel reductive &#946;-elimination, combined with permethylation and a rapid phase-partition method, is applied to the analysis of O-linked glycans directly released from glycoproteins resolved by SDS-PAGE and amenable to subsequent glycomic analysis by mass spectrometry.

Kütle spektrometresi ile In-jel Geliştirilmiş İndirgemeli β-Eleme Kapsamlı O-bağlı ve için Sulfo-Glikomik

Separation of proteins by SDS-PAGE followed by in-gel proteolytic digestion of resolved protein bands has produced high-resolution proteomic analysis of ...

Kimya

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

Karmaşık Oksit İnce Filmlerin Epitaksiyel Büyüme için atomik Tanımlı Şablonlar

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Transport of Surface-modified Carbon Nanotubes through a Soil Column

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, electronics and biomedical applications. Due to their accelerating production and use, CNTs constitute a potential environmental risk if they are released to soil and groundwater systems. It is therefore essential to improve the current understanding of environmental fate and transport of CNTs. The transport and retention of CNTs in both natural and artificial media have been reported in literature, but the findings widely vary and are thus not conclusive. There are a number of physical and chemical parameters responsible for variation in retention and transport. In this study, a complete procedure of selected multiwalled carbon nanotubes (MWCNTs) is presented starting from their surface modification to a complete set of laboratory column experiments at critical physical and chemical scenarios. Results indicate that the stability of the commercially available MWCNTs are critical with their attached surface functional group which can also influence the transport and retention of MWCNT through the surrounding medium.

Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles.

Bir Toprak Kolonundaki Yüzey modifiye Karbon Nanotüpler taşınması

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, ...

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

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

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

CdSe @ CdS nanorods üzerinde İridyum Oksit Nanopartiküller Fotokimyasal Oksidatif Büyüme

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

On-line Analysis of Nitrogen Containing Compounds in Complex Hydrocarbon Matrixes

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The composition of heavy crude oils and shale oils varies substantially depending on the origin of the mixture. In particular they contain an increased amount of nitrogen containing compounds compared to the conventionally used sweet crude oils. As nitrogen compounds have an influence on the operation of thermal processes occurring in coker units and steam crackers, and as some species are considered as environmentally hazardous, a detailed analysis of the reactions involving nitrogen containing compounds under pyrolysis conditions provides valuable information. Therefore a novel method has been developed and validated with a feedstock containing a high nitrogen content, i.e., a shale oil. First, the feed was characterized offline by comprehensive two-dimensional gas chromatography (GC &#215; GC) coupled with a nitrogen chemiluminescence detector (NCD). In a second step the on-line analysis method was developed and tested on a steam cracking pilot plant by feeding pyridine dissolved in heptane. The former being a representative compound for one of the most abundant classes of compounds present in shale oil. The composition of the reactor effluent was determined via an in-house developed automated sampling system followed by immediate injection of the sample on a GC &#215; GC coupled with a time-of-flight mass spectrometer (TOF-MS), flame ionization detector (FID) and NCD. A novel method for quantitative analysis of nitrogen containing compounds using NCD and 2-chloropyridine as an internal standard has been developed and demonstrated.

A method combining comprehensive two-dimensional gas chromatography with nitrogen chemiluminescence detection has been developed and applied to on-line analysis of nitrogen containing compounds in a complex hydrocarbon matrix.

Karmaşık Hidrokarbon Matrisler içinde İçeren Bileşiklerin Azot On-line Analizi

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The ...

Investigations on the Ga(III) Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) complex and protocols for the preparation of its novel non-radioactive, i.e., natural Ga(III) as well as radioactive 68Ga complex. The ligand as well as the Ga(III) complex were characterized by nuclear magnetic resonance (NMR) spectroscopy, mass spectrometry and elemental analysis. 68Ga was obtained by a standard elution method from a 68Ge/68Ga generator. Experiments to evaluate the 68Ga-labeling efficiency of EOB-DTPA at pH 3.8&#8211;4.0 were performed. Established analysis techniques radio TLC (thin layer chromatography) and radio HPLC (high performance liquid chromatography) were used to determine the radiochemical purity of the tracer. As a first investigation of the 68Ga tracers&#39; lipophilicity the n-octanol/water distribution coefficient of 68Ga species present in a pH 7.4 solution was determined by an extraction method. In vitro stability measurements of the tracer in various media at physiological pH were performed, revealing different rates of decomposition.

Investigations on the GaIII Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

A procedure for the isolation of EOB-DTPA and subsequent complexation with natural Ga(III) and 68Ga is presented herein, as well as a thorough analysis of all compounds and investigations on labeling efficiency, in vitro stability and the n-octanol/water distribution coefficient of the radiolabeled complex.

EOB-DTPA ve Ga (III) Complex Araştırmalar Onun<sup&gt; 68</sup&gt; Ga Radyoaktif Analog

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) ...

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a free-radical polymerization strategy to enable the modulation of the nanotube surface properties and produce supramolecular self-assembly of the nanostructures. First, a selective hydroxylation of the pristine nanotubes through a biphasic catalytically mediated oxidation reaction creates superficially distributed reactive sites at the sidewalls. The latter reactive sites are subsequently modified with methacrylic moieties using a silylated methacrylic precursor to create polymerizable sites. Those polymerizable groups can address further polymerization of styrene to produce a hybrid nanomaterial containing PS chains grafted to the nanotube sidewalls. The polymer-graft content, amount of silylated methacrylic moieties introduced and hydroxylation modification of the nanotubes are identified and quantified by Thermogravimetric Analysis (TGA). The presence of reactive functional groups hydroxyl and silylated methacrylate are confirmed by Fourier Transform Infrared Spectroscopy (FT-IR). Polystyrene-grafted carbon nanotube solutions in tetrahydrofuran (THF) provide wall-to-wall collinearly self-assembled nanotubes when cast samples are analyzed by transmission electron microscopy (TEM). Those self-assemblies are not obtained when suitable blanks are similarly cast from analogous solutions containing non-grafted counterparts. Therefore, this method enables the modification of the nanotube anisotropic patchiness at the sidewalls which results into spontaneous auto-organization at the nanoscale.

A procedure for the synthesis of polystyrene-grafted multiwalled carbon nanotubes using successive chemical modification steps to selectively introduce the polymer chains to the sidewalls and their self-assembly via anisotropic patchiness is presented.

Multiwalled karbon nanotüpler kendinden montajlı etkinleştirmek için polistiren ve Anizotropik seçimdeki aşılama

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a ...

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.

Elektrokimyasal empedans spektroskopisi elektrokimyasal oranı sürekli tahmini için bir araç olarak

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

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

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven effective in gas adsorption, separations, and catalysis. MOFs are most commonly synthesized as bulk powder, requiring additional processes to adhere them to functional devices and fabrics that risk decreasing the powder porosity and adsorption capacity. Here, we demonstrate a method of first coating fabrics with metal oxide films using atomic layer deposition (ALD). This process creates conformal films of controllable thickness on each fiber, while providing a more reactive surface for MOF nucleation. By submerging the ALD coated fabric in solution during solvothermal MOF synthesis, the MOFs create a conformal, well-adhered coating on the fibers, resulting in a MOF-functionalized fabric, without additional adhesion materials that may block MOF pores and functional sites. Here we demonstrate two solvothermal synthesis methods. First, we form a MIL-96(Al) layer on polypropylene fibers using synthetic conditions that convert the metal oxide to MOF. Using initial inorganic films of varying thicknesses, diffusion of the organic linker into the inorganic allows us to control the extent of MOF loading on the fabric. Second, we perform a solvothermal synthesis of UiO-66-NH2 in which the MOF nucleates on the conformal metal oxide coating on polyamide-6 (PA-6) fibers, thereby producing a uniform and conformal thin film of MOF on the fabric. The resulting materials can be directly incorporated into filter devices or protective clothing and eliminate the maladroit qualities of loose powder.

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

Metal-organic frameworks are effective in gas storage and heterogeneous catalysis, but typical synthesis methods result in loose powders that are difficult to incorporate into smart materials. We demonstrate a method of first coating fabrics with ALD metal oxides, resulting in conformal films of MOF on the fabrics during solvothermal synthesis.

Solvothermal sentez MIL-96 ve UIO-66-NH2 atom katman üzerinde Metal oksit kaplama Fiber paspaslar üzerine yatırılır.

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven ...

Negative Additive Manufacturing of Complex Shaped Boron Carbides

Boron carbide (B4C) is one of the hardest materials in existence. However, this attractive property also limits its machineability into complex shapes for high wear, high hardness, and lightweight material applications such as armors. To overcome this challenge, negative additive manufacturing (AM) is employed to produce complex geometries of boron carbides at various length scales. Negative AM first involves gelcasting a suspension into a 3D-printed plastic mold. The mold is then dissolved away, leaving behind a green body as a negative copy. Resorcinol-formaldehyde (RF) is used as a novel gelling agent because unlike traditional hydrogels, there is little to no shrinkage, which allows for extremely complex molds to be used. Furthermore, this gelling agent can be pyrolyzed to leave behind ~50 wt% carbon, which is a highly effective sintering aid for B4C. Due to this highly homogenous distribution of in situ carbon within the B4C matrix, less than 2% porosity can be achieved after sintering. This protocol highlights in detail the methodology for creating near fully dense boron carbide parts with highly complex geometries.

A method called negative additive manufacturing is used to produce near fully dense complex shaped boron carbide parts of various length scales. This technique is possible via the formulation of a novel suspension involving resorcinol-formaldehyde as a unique gelling agent that leaves behind a homogenous carbon sintering aid after pyrolysis.

Karmaşık şekilli bor karbürler katkı üretimini olumsuz

Boron carbide (B4C) is one of the hardest materials in existence. However, this attractive property also limits its machineability into complex shapes for ...