Ulusal anahtar araştırma & geliştirme Program Bakanlığı bilim ve teknoloji Çin (2016YFB0600305), Ulusal Doğa Bilimleri Foundation of China (NOS 21573031 ve 21373038), Program tarafından sağlanan mali destek minnetle anıyoruz Dalian City (2016RD09) ve teknolojik ve daha yüksek Eğitim Enstitüsü Hong Kong (THEi SG1617105 ve THEi SG1617127) mükemmel yetenekleri için.

Uyarı: Uygun işleme yöntemlerini, özelliklerini ve bu makalede açıklanan kimyasal maddelerin toksisite ilgili malzeme güvenlik bilgi formları (MSDS) bakın. Bazı kullanılan kimyasalların toksik ve kanserojen ve özel bakımları alınmalıdır. Nanomalzemeler potansiyel güvenlik tehlikesi ve sağlık etkileri oluşturabilecek. Solunum yolu ve deri temas kaçınılmalıdır. Otoklav reaktörleri ile duman hood ve katalizör performans değerlendirme katalizör sentez gerçekleştirme gibi güvenlik önlemi uygulanmalıdır. Kişisel koruyucu donanım takılmalıdır.
1. Ni0,97Nb0.03O Nb:(Ni+Nb) molar oranları 0.03 olduğu katalizörler hazırlanması
<ol><li>Niyobyum (V) oksalat hidrat 0.161 g nikel nitrat 100 ml deiyonize suyla karıştırın bar ile donatılmış bir 250 mL üç yakalı yuvarlak alt şişesi 2.821 g ile birleştirir.</li>
	<li>50 mil ve 70 ° C çözüm Isıtma manyetik karıştırıcı kullanarak çökelti kaybolması kadar bileşikleri çözülmeye karıştırın.</li>
	<li>Sıcaklığı 80 ° C 2 ° C/dk hızında için hızla artırmak.</li>
	<li>Ni/Nb çözüm pH 9.0 ulaşıncaya kadar karışık bir temel çözüm [sulu amonyum hidroksit (50 mL, 1,0 M) ve sodyum hidroksit (50 mL, 0.2 M)] dropwise reaksiyon karışım içine ekleyin.</li>
	<li>Reaksiyon karışımı karıştırarak, sıcaklığı 120 ° c 2 ° C/dk artırmak.</li>
	<li>Reaksiyon karışımı gecede 50 devirde 120 ° C'de çözüm yeşil rengini tam ortadan kaybolması kadar ilave edin.</li>
	<li>İndüktif eşleşmiş plazma optik emisyon spektrometresi (ICP-OES) çözümlemesi için kalan Ni2 + ve çözüm Nb5 + iyonu konsantrasyonu değerlendirmek ve kalan nikel tam yağış emin olmak belgili tanımlık eriyik nitrat.</li>
	<li>Katı Büchner şişesi kullanarak filtreleme tarafından toplamak. Katı art arda kalan Na+ katyon kaldırmak için 20 dakika içinde 2 lt deiyonize su ekleyerek yıkayın.</li>
	<li>Düz bir saati cam toplamak. 110 ° c kuru fırında 12 h için katı kuru.</li>
	<li>450 ° c 5 h tüp ocağı için sentetik hava (20 mL/dk O2 ve 80 mL/dk N2) halinde katı Isıtma tarafından calcine. Kullanım yüksek sıcaklıkta tepki önce hatası için tüm Züccaciye Mağazaları kontrol edin.</li>
	<li>Calcination sonra 1 g Ni0,97Nb0.03O katalizör edinin. Hood nanocrystal reaksiyon potansiyel güvenlik tehlikesi ve Nanomalzemeler sağlığa etkileri nedeniyle gerçekleştirmek için duman ve uygun koruyucu ekipman koruyucu gözlük, eldiven, önlük gibi kullanın.</li>
</ol>2. Ni0,92Nb0,08O Nb:(Ni+Nb) molar oranları için 0,08 olduğu katalizörler hazırlanması
<ol><li>Bu yordamı 1 ilk iki adımı dışında benzer:<ol>
<li>Niyobyum (V) oksalat hidrat 100 ml deiyonize su 0.43 g geçiyoruz.</li>
		<li>Ayrı ayrı, nikel nitrat 100 ml deiyonize su 2.675 g geçiyoruz.</li>
	</ol>
</li>
</ol>3. Ni0,85Nb0,15O Nb:(Ni+Nb) molar oranları için 0,15 olduğu katalizörler hazırlanması
<ol><li>Yordam 1 ilk iki adımı dışında benzer:<ol>
<li>Niyobyum (V) oksalat hidrat 100 ml deiyonize su 0,807 g geçiyoruz.</li>
		<li>Ayrı ayrı, nikel nitrat 100 ml deiyonize su 2.472 g geçiyoruz.</li>
	</ol>
</li>
</ol>4. Ni0,80Nb0,20O Nb:(Ni+Nb) molar oranı 0,20 için olduğu katalizörler hazırlanması
<ol><li>Yordam 1 ilk iki adımı dışında benzer:<ol>
<li>Niyobyum (V) oksalat hidrat 100 ml deiyonize su 1.076 g geçiyoruz.</li>
		<li>Ayrı ayrı, nikel nitrat 100 ml deiyonize su 2.326 g geçiyoruz.</li>
	</ol>
</li>
</ol>5. kimyasal yağış yöntemini kullanarak Nb2O5 hazırlanması
<ol><li>Niobic asit (Nb2O5·nH2O) O5 parçacıklar saf Nb2' yi edinmek için 450 ° c 5 h için sentetik havada calcine. Not: burada Nb2O5·nH2O Amorphous, Nb2O5 kristal x-ışını toz kırınım (XRD) analizi ile reaksiyon tamamlanması onaylayın. Analizine göre calcination 450 ° c 5 h için tepki tamamlamak için yeterliydi.</li>
</ol>6. β-O-4 lignin modeli bileşim, 2-(2-methoxyphenoxy)-1-phenylethan-1-one sentezi
<ol><li>Bromoacetophenone (9.0 g, 45 mmol) ve 2-methoxyphenol (6,6 g, 53 mmol) dimethylformamide (DMF) 500 mL konik şişesi bir manyetik karıştırıcı ile 200 ml geçiyoruz. Uygun koruyucu ekipman ve duman hood aşındırıcı ve kanserojen kimyasallar ve Kimyasalları kullanarak tepki gerçekleştirmek için kullanın.</li>
	<li>Potasyum hidroksit (3.0 g, 53 mmol) Yukarıdaki DMF çözüm mix ve karışımı bir gecede manyetik karıştırıcı kullanarak oda sıcaklığında 50 rpm'de ilave edin.</li>
	<li>Karışım çözüm H2O 200 mL ve 600 mL Dietil eter ile ürün ayıklamak (1:3, v/v) ayırma huni kullanarak. Çözüm üst Dietil eter tabakası elde edilir.</li>
	<li>Dietil eter çözüm nem absorbe MgSO4 (10 g) ekleyin. Dietil eter çözüm filtre kağıdı ve huni kullanarak elde etmek için MgSO4 filtre.</li>
	<li>Dietil eter çözüm 0,08 MPa rotary Evaporatör kullanarak düşük basınç altında kaldırıldıktan sonra kalıntı 5 ml etanol geçiyoruz.</li>
	<li>Ürün bir 10 mL ölçek Li2 için etanol solvent yavaş yavaş buharlaşır. Sarı toz olarak (11,5 g) ürün elde etmek ve ürün verimi % 90'ı bromoacetophenone üzerinde dayalı olduğunu. 1H NMR analizi, 1H NMR (DMSO): δ 3,78 (s, 3 H, ve3), 5,54 (s, 2 H CH2), 6,82-8.01 (m, 9 H, aromatik) ppm. 17
</li>
</ol>7. Hydrodeoxygenation aromatik eter Lignin kaynaklı
Not: Seçilen lignin elde edilen aromatik eter ANISOL bu deneyde ve Ni0,92Nb0,08O. kullanımı uygun koruyucu ekipman ve duman hood kanserojen reaktifler kullanarak tepki gerçekleştirmek için katalizördür.
<ol><li>50 mL paslanmaz çelik otoklav reaktör bir ısıtıcı ve bir manyetik karıştırıcı ile donatmak.</li>
	<li>Ni0,92400 ° c 2 h H2 atmosfer basınçlı kap reaktörde 2 adımda elde edilen Nb0,08O katalizör (1 g) azaltmak ve katalizör Argon (50 mL/dk) altında bir gecede passivate.</li>
	<li>ANISOL (1.1712 g, 8 wt %) içine n-decane (20 mL) kantitatif Gaz Kromatografi (GC) analiz bir iç standart olarak n-dodecane (0.2928 g, 2 wt %) kullanımı ile çözülür.</li>
	<li>Azaltılmış katalizörler (0,1 g) hızla uzun çekim hızı ile hava (< 5 dakika) önlemek için otoklav reaktör içine tanıtmak.</li>
	<li>Otoklav reaktör mühür, H2 ile art arda (3 kez, 3 MPa basınç) hava ve atmosfer basıncı tepki karisimin ortadan kaldırmak için temizle.</li>
	<li>Karıştırma hızı 700 rpm ayarlayın.</li>
	<li>2 ° C/dk 160-210 ° c sıcaklığa istenen Isıtma sonra 3 MPa otoklav reaktöre basınç ve sıfır saat noktasını ayarlayın (t = 0). Not: 160-210 ° C sıcaklık aralığı bu raporda uygundur.</li>
	<li>Daha sonra Oda sıcaklığı 10 ° C/dk karışıma hemen serin ve deoxygenated ürünleri Gaz Kromatografi Kütle seçici bulmak ile kullanarak çözümleyebilirsiniz. 17
</li>
	<li>Lignin modeli göre aşağıdaki denklemi bileşik dönüşüm belirleyin: <img alt="Equation 1" src="/files/ftp_upload/56987/56987eq1.jpg">
</li>
	<li>Ürün selectivity aşağıdaki denklemi göre belirler: <img alt="Equation 2" src="/files/ftp_upload/56987/56987eq2.jpg">
</li>
</ol>

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Res. 18 (5), 1-12 (2016).</li><li>Wang, K., Yang, L., Zhao, W., Cao, L., Sun, Z., Zhang, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+facile+synthesis+of+copper+nanoparticles+supported+on+an+ordered+mesoporous+polymer+as+an+efficient+and+stable+catalyst+for+solvent-free+sonogashira+coupling+Reactions.">A facile synthesis of copper nanoparticles supported on an ordered mesoporous polymer as an efficient and stable catalyst for solvent-free sonogashira coupling Reactions.</a> Green Chem. 19, 1949-1957 (2017).</li><li>Song, 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=High-Selectivity+Electrochemical+Conversion+of+CO2+to+Ethanol+using+a+Copper+Nanoparticle/N-Doped+Graphene+Electrode.">High-Selectivity Electrochemical Conversion of CO2 to Ethanol using a Copper Nanoparticle/N-Doped Graphene Electrode.</a> Chemistry Select. 1, 6055-6061 (2016).</li></ol>

İfşa etmek yok.

Nikel-katkılı yığın niyobyum oksit nano tanecikleri hazırlamak için yaygın yöntemlerden birini döner buharlaşma yöntemidir. 9 çeşitli basınç ve sıcaklık koşulları döner buharlaşma, Ni-Nb-O parçacıklar ticaret yağış ile solvent yavaş kaldırma işlemi sırasında istihdam ederek. Döner buharlaşma yöntemi aksine bu çalışmada bildirilen kimyasal yağış yöntemi bu gerekmez gibi solventler kaldırılması nano tanecikleri hazırlamak için artan ilgi aldı. Nanocata...

Nanokompozitlerin hazırlanması çok önemli uygulama nedeniyle artan ilgi çeşitli alanına aldı. Ni-Nb-O karışık oksit nano tanecikleri hazırlamak için gibi kuru karıştırma yöntemi,71,2,3,4,5,6 farklı yöntemler geliştirilmiştir, 8 buharlaşma yöntemi,9,10,11,12,13 sol jel yöntemi,14 termal ayrıştırma yöntemi,15 ve Auto-yanma. 16 bir tipik buharlaşma yöntem9' da metal öncüleri, uygun miktarda içeren sulu çözümler nikel nitrat hekzahidrat ve amonyum niyobyum oksalat ısıtmalı 70 ° C'de Solvent ve diğer kurutma ve calcination kaldırıldıktan sonra karışık oksit elde edildi. Bu oksit katalizörler sergi mükemmel katalitik aktivitesi ve niyobyum katyonlar NiO kafes içinde birleşme tarafından indüklenen elektronik ve yapısal düzenlenmesi ile ilgili etan oksidatif dehydrogenation (ODH) doğru seçicilik . 11 Nb ekleme etan12oksidasyon reaksiyonları için sorumludur electrophilic oksijen türleri büyük ölçüde azaltır. Sonuç olarak, bu yöntemin uzantıları karışık Ni-beni-O oksitler, farklı türde hazırlanması yapılmıştır nerede bana Li, Mg, Al, Ga, Ti ve Ta =. 13 bu metal dopants varyasyon NiO unselective ve electrophilic oksijen radikalleri alter, böylece sistematik ODH etkinlik ve seçicilik etan doğru ayarlamak bulunur. Ancak, genellikle yüzey bu oksitler nispeten alanıdır küçük (< 100 m2/g), genişletilmiş aşamasında segregasyon ve büyük Nb2O5 crystallites, oluşumu nedeniyle ve böylece onların kullandığı diğer katalitik engel uygulamaları.
Karışık oksit katalizörler hazırlamak için başka bir sık kullanılan yöntem yöntemi, katı hal taşlama yöntemi olarak da bilinir, karıştırma kurudur. Katalitik malzeme solvent içermeyen bir şekilde elde edilen, bu yöntem karışık oksit hazırlanması için umut verici bir yeşil ve sürdürülebilir alternatif sağlar. Bu yöntemle elde edilen en yüksek yüzey alanı 172 m2/g Ni80Nb20 250 ° c calcination sıcaklıkta olduğunu 8 Reaktanları iyi atom ölçeğinde karışık değil gibi Ancak, katı hal bu yöntem güvenilir değildir. Bu nedenle, kimyasal homojenliği ve belirli parçacık boyutu dağıtım ve Morfoloji daha iyi kontrol için Ni-Nb-O hazırlamak için uygun diğer yöntemleri oksit nano tanecikleri hala aranır karışık. 7
Nano tanecikleri gelişmesinde çeşitli stratejileri arasında kimyasal yağış metal iyonları tam yağış sağlar beri nanocatalysts geliştirmek için umut verici yöntemlerden birini hizmet vermektedir. Ayrıca, daha yüksek yüzey alanlarda nano tanecikleri yaygın olarak bu yöntem kullanılarak hazırlanır. Ni-Nb-O nano tanecikleri katalitik özelliklerini geliştirmek için biz burada Ni-Nb-O karışık oksit katalizörler yüksek yüzey alanı ile bir dizi sentezi için protokol kimyasal yağış yöntemi tarafından Raporu. Nb:Ni molar oranı lignin kaynaklı Organik bileşiklerin hydrodeoxygenation doğru oksitler katalitik aktivitesini belirlemede önemli bir faktör olduğunu gösterdi. 0.087 yukarıda yüksek Nb:Ni oranı ile etkin olmayan NiNb2O6 tür kuruldu. Ni0,92Nb0,08en büyük yüzey alanı (173 m2/g) vardı, O kat benzeri nanosheets yapıları sergiler ve en iyi aktivite ve seçicilik doğru ANISOL Siklokekzan için hydrodeoxygenation gösterdi.

<table>
	<tbody>
		<tr>
			<td>Niobium(V) oxalate hydrate, 98%</td>
			<td>Alfa</td>
			<td>L04481902</td>
			<td></td>
		</tr>
		<tr>
			<td>Nickel nitrate hexahydrate, 99%</td>
			<td>Aladdin</td>
			<td>N108891</td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium hydroxide, 98%</td>
			<td>Aladdin</td>
			<td>S111501</td>
			<td></td>
		</tr>
		<tr>
			<td>Ammonium hydroxide, 23-25%</td>
			<td>Aladdin</td>
			<td>A112077</td>
			<td></td>
		</tr>
		<tr>
			<td>Anisole, 99%</td>
			<td>Sinopharm</td>
			<td>81001728</td>
			<td></td>
		</tr>
		<tr>
			<td>Diphenyl ether, 98%</td>
			<td>Aladdin</td>
			<td>D110644</td>
			<td></td>
		</tr>
		<tr>
			<td>Phenol, 98%</td>
			<td>Sinopharm</td>
			<td>100153008</td>
			<td></td>
		</tr>
		<tr>
			<td>2-Methoxyphenol, 98%</td>
			<td>Sinopharm</td>
			<td>30114526</td>
			<td></td>
		</tr>
		<tr>
			<td>Vanillin, 99.5%</td>
			<td>Sinopharm</td>
			<td>69024316</td>
			<td></td>
		</tr>
		<tr>
			<td>Potassium hydroxide, AR</td>
			<td>Aladdin</td>
			<td>P112284</td>
			<td></td>
		</tr>
		<tr>
			<td>N,N-Dimethylformamide, 99.5%</td>
			<td>Sinopharm</td>
			<td>40016462</td>
			<td></td>
		</tr>
		<tr>
			<td>2-Bromoacetophenone,98%</td>
			<td>Aladdin</td>
			<td>B103328</td>
			<td></td>
		</tr>
		<tr>
			<td>Diethyl ether,99.5%</td>
			<td>Sinopharm</td>
			<td>10009318</td>
			<td></td>
		</tr>
		<tr>
			<td>Decane,98%</td>
			<td>Aladdin</td>
			<td>D105231</td>
			<td></td>
		</tr>
		<tr>
			<td>Dodecane,99%</td>
			<td>Aladdin</td>
			<td>D119697</td>
			<td></td>
		</tr>
		<tr>
			<td>Niobic acid</td>
			<td>CBMM</td>
			<td>1313968</td>
			<td></td>
		</tr>
		<tr>
			<td>Heating and Drying Oven</td>
			<td></td>
			<td></td>
			<td>DHG Series (shanghai jinghong laboratory instrument co. ltd)</td>
		</tr>
		<tr>
			<td>Autoclave Reactor</td>
			<td></td>
			<td></td>
			<td>CJF-0.05&#8212;0.1L (Dalian Tongda Equipment Technology Development Co., Ltd)</td>
		</tr>
		<tr>
			<td>Tube&#160;furnace</td>
			<td></td>
			<td></td>
			<td>SK2-1-10/12 (Luoyang Huaxulier Electric Stove Co., Ltd)</td>
		</tr>
		<tr>
			<td>Heating magnetic stirrer</td>
			<td></td>
			<td></td>
			<td>DF-101 (Yu Hua Instrument Co. Ltd.)</td>
		</tr>
		<tr>
			<td>Rotary evaporator</td>
			<td></td>
			<td></td>
			<td>RE-3000A (Shanghai Yarong Biochemical Instrument Factory)</td>
		</tr>
		<tr>
			<td>Synthetic air</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Hydrogen gas</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Argon gas</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

chemical precipitation method for the synthesis of nb2o5 modified bulk nickel catalysts with high specific surface area

Biz bir yöntemi NixNb1-xO katalizörler sünger benzeri ve kat benzeri taşınımı ile sentezi için göstermek. Nb:Ni oranı, NixNb1-xO nano tanecikleri farklı atom besteleri ile bir dizi değişen tarafından (x = 0,03 0,08, 0,15 ve 0,20) kimyasal yağış tarafından hazırlanmıştır. Bu NixNb1-xO katalizörler x-ışını kırınım, x-ışını photoelectron spektroskopisi ve tarama elektron mikroskobu ile karakterizedir. Ni0,97Nb0.03O sünger benzeri ve kat benzeri görünümünü ve Ni0,92Nb0,08O NiO yüzey ve toplu ile karşılaştırıldığında bu NixNb1-xO katalizörler büyük yüzey alanı çalışmada ortaya NiO. 173 m2/g maksimum yüzey alanı Ni0,92Nb0,08O katalizörler için elde edilebilir. Buna ek olarak, katalitik hydroconversion sentezlenmiş Ni0,92Nb0,08O katalizörler kullanarak lignin türevi bileşiklerin araştırdık.

X-ışını kırınım (XRD) desenleri (Resim 1 ve Şekil 2), bahis yüzey alanlarını, sıcaklık programlanmış azaltma ile hidrojen hidrojen (H2- TPR), elektron mikroskobu (SEM) bir enerji dağıtıcı x-ışını (EDX ile donatılmış tarama ) Çözümleyicisi, x-ışını photoelectron spektroskopisi (XPS) toplanan nano tanecikleri için NiO, Ni-Nb-O ve Nb2O5 oksitler17</...

Watch this Scientific Journal Video about Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area at JoVE.com

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

Sünger benzeri ve kat benzeri Ni1-xNbxO nano tanecikleri kimyasal yağış tarafından sentezi için bir protokol sunulmuştur.

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 ...

chemical-precipitation-method-for-synthesis-nb2o5-modified-bulk

Research

JoVE Journal

Chemistry

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

11.7K Görüntüleme.  Dalian University of Technology. Sünger benzeri ve kat benzeri Ni1-xNbxO nano tanecikleri kimyasal yağış tarafından sentezi için bir protokol sunulmuştur.

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

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, have high porosity, high surface-to-volume and strength-to-weight ratio. Unfortunately, common approaches for preparation of metallic nanostructures render materials with highly disordered architecture, which might have an adverse effect on their mechanical properties. Block copolymers have the ability to self-assemble into ordered nanostructures and can be applied as templates for the preparation of well-ordered metal nanofoams. Here we describe the application of a block copolymer-based supramolecular complex - polystyrene-block-poly(4-vinylpyridine)(pentadecylphenol) PS-b-P4VP(PDP) - as a precursor for well-ordered nickel nanofoam. The supramolecular complexes exhibit a phase behavior similar to conventional block copolymers and can self-assemble into the bicontinuous gyroid morphology with two PS networks placed in a P4VP(PDP) matrix. PDP can be dissolved in ethanol leading to the formation of a porous structure that can be backfilled with metal. Using electroless plating technique, nickel can be inserted into the template&#39;s channels. Finally, the remaining polymer can be removed via pyrolysis from the polymer/inorganic nanohybrid resulting in nanoporous nickel foam with inverse gyroid morphology.

This article describes the preparation of well-ordered nickel nanofoams via electroless metal deposition onto nanoporous templates obtained from self-assembled diblock copolymer based supramolecules.

Buradaki iki bloklu kopolimer Supramolecules ikinci Gyroid Nikel Nanoyapılar

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

Kimya

A Method to Manipulate Surface Tension of a Liquid Metal via Surface Oxidation and Reduction

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where interfacial tension is a dominant force. A variety of methods exist for controlling the interfacial tension of aqueous and organic liquids on this scale; however, these techniques have limited utility for liquid metals due to their large interfacial tension.
Liquid metals can form soft, stretchable, and shape-reconfigurable components in electronic and electromagnetic devices. Although it is possible to manipulate these fluids via mechanical methods (e.g., pumping), electrical methods are easier to miniaturize, control, and implement. However, most electrical techniques have their own constraints: electrowetting-on-dielectric requires large (kV) potentials for modest actuation, electrocapillarity can affect relatively small changes in the interfacial tension, and continuous electrowetting is limited to plugs of the liquid metal in capillaries.
Here, we present a method for actuating gallium and gallium-based liquid metal alloys via an electrochemical surface reaction. Controlling the electrochemical potential on the surface of the liquid metal in electrolyte rapidly and reversibly changes the interfacial tension by over two orders of magnitude ( &#820;500 mN/m to near zero). Furthermore, this method requires only a very modest potential (&#60; 1 V) applied relative to a counter electrode. The resulting change in tension is due primarily to the electrochemical deposition of a surface oxide layer, which acts as a surfactant; removal of the oxide increases the interfacial tension, and vice versa. This technique can be applied in a wide variety of electrolytes and is independent of the substrate on which it rests.

We present a method to control the interfacial energy of a liquid metal in an electrolyte via electrochemical deposition (or removal) of a surface oxide layer. This simple method can control the capillary behavior of gallium-based liquid metals by tuning the interfacial energy rapidly, significantly, and reversibly using modest voltages.

Bir Yöntem Yüzey Oksidasyon ve İndirgeme yoluyla Sıvı Metal Yüzey Gerilim işleyin

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where ...

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of trifluoromethoxylated aromatic compounds remains a formidable challenge in organic synthesis. Conventional approaches often suffer from poor substrate scope, or require use of highly toxic, difficult-to-handle, and/or thermally labile reagents. Herein, we report a user-friendly protocol for the synthesis of methyl 4-acetamido-3-(trifluoromethoxy)benzoate using 1-trifluoromethyl-1,2-benziodoxol-3(1H)-one (Togni reagent II). Treating methyl 4-(N-hydroxyacetamido)benzoate (1a) with Togni reagent II in the presence of a catalytic amount of cesium carbonate (Cs2CO3) in chloroform at RT afforded methyl 4-(N-(trifluoromethoxy)acetamido)benzoate (2a). This intermediate was then converted to the final product methyl 4-acetamido-3-(trifluoromethoxy)benzoate (3a) in nitromethane at 120 &#176;C. This procedure is general and can be applied to the synthesis of a broad spectrum of ortho-trifluoromethoxylated aniline derivatives, which could serve as useful synthetic building blocks for the discovery and development of new pharmaceuticals, agrochemicals, and functional materials.

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

An operationally simple procedure for the synthesis of ortho-trifluoromethoxylated aniline derivatives via a two-step sequence of O-trifluoromethylation of N-aryl-N-hydroxyacetamide followed by thermally induced intramolecular OCF3-migration is reported.

Sentezi İçin Protokol<em&gt; Ortho</em&gt; -trifluoromethoxylated Anilin türevleri

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of ...

Facile Synthesis of Worm-like Micelles by Visible Light Mediated Dispersion Polymerization Using Photoredox Catalyst

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins with the synthesis of a hydrophilic poly(oligo(ethylene glycol) methyl ether methacrylate) (POEGMA) homopolymer using reversible addition-fragmentation chain-transfer (RAFT) polymerization. Under mild visible light irradiation (&#955; = 460 nm, 0.7 mW/cm2), this macro-chain transfer agent (macro-CTA) in the presence of a ruthenium based photoredox catalyst, Ru(bpy)3Cl2 can be chain extended with a second monomer to form a well-defined block copolymer in a process known as Photoinduced Electron Transfer RAFT (PET-RAFT). When PET-RAFT is used to chain extend POEGMA with benzyl methacrylate (BzMA) in ethanol (EtOH), polymeric nanoparticles with different morphologies are formed in situ according to a polymerization-induced self-assembly (PISA) mechanism. Self-assembly into nanoparticles presenting POEGMA chains at the corona and poly(benzyl methacrylate) (PBzMA) chains in the core occurs in situ due to the growing insolubility of the PBzMA block in ethanol. Interestingly, the formation of highly pure worm-like micelles can be readily monitored by observing the onset of a highly viscous gel in situ due to nanoparticle entanglements occurring during the polymerization. This process thereby allows for a more reproducible synthesis of worm-like micelles simply by monitoring the solution viscosity during the course of the polymerization. In addition, the light stimulus can be intermittently applied in an ON/OFF manner demonstrating temporal control over the nanoparticle morphology.

This article describes a process for producing polymeric self-assembled nanoparticles using visible light mediated dispersion polymerization. Using low energy visible light to control the polymerization allows for the reproducible formation of self-assembled worm-like micelles at high solids content.

Photoredox Katalizörü kullanarak görünür ışık aracılığı ile dispersiyon polimerleştirilmesi ile solucan gibi miseller Facile sentezi

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins ...

Synthesis and Testing of Supported Pt-Cu Solid Solution Nanoparticle Catalysts for Propane Dehydrogenation

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are demonstrated here. The catalyst forms a substitutional solid solution structure, with a small and uniform particle size around 2 nm. This is realized by careful control over the impregnation, calcination, and reduction steps during catalyst preparation and is identified by advanced in situ synchrotron techniques. The catalyst propane dehydrogenation performance continuously improves with increasing Cu:Pt atomic ratio.

A convenient method for the synthesis of 2 nm supported bimetallic nanoparticle Pt-Cu catalysts for propane dehydrogenation is reported here. In situ synchrotron X-ray techniques allow for the determination of the catalyst structure, which is typically unobtainable using laboratory instruments.

Propan Dehidrojenasyon için Desteklenen Pt-Cu Katı Solüsyon Nanopartikül Katalizörlerinin Sentezi ve Testi

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are ...

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 ...

Synthesis of a Thiol Building Block for the Crystallization of a Semiconducting Gyroidal Metal-sulfur Framework

We present a method for preparing thioester molecules as the masked form of the thiol linkers and their utilization for accessing a semiconducting and porous metal-dithiolene network in the highly ordered single crystalline state. Unlike the highly reactive free-standing thiols, which tend to decompose and complicate the crystallization of metal-thiolate open frameworks, the thioester reacts in situ to provide the thiol species, serving to mitigate the reaction between the mercaptan units and the metal centers, and to improve crystallization consequently. Specifically, the thioester was synthesized in a one-pot procedure: an aromatic bromide (hexabromotriphenylene) reacted with excess sodium thiomethoxide under vigorous conditions to first form the thioether intermediate product. The thioether was then demethylated by the excess thiomethoxide to provide the thiolate anion that was acylated to form the thioester product. The thioester was conveniently purified by standard column chromatography, and then used directly in the framework synthesis, wherein NaOH and ethylenediamine serve to revert in situ the thioester to the thiol linker for assembling the single-crystalline Pb(II)-dithiolene network. Compared with other methods for thiol synthesis (e.g., by cleaving alkyl thioether using sodium metal and liquid ammonia), the thioester synthesis here uses simple conditions and economical reagents. Moreover, the thioester product is stable and can be conveniently handled and stored. More importantly, in contrast to the generic difficulty in accessing crystalline metal-thiolate open frameworks, we demonstrate that using the thioester for in situ formation of the thiol linker greatly improves the crystallinity of the solid-state product. We intend to encourage broader research efforts on the technologically important metal-sulfur frameworks by disclosing the synthetic protocol for the thioester as well as the crystalline framework solid.

Here, we present a one-pot, transition-metal-free synthesis of thiols and thioesters from aromatic halides and sodium thiomethoxide, followed by the preparation of single crystals of a metal-dithiolene network using thiol species generated in situ from the more stable and tractable thioester.

Bir yarıiletken Gyroidal Metal-kükürt çerçeve kristalleşme için Thiol yapı taşı sentezi

We present a method for preparing thioester molecules as the masked form of the thiol linkers and their utilization for accessing a semiconducting and ...

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

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

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

Substrat bağlı Au Nanowires bir aktif yüzey büyüme mekanizması yoluyla sentezi

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

Synthesis and Characterization of 1,2-Dithiolane Modified Self-Assembling Peptides

This report focuses on the synthesis of an N-terminus 1,2-dithiolane modified self-assembling peptide and the characterization of the resulting self-assembled supramolecular structures. The synthetic route takes advantage of solid-phase peptide synthesis with the on-resin coupling of the dithiolane precursor molecule, 3-(acetylthio)-2-(acetylthiomethyl)propanoic acid, and the microwave-assisted thioacetate deprotection of the peptide N-terminus before final cleavage from the resin to yield the 1,2-dithiolane modified peptide. After the high-performance liquid chromatography (HPLC) purification of the 1,2-dithiolane peptide, derived from the nucleating core of the A&#946; peptide associated with Alzheimer&#39;s disease, the peptide is shown to self-assemble into cross-&#946; amyloid fibers. Protocols to characterize the amyloid fibers by Fourier-transform infrared spectroscopy (FT-IR), circular dichroism spectroscopy (CD) and transmission electron microscopy (TEM) are presented. The methods of N-terminal modification with a 1,2-dithiolane moiety to well-characterized self-assembling peptides can now be explored as model systems to develop post-assembly modification strategies and explore dynamic covalent chemistry on supramolecular peptide nanofiber surfaces.

A protocol for the synthesis of a 1,2-dithiolane modified peptide and the characterization of the supramolecular structures resulting from the peptide self-assembly.

1,2-Dithiolane malzemelerin ve kendi kendine montaj peptidler değiştirilme tarihi

This report focuses on the synthesis of an N-terminus 1,2-dithiolane modified self-assembling peptide and the characterization of the resulting ...

Synthesis and Bioconjugation of Thiol-Reactive Reagents for the Creation of Site-Selectively Modified Immunoconjugates

Maleimide-bearing bifunctional probes have been employed for decades for the site-selective modification of thiols in biomolecules, especially antibodies. Yet maleimide-based conjugates display limited stability in vivo because the succinimidyl thioether linkage can undergo a retro-Michael reaction. This, of course, can lead to the release of the radioactive payload or its exchange with thiol-bearing biomolecules in circulation. Both of these processes can produce elevated activity concentrations in healthy organs as well as decreased activity concentrations in target tissues, resulting in reduced imaging contrast and lower therapeutic ratios. In 2018, we reported the creation of a modular, stable, and easily accessible phenyloxadiazolyl methyl sulfone reagent &#8212; dubbed &#8216;PODS&#8217; &#8212; as a platform for thiol-based bioconjugations. We have clearly demonstrated that PODS-based site-selective bioconjugations reproducibly and robustly create homogenous, well-defined, highly immunoreactive, and highly stable radioimmunoconjugates. Furthermore, preclinical experiments in murine models of colorectal cancer have shown that these site-selectively labeled radioimmunoconjugates exhibit far superior in vivo performance compared to radiolabeled antibodies synthesized via maleimide-based conjugations. In this protocol, we will describe the four-step synthesis of PODS, the creation of a bifunctional PODS-bearing variant of the ubiquitous chelator DOTA (PODS-DOTA), and the conjugation of PODS-DOTA to the HER2-targeting antibody trastuzumab.

In this protocol, we will describe the synthesis of PODS, a phenyoxadiazolyl methyl sulfone-based reagent for the site-selective attachment of cargos to the thiols of biomolecules, particularly antibodies. In addition, we will describe the synthesis and characterization of a PODS-bearing bifunctional chelator and its conjugation to a model antibody.

Sentez ve Site seçici olarak oluşturulması için Thiol reaktif reaktif Bioconjugation Immunoconjugates modifiye

Maleimide-bearing bifunctional probes have been employed for decades for the site-selective modification of thiols in biomolecules, especially antibodies. ...