Bu eser Rowland Fellows programı Rowland Enstitüsü Harvard Üniversitesi tarafından desteklenmiştir. Bu eser kısmen için Nano sistemleri (CNS), Ulusal Bilim Vakfı Ödülü altında tarafından desteklenen Ulusal nanoteknoloji altyapı ağı üyesi merkezinde gerçekleştirilen yok. ECS-0335765. MSS Harvard Üniversitesi bir parçasıdır.

1. hazırlanması Ni tek Atom katalizör (NiN-GS)
<ol><li>Electrospinning öncü çözüm hazırlanması<ol>
<li>20 mL mercek şişeyi al, poliakrilonitril 0.5 g dağıtılması (Mw= 150.000), polypyrrolidone 0.5 g (Mw1,300,000 =), 0,5 g Ni (NO3)2·6H2O ' ya ve dicyandiamide (DCDA) 10 ml 0.1 g dimethylformamide (DMF).</li>
		<li>DMF karışımı ile 80 ° C ısı ve 80 ° C'de sabit tüm Polimerler ve tuz çözünmüş ve net bir çözüm görülmektedir kadar karıştırma ile karışımı tutmak.</li>
	</ol>
</li>
	<li>Polimer lifleri üretmek için Electrospinning<ol>
<li>Geleneksel electrospinning parametreleri olarak belirleme: 15 kV statik elektrik gerilimi, hava 15 cm boşluk mesafe, 8 × 8 cm karbon elyaf kağıt (CFP) ile - bir koleksiyon substrat 4 kV elektrik voltaj.</li>
		<li>Öncü çözüm 5 mL 5 mL şırınga hulâsa, şırınga pompa 1.2 mL akış hızında başlangıç s−1, sonra Başlat electrospinning. Not: Yüksek gerilim electrospinning için kullanılır. Çok düşük akım sistemi üzerinden işlem iplik sırasında gider de, yalıtılmış bir ahşap dolap önerilmektedir.</li>
		<li>Electrospinning işlemi bittiğinde CFP substrat al. Bir polimer fiber film CFP yüzey kapsar.</li>
	</ol>
</li>
	<li>Polimer lifleri karbon nanotüpler tavlama<ol>
<li>Olarak hazırlanan polimer fiber film/CFP bir kutu fırın içinde 1,5 saat içinde 300 ° c ısı ve sıcaklık polimerler okside 0,5 h için devam. Not: oksitlenmeye işleminden sonra nanofibers (NFs) duran filmde kaynaklanan karbon kağıdı kendi kendine müstakil.</li>
		<li>Bu nanofibers küçük parçalar halinde kesmek için bir makas kullanın (~ 0.5 cm × 2 cm) ve kuvars tekne içine koyun.</li>
		<li>Kuvars tekne bir tüp fırın içine yerleştirin ve gaz (%5 H2 ' Ar) atmosfer oluşturan içinde deaerate. 100 sccm olarak gaz debi ve basınç 1 Tor olarak tutun.</li>
		<li>300 ° C-10 dk ramping ve 750 ° c, nerede o başka bir 1 h için tutulur ve aşağı doğal soğutma ardından 2 h ramping içinde ısıtır.</li>
	</ol>
</li>
	<li>Top fabrikası olarak sentezlenmiş NiN-GS katalizör nanopowders kataliz ve karakterizasyonu için 5 min için.</li>
</ol>2. elektrokimyasal CO2 azaltma ölçümleri
<ol><li>Hücre ve elektrotları<ol>
<li>MA 24 h için herhangi kaldırmak için izleme metal miktarını için aşağıdaki ölçümler 0.1 M KHCO3 elektrolit hazırlamak, ilk KHCO3 ultrasaf su 250 ml 2.5 g geçiyoruz, o zaman elektroliz 0,1 adlı iki grafit çubuk arasındaki tarafından elektrolit arındırmak için iyonları.</li>
		<li>Bir taze (mamüllerinin) cilalı cam gibi karbon (1 cm × 2 cm) alın ve çalışma elektrot substrat olarak bir mamüllerinin etkisiz, hidrofobik balmumu ile onun arka kapak.</li>
		<li>4 mL mercek şişe alın, 1 mL etanol ve İonomeri çözüm (%5 2-proponal) şişe içinde 100 µL NiN-GS katalizör hazırlanan 5 mg karıştırın ve bir homojen katalizör mürekkep askıya almak 20 dk için solüsyon içeren temizleyicide.</li>
		<li>Damlalıklı 80 µL üzerine 2 cm2 cam gibi karbon yüzey (0.2 mg cm-2 toplu yükleme) ve vakumlu katalizör mürekkebin kuru katalizör örtülü elektrot kullanımı önce bir desiccator.</li>
		<li>Platin bir folyo ve doymuş kalomel elektrot (SCE) sayaç ve referans elektrot, sırasıyla kullanın.</li>
		<li>Proton değişim membran, elektrokimyasal testleri çalıştıran yanı sıra montaj Yukarıdaki 3 elektrotlar için ayrılmış bir özelleştirilmiş gastight H-tipi cam hücre, kullanın.</li>
		<li>Çalışma elektrot ve SCE referans elektrot bir yerde H-hücre ve Pt folyo elektrot diğer odasında yerleştirin. Enjekte ~ her yerde H-hücre elektrolit 25 mL.</li>
		<li>H-hücredeki 3 elektrotlar elektrokimyasal iş istasyonu potansiyel denetim için bağlayın.</li>
		<li>N2doğru 30 dk için N2 (kütle akış denetleyicisi tarafından izlenen) 50.0 sccm adlı elektrolit kabarcık-doymuş 0.1 M KHCO3.</li>
		<li>EC-Lab yazılımında çevrimsel Voltammetry (CV) tekniği seçin, "-10 V 10 V", "E aralığı (potansiyel)" ayarla "Ben"Otomatik ", (geçerli) aralığı" gerçekleştirmek 5 sürekli CV tarama -0,5 V-1.8 V 50 mV/s N2tarama oranında (SCE) vs için-doymuş 0.1 M KHCO3.</li>
		<li>Değiştirmek 50 sccm CO2 gaz akışı için CO2doğru 30 dk bekleyin-doymuş 0.1 M KHCO3 elektrolit ve aynı CO2 akışını aşağıdaki elektroliz boyunca korumak.</li>
		<li>EC-Lab yazılımında CV tekniği seçin, "-10 V 10 V", "E aralığı (potansiyel)" ayarla "Ben"Otomatik ", (geçerli) aralığı" gerçekleştirmek 5 sürekli CV tarama -0,5 V-1.8 V 50 mV/s CO2tarama oranında (SCE) vs için-doymuş 0.1 M KHCO3.</li>
		<li>Bir pH metre elektrolitler, YanipH değerini belirlemek için kullanın., 0.1 M KHCO3 N2 veya CO2ile doymuş.</li>
		<li>Tüm potansiyelleri içinde bu iş istimal tersinir hidrojen elektrot (RHE) ölçek SCE karşı ölçülen dönüştürmek E (vs RHE) = E (vs SCE) + 0,244 V + 0.0591 × pH.</li>
		<li>EC-Lab yazılım çözüm direnç (Ru) Potentiostatic elektrokimyasal empedans spektroskopisi (PEIS) tekniği, sonra frekans ayarı aralığı 200 kHz ila 0.1 Hz den seçerek belirlemek, direnç değeri kaydedin.</li>
		<li>El ile telafi IR-damla E (IR düzeltilmiş vs RHE) = E (vs RHE) - Ru × ben (ortalama geçerli amper).</li>
	</ol>
</li>
	<li>CO2 azaltma ürünleri analiz on-line gaz Kromatograf (GC) tarafından<ol>
<li>Gaz ürünleri Çözümleme sırasında CO2RR için moleküler elek 5A ve micropacked sütun birleşimi ile donatılmış bir GC, istihdam. Not: Detaylı GC sütun türleri ekli Malzemeler tablobulunabilir.</li>
		<li>H2 konsantrasyon ölçmek için bir ısı iletkenlik dedektörü (TCD) ve bir alev iyonizasyon detektörü (FID) bir methanizer kantitatif analiz CO içerik ve/veya herhangi bir diğer Alkan türler ile kullanın.</li>
		<li>İki farklı standart gazlar CO konsantrasyon ve H2 kalibrasyon Eğriler için kullanın (H2: 100 ve 1042 ppm; CO: 100 ve 496.7 ppm; Argon ile dengeli bir).</li>
		<li>Elektroliz sırasında CO2 gaz debisi 50.0 sccm adlı korumak, CO2 CO2içeren Katodik bölmesine teslim-doymuş 0.1 M KHCO3 elektrolit ve havalandırma egzoz GC içine.</li>
		<li>Kademeli ayar çalışma elektrodu,--dan-0.3-V 1.0 RHE, vs arasında değişen üzerinde gerilim devam ~ her potansiyel ve kayda karşılık gelen chronoamperimetric eğrisi 15 dakikadır.</li>
		<li>H2 ve CO içindekiler TCD ve FID sinyalleri, egzoz içinde sırasıyla belirler. Not: Gaz ürünleri sonra sürekli bir elektroliz örneklenmiş ~ her potansiyel altında 10 dak. Sürekli olarak karışık 50 sccm CO2 gaz H2 ve CO, GC örnekleme döngü (1 mL) elektroliz sırasında akan üretti.</li>
		<li>Kısmi akım yoğunluğu için verilen gaz ürün olarak hesapla: <img alt="Equation" src="/files/ftp_upload/57380/57380eq2.jpg"> Ben x online GC kalibrasyon Eğriler için başvurulan tarafından belirlenen belirli ürün birim kısmını olduğu yerde iki standart gaz örnekleri (Scott ve Airgas), v 50 sccm akış hızı, nben sayısı Elektron dahil, p0 101.3 kPa, = ve F Faradaic sabiti ve R gaz sabiti.</li>
		<li>Her potansiyel olarak, karşılık gelen Faradaic verimlilik (FE) hesaplamak <img alt="Equation" src="/files/ftp_upload/57380/57380eq7.jpg"> </img>. Not: Genel olarak Faradaic verimliliği gaz debisi, akım yoğunluğu ve GC gaz toplama çözümleme hataları nedeniyle % 90-110 aralığındaki olabilir.</li>
	</ol>
</li>
</ol>

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Yukarıdaki electrospinning süreç içinde iki önemli adım malzeme sentezi yordamlarda belirtmek gerekir: 1) Isıtma DMF karışımı (Adım 1.1.2) iplik oranı eşleşecek şekilde ve 2) pompa hızını (Adım 1.2.2) ayarlama. Şekil 1A SEM görüntü birbirleri ile bağlantılı elde edilen karbon nanofibers gösterir (~ 200 nm çapında). Küçük parçalar halinde şekil 1Badımında gösterildiği gibi karakterizasyonu için freze topu tarafından kırı...

Dönüştürme CO2 kimyasal madde veya yakıtlar temiz elektrik kullanarak içine daha fazla CO2 emisyonu1,2,3,4önlemek için olası bir yol olarak giderek önem kazanıyor, 5,6. Ancak, pratik Bu uygulama şu anda düşük etkinlik ve seçicilik CO2 azaltma tepki (CO2RR) yüksek Kinetik engelleri ve rekabet nedeniyle ile hidrojen evrim reaksiyonu (HER) sulu tarafından meydan medya. Fe, Co, Ni, gibi geleneksel Geçiş metalleri katalizör çoğunu kendi mükemmel HER etkinlikler7,8nedeniyle düşük CO2RR seçicilik sergi. Etkili bir şekilde tepki yolları bu geçiş metal katalizörler üzerinde değiştirmek için malzeme özellikleri ayarlama onların CO2RR seçicilik geliştirmek için kritik hale gelir. Katalizörler elektronik özelliklerini değiştirmek için farklı yöntemler arasında bir tek-atom Morfoloji metal atomları Dispergatör onların toplu muadili karşılaştırıldığında son zamanlarda önemli ölçüde değiştirilmiş katalitik davranışları nedeniyle yoğun ilgi çekiyor 9 , 10 , 11. ancak, sınırsız atomlar yüksek hareketlilik nedeniyle, tek metal atomları destekleyici malzemeler varlığı olmaksızın elde etmek oldukça zor. Bu nedenle, bir ana bilgisayar matris malzeme ile sınırlandırmak ve geçiş metal atomları ile koordine etmek için oluşturulan hataları gereklidir. Bu yeni fırsatlar için açabilir: 1) CO2RR etkin sitelere ve 2 geçiş metal elektronik özellikleri ayarlamak) aynı zamanda temel mekanizması çalışmaları için nispeten basit atomik koordinasyon korumak. Ayrıca, kapalı bir ortamda sıkışıp bu geçiş metal atomları kolayca çekirdekleşme veya rekonstrüksiyonlar birçok durumlarda12,13 gözlenen yüzey atomlarının engeller kataliz sırasında taşınamaz ,14.
İki boyutlu katmanlı Grafin CO2 azaltma ve onu katalitik reaksiyonlar için onların yüksek elektron iletkenlik, kimyasal kararlılık ve hareketsizlik nedeniyle metal tek atom için konağı olarak özel ilgi var. Daha da önemlisi, Fe, Co, Ni metaller ve onların yüzey15karbon graphitization göreve katalizler edebilmek için biliniyordu. Kısacası, bu geçiş metallerden karbon ile işlem tavlama yüksek sıcaklık termal sırasında alaşım. Sıcaklık düştüğünde, karbon Alaşımlandırma faz dışı çökelti başlar ve geçiş metal yüzeyi formu grafen katmanlara katalizlenir. Bu işlem sırasında oluşturulan, Grafin kusurları ile metal tek atom bu grafen hataları etkin sitelere CO2RR16,17,18,19olarak tuzağa. Burada, yeni uygulayıcıları tek atom kataliz, de alanında açık bir gösteri on-line co2 azaltma ürün analizi sağlamak için yardım isteyen bu ayrıntılı iletişim kuralı raporu. Daha fazla bilgi-ebilmek bulunmak bizim kısa bir süre önce madde19 ve bir dizi ilgili işleri20,21,22,23.

<table><tbody><tr><td>syringe pump&amp;nbsp;</td><td>KD Scientific</td><td>KDS-100</td><td></td></tr><tr><td>tube furnance</td><td>Lindberg/Blue M</td><td>TF55035A-1</td><td></td></tr><tr><td>ball miller</td><td>SPEX SamplePrep</td><td>5100</td><td></td></tr><tr><td>electrochemical work station</td><td>BioLogic</td><td>VMP3</td><td></td></tr><tr><td>pH meter</td><td>Orion</td><td>320 PerpHecT&amp;nbsp;</td><td>2 points calibration before use</td></tr><tr><td>gas chromatograph</td><td>Shimadzu</td><td>GC-2014</td><td>a combined seperation system consisting of molecular sieve 5A, Hayesep Q, Hayesep T, and Hayesep N</td></tr><tr><td>mass flow controller</td><td>Alicat Scientific&amp;nbsp;</td><td>MC-50SCCM-D/5M</td><td></td></tr><tr><td>ultrapure water system</td><td>Millipore</td><td>Synergy</td><td></td></tr><tr><td>vacuum desiccator&amp;nbsp;</td><td>PolyLab</td><td>55205</td><td></td></tr><tr><td>polyacrylonitrile</td><td>Sigma-Aldrich</td><td>181315</td><td>M&lt;sub&gt;w&lt;/sub&gt;=150,000</td></tr><tr><td>polypyrrolidone</td><td>Sigma-Aldrich</td><td>437190</td><td>M&lt;sub&gt;w&lt;/sub&gt;=1,300,000</td></tr><tr><td>Ni(NO&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;6H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>244074</td><td></td></tr><tr><td>dicyandiamide</td><td>Sigma-Aldrich</td><td>D76609</td><td></td></tr><tr><td>dimethylformamide</td><td>Sigma-Aldrich</td><td>227056</td><td></td></tr><tr><td>carbon fiber paper&amp;nbsp;</td><td>AvCarb</td><td>MGL370</td><td></td></tr><tr><td>Nafion 117 membrane</td><td>Fuel Cell Store</td><td>117</td><td>used as proton exchange membrane in H-cell</td></tr><tr><td>KHCO&lt;sub&gt;3&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>431583</td><td>further purified by electrolysis</td></tr><tr><td>platinum foil&amp;nbsp;</td><td>Beantown Chemical</td><td>126580</td><td></td></tr><tr><td>saturated calomel electrode</td><td>CH Instruments</td><td>CHI150</td><td></td></tr><tr><td>glassy carbon electrode</td><td>HTW GmbH</td><td>SIGRADUR</td><td>1 cm &amp;times; 2 cm</td></tr><tr><td>wax</td><td>Apiezon</td><td>W-W100</td><td></td></tr><tr><td>Nafion 117 solution</td><td>Sigma-Aldrich</td><td>70160</td><td>used as ionomer in catalyst ink preparation&amp;nbsp;</td></tr><tr><td>forming gas</td><td>Airgas</td><td>UHP</td><td>5% H&lt;sub&gt;2&lt;/sub&gt; balanced with Ar</td></tr><tr><td>carbon dioxide</td><td>Airgas</td><td>LaserPlus</td><td></td></tr><tr><td>sandard gas</td><td>Airgas</td><td>customized</td><td>500 ppm CO, 500 ppm CH&lt;sub&gt;4&lt;/sub&gt;, 1000 ppm H&lt;sub&gt;2&lt;/sub&gt; balanced with Ar</td></tr><tr><td>sandard gas</td><td>Air Liquide</td><td>customized</td><td>100 ppm H&lt;sub&gt;2&lt;/sub&gt;, 100 ppm CO and other alkanes balanced with Ar</td></tr></tbody></table>

synthesis and performance characterizations of transition metal single atom catalyst for electrochemical co2 reduction

Bu iletişim kuralı hem sentez yöntemi Ni tek atom katalizör ve katalitik aktivitesi ve seçicilik sulu CO2 azaltma içinde elektrokimyasal test sunar. Farklı geleneksel metal nanocrystals, metal tek atom sentezi tek o atomları sınırlandırmak ve önlemek onları--dan toplama bir matris malzeme içerir. Biz bir electrospinning ve tek atom ve dağınık bir grafen kabuğu olarak, co CO2 azaltılması için etkin merkezleri olarak koordine Ni hazırlamak için yöntem tavlama termal raporu. Sentez sırasında N dopants graphene boş pozisyonlar Ni atomlar yakalamak için üreten bir kritik rol oynamaktadır. Tarama transmisyon elektron mikroskobu sapmaları-düzeltilir ve üç boyutlu atom sonda tomografi grafen boş pozisyonlar tek Ni atomik Siteler'de tanımlamak için istihdam edildi. Detaylı Kurulum elektrokimyasal CO2 azaltma aygıtının bir on-line Gaz Kromatografi ile birleştiğinde de gösterdi. Metalik Ni için karşılaştırıldığında, Ni tek atom katalizör büyük ölçüde geliştirilmiş CO2 azaltma sergi ve H2 evrim yan reaksiyon bastırılır.

Elektron mikroskobu (SEM), transmisyon elektron mikroskobu (kök) ve enerji dağıtıcı x-ışını spektroskopisi (EDX) tarama tarama eşleme görüntüleri NiN-GS Morfoloji karakterizasyonu için şekil 1 ' de gösterilmektedir. Üç boyutlu atom sonda tomografi (3D-APT) sonuçları için tek Ni siteleri dağıtım hem de komşu kimyasal çevre kimlik doğrudan Şekil 2 ' de gösterilmiştir. On-line elektrokimyasal GC ölçü...

Watch this Scientific Journal Video about Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction at JoVE.com

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Sentez ve elektrokimyasal CO2 azaltılması için geçiş metalleri tek Atom katalizör performans karakterizasyonu

Burada, biz sentezi için bir iletişim kuralı mevcut ve elektrokimyasal test geçiş metalleri tek atomlarının grafen boş seçici karbon dioksit azaltılması için sulu çözümler karbon monoksit için etkin merkezleri olarak koordine.

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

synthesis-performance-characterizations-transition-metal-single-atom

Universidad de Cartagena UDEC

Research

JoVE Journal

Chemistry

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

18.0K Görüntüleme.  Harvard University. Burada, biz sentezi için bir iletişim kuralı mevcut ve elektrokimyasal test geçiş metalleri tek atomlarının grafen boş seçici karbon dioksit azaltılması için sulu çözümler karbon monoksit için etkin merkezleri olarak koordine.

Video: Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

Monometalik ve Bimetalik Erken Geçiş Metal Carbide ve Nitrür Nanopartiküller Ters Mikroemülsiyon aracılı sentezi

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

Kimya

On the Preparation and Testing of Fuel Cell Catalysts Using the Thin Film Rotating Disk Electrode Method

We present a step-by-step tutorial to prepare proton exchange membrane fuel cell (PEMFC) catalysts, consisting of Pt nanoparticles (NPs) supported on a high surface area carbon, and to test their performance in thin film rotating disk electrode (TF-RDE) measurements. The TF-RDE methodology is widely used for catalyst screening; nevertheless, the measured performance sometimes considerably differs among research groups. These uncertainties impede the advancement of new catalyst materials and, consequently, several authors discussed possible best practice methods and the importance of benchmarking.
The visual tutorial highlights possible pitfalls in the TF-RDE testing of Pt/C catalysts. A synthesis and testing protocol to assess standard Pt/C catalysts is introduced that can be used together with polycrystalline Pt disks as benchmark catalysts. In particular, this study highlights how the properties of the catalyst film on the glassy carbon (GC) electrode influence the measured performance in TF-RDE testing. To obtain thin, homogeneous catalyst films, not only the catalyst preparation, but also the ink deposition and drying procedures are essential. It is demonstrated that an adjustment of the ink&#39;s pH might be necessary, and how simple control measurements can be used to check film quality. Once reproducible TF-RDE measurements are obtained, determining the Pt loading on the catalyst support (expressed as Pt wt%) and the electrochemical surface area is necessary to normalize the determined reaction rates to either surface area or Pt mass. For the surface area determination, so-called CO stripping, or the determination of the hydrogen underpotential deposition (Hupd) charge, are standard. For the determination of the Pt loading, a straightforward and cheap procedure using digestion in aqua regia with subsequent conversion of Pt(IV) to Pt(II) and UV-vis measurements is introduced.

Preparing and testing Pt/C fuel cell catalysts is subject to continuous discussion in the scientific community with respect to reproducibility and best practice. With the presented work, we intend to present a step-by-step tutorial to make and test Pt/C catalysts, which can serve as benchmark for novel catalyst systems.

Hazırlık ve ince Film dönen Disk elektrot yöntemi kullanarak yakıt hücresi katalizörler test

We present a step-by-step tutorial to prepare proton exchange membrane fuel cell (PEMFC) catalysts, consisting of Pt nanoparticles (NPs) supported on a ...

Çevre

Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and composition of the material was characterized via powder X-ray diffraction (PXRD), M&#246;ssbauer spectroscopy (MB), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX). Two preparation methods of pentlandite bulk electrodes are presented. In the first approach a piece of synthetic pentlandite rock is directly contacted via a wire ferrule. The second approach utilizes pentlandite pellets, pressed from finely ground powder, which is immobilized in a Teflon casing. Both electrodes, whilst being prepared by an additive-free method, reveal high durability during electrocatalytic conversions in comparison to common drop-coating methods. We herein showcase the striking performance of such electrodes to accomplish the hydrogen evolution reaction (HER) and present a standardized method to evaluate the electrocatalytic performance by electrochemical and gas chromatographic methods. Furthermore, we report stability tests via potentiostatic methods at an overpotential of 0.6 V to explore the material limitations of the electrodes during electrolysis under industrial relevant conditions.

A facile preparation method of electrodes using the bulk material Fe4.5Ni4.5S8 is presented. This method provides an alternative technique to conventional electrode fabrication and describes prerequisites for unconventional electrode materials including a straightforward electrocatalytic testing method.

Elektrokatalitik Uygulamalar İçin Asal Olmayan Metal Dökme Elektrodların Hazırlanması İçin Basit Yöntemler

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

Platin-nikel Nanowires ve oksijen azaltma performansı için en iyi duruma getirme sentezi

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

Nb2O5 sentezi için kimyasal yağış yöntemi toplu nikel katalizör yüksek belirli yüzey alanı ile modifiye

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Preparation of Polyoxometalate-based Photo-responsive Membranes for the Photo-activation of Manganese Oxide Catalysts

This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic polymers, with the aim of photo-activating oxygen-evolving manganese oxide catalysts, which are important components in artificial photosynthesis. The cross-linking technique was applied to obtain a self-standing membrane with a high PW12O403- content. Incorporation and structure retention of PW12O403- within the polymer matrix were confirmed by FT-IR and micro-Raman spectroscopy, and optical characteristics were investigated by UV-Vis spectroscopy, which revealed successful construction of the metal-to-metal charge transfer (MMCT) unit. After deposition of MnOx oxygen evolving catalysts, photocurrent measurements under visible light irradiation verified the sequential charge transfer, Mn &#8594; MMCT unit &#8594; electrode, and&#160;the photocurrent intensity was consistent with the redox potential of the donor metal (Ce or Co). This method provides a new strategy for preparing integrated systems involving catalysts and photon-absorption parts for use with photo-functional materials.

Here, we present a protocol to prepare charge transfer chromophores based on a polyoxometalate/polymer composite membrane.

Mangan oksit katalizörler fotoğraf aktivasyonu için fotoğraf duyarlı membranlar Polyoxometalate tabanlı hazırlanması

This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic ...

Multiscale Sampling of a Heterogeneous Water/Metal Catalyst Interface using Density Functional Theory and Force-Field Molecular Dynamics

A significant number of heterogeneously-catalyzed chemical processes occur under liquid conditions, but simulating catalyst function under such conditions is challenging when it is necessary to include the solvent molecules. The bond breaking and forming processes modeled in these systems necessitate the use of quantum chemical methods. Since molecules in the liquid phase are under constant thermal motion, simulations must also include configurational sampling. This means that multiple configurations of liquid molecules must be simulated for each catalytic species of interest. The goal of the protocol presented here is to generate and sample trajectories of configurations of liquid water molecules around catalytic species on flat transition metal surfaces in a way that balances chemical accuracy with computational expense. Specifically, force field molecular dynamics (FFMD) simulations are used to generate configurations of liquid molecules that can subsequently be used in quantum mechanics-based methods such as density functional theory or ab initio molecular dynamics. To illustrate this, in this manuscript, the protocol is used for catalytic intermediates that could be involved in the pathway for the decomposition of glycerol (C3H8O3). The structures that are generated using FFMD are modeled in DFT in order to estimate the enthalpies of solvation of the catalytic species and to identify how H2O molecules participate in catalytic decompositions.

The goal of the protocol presented here is to generate and sample trajectories of configurations of liquid water molecules around catalytic species on a flat transition metal surface. The sampled configurations can be used as starting structures in quantum mechanics-based methods.

Türdeş olmayan su/Metal Catalyst arabirimi yoğunluğu fonksiyonel teorisi ve güç alanı moleküler dinamik kullanarak multiscale örnekleme

A significant number of heterogeneously-catalyzed chemical processes occur under liquid conditions, but simulating catalyst function under such conditions ...

Tuning the Acidity of Pt/ CNTs Catalysts for Hydrodeoxygenation of Diphenyl Ether

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid nanosheets, a series of Pt/xHMNO6/CNTs with different solid acid compositions (x = 5, 20 wt%; M = Nb, Ta; N = Mo, W) have been prepared by carbon nanotube pretreatment, protonic exchange, solid acid exfoliation, aggregation and finally Pt particles impregnation. The Pt/xHMNO6/CNTs are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and NH3-temperature programmed desorption. The study revealed that HNbWO6 nanosheets were attached on CNTs, with some edges of the nanosheets being bent in shape. The acid strength of the supported Pt catalysts increases in the following order: Pt/CNTs &#60; Pt/5HNbWO6/CNTs &#60; Pt/20HNbMoO6/CNTs &#60; Pt/20HNbWO6/CNTs &#60; Pt/20HTaWO6/CNTs. In addition, the catalytic hydroconversion of lignin-derived model compound: diphenyl ether using the synthesized Pt/20HNbWO6 catalyst has been investigated.

A protocol for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs is presented.

Difenil Eterhidrodeoksijenasyonu için Pt/ CNTs Katalizörlerinin Asitliğini Değiştirme

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid ...

Versatile CO2 Transformations into Complex Products: A One-pot Two-step Strategy

CO2 transformations using a one-pot two-step method are presented herein. The purpose of the method is to give access to a variety of value-added products and notably to generate chiral carbon centers. The crucial first step consists in the selective double hydroboration of CO2 catalyzed by an iron hydride complex. The product obtained with this 4 e- reduction is a rare bis(boryl)acetal, compound 1, which is subjected in situ to three different reactions in a second step. The first reaction concerns a condensation reaction with (diisopropyl)phenylamine affording the corresponding imine 2. In the second and third reaction, intermediate 1 reacts with triazol-5-ylidene (Enders&#39; carbene) to afford compounds 3 or 4, depending on the reaction conditions. In both compounds, C-C bonds are formed, and chiral centers are generated from CO2 as the only source of carbon. Compound 4 exhibits two chiral centers obtained in a diastereoselective manner in a formose-type mechanism. We proved that the remaining boryl fragment plays a key role in this unprecedented stereocontrol. The interest of the method stands on the reactive and versatile nature of 1, giving rise to various complex molecules from a single intermediate. The complexity of a two-step method is compensated by the overall short reaction time (2 h for the larger reaction time), and mild reaction conditions (25 &#176;C to 80 &#176;C and 1 to 3 atm of CO2).

Versatile CO2 Transformations into Complex Products: A One-pot Two-step Strategy

CO2 transformations are conducted in a one-pot two-step procedure for the synthesis of complex molecules. The selective 4 e- reduction of CO2 with a hydroborane reductant affords a reactive and versatile bis(boryl)acetal intermediate which is subsequently involved in condensation reaction or carbene-mediated C-C coupling generation.

Çok Yönlü CO2 Karmaşık Ürünlere Dönüşümler: Tek potlu İki Aşamalı Strateji

CO2 transformations using a one-pot two-step method are presented herein. The purpose of the method is to give access to a variety of value-added products ...

Synthesis of Metal Nanoparticles Supported on Carbon Nanotube with Doped Co and N Atoms and its Catalytic Applications in Hydrogen Production

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented herein. The novel strategy is based on a facile one-pot pyrolysis treatment of cobalt (II) acetylacetonate and nitrogen-rich organic precursors under Ar atmosphere at 800 &#176;C, resulting in the formation of Co- and N- co-doped carbon nanotube with earthworm-like morphology. The obtained catalyst was found to have a high density of defect sites, as confirmed by Raman spectroscopy. Here, cobalt (II) nanoparticles were stabilized on the atomically dispersed cobalt- and nitrogen-doped carbon nanotubes. The catalyst was confirmed to be effective in the catalytic hydrolysis of ammonia borane, in which the turnover frequency was 5.87 mol H2&#183;molCo-1&#183;min-1, and the specific hydrogen generation rate was determined to be 2447 mL H2&#183;gCo-1&#183;min-1. A synergistic function between the Co nanoparticle and the doped carbon nanotubes was proposed for the first time in the catalytic hydrolysis of ammonia borane reaction under a mild condition. The resulting hydrogen production with its high energy density and minimal refueling time could be suitable for future development as energy sources for mobile and stationary applications such as road trucks and forklifts in transport and logistics.

Here, we present a protocol to synthesize Co nanoparticles supported on carbon nanotubes with Co- and N- dopants for hydrogen productions.

Karbon Nanotüp Üzerinde Katkılı Co ve N Atomları ile Desteklenen Metal Nanopartiküllerin Sentezi ve Hidrojen Üretiminde Katalitik Uygulamaları

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented ...

Sentez ve elektrokimyasal CO₂ azaltılması için geçiş metalleri tek Atom katalizör performans karakterizasyonu

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