Dr. B.P.S. Chauhan would like to gratefully acknowledge William Paterson University for assigned release time (ART) award for part of the research described here and also for the research program in general.

Not: daha fazla saflaştırılmadan bir üreticiden olduğu gibi tüm reaktifler kullanılır. Reaksiyonlar tamamlandıktan azalma sağlamak için, UV-Vis spektroskopisi yoluyla en fazla bir hafta izlenmiştir. Tüm reaksiyonlar bir havalandırma başlık altında yürütülmektedir ve uygun güvenlik kıyafetleri eldiven, göz gözlük ve laboratuvar kat dahil olmak üzere tüm zamanlarında giyilir. Gümüş Nanopartiküller 1. Sentezi <ol><li> 50 ml&#39;lik bir Erlenmeyer şişesi içine doğrudan gümüş nitrat 0.0169 g (0.1 mmol) tartılır. </li><li> ultra saf su MQ ve manyetik bir karıştırıcı çubuğu 18.2, 20 ml ekle. buharlaşmasını önlemek için tapa ile şişeyi örtün. </li><li> Bir yağ banyosu içinde yer şişe bir karıştırıcısı / hot plate üzerine alan ve bu sıcaklık 60 ° C&#39;de muhafaza edilir sağlar. </li><li> Yavaş yavaş hassas bir mikropipet kullanılarak 2-AST 144 ul (0.2 mmol) ekleyin. Tüm silan sağlamak için çözelti içinde gömme pipet birkaç kez çözeltiye aktarılır. </li><li> UV-Vis spektroskopisi okumaları alınBölüm 5&#39;de listelenen protokole göre. </li><li> 6 saat sonra, yağ banyosundan örneği kaldırmak ve depolama, TEM, FTIR ve daha fazla analiz için 20 ml&#39;lik bir numune şişesine transfer et. Not: altın ve paladyum nanopartiküllerinin sentezi 216 ul (0.3 mmol) 2-AST gerektiren altın nanopartiküllerinin dışında aynı yöntem kullanılır ve stokiyometrik miktarda izler. Reaksiyon, 2 hafta boyunca nanopartiküller üretmek için devam edebilir, ancak kuru bir protokol düşünülebilir önemli değildir. </li></ol> 2. Transmisyon Elektron Mikroskobu (TEM) Numune Hazırlama <ol><li> Bu örnek, oda sıcaklığına kadar soğutuldu sahip olduğundan emin olun. </li><li> filtre kağıdı temiz parça üzerine bir 200 C-gözenekli formvar kaplı bakır ızgara yerleştirin. </li><li> 1 ml plastik Pasteur pipeti, dökme damla doğrudan ızgara üzerine nanoparçacık numune yaklaşık 60 ul kullanma. </li><li> ızgara görüntüleme önce 24 saat kurumasını bekleyin. </li><li> aşağıdaki koşullar ile yüksek çözünürlüklü TEM görüntüleri çekmek:10 uA akım ve gerilim 22 hızlanan 100 kV. </li></ol> 3. Nükleer Manyetik Rezonans (NMR) Numune Hazırlama Not: oda sıcaklığında NMR gerçekleştirin. Yüksek sıcaklıklarda sinyaller elde edilen spektrumları kalitesini düşüren, hangi kaynasabilir. <ol><li> Hassas pipet, pipet temiz bir NMR tüpü içine döteryum dioksit (D 2 O) 50 ul kullanma. </li><li> temiz başka hassas pipet ile, pipet aynı NMR tüpe nanoparçacık örnek 400 ul. <ol><li> Örnekler NMR tüpü iç duvarlarına bağlı gibi, yavaş NMR tüpü içine çözüm ekleyin. Örnek uymak yoksa, tüp kap ve alt çözüm zorlamak için tüpün üst sallayın. </li></ol></li><li> NMR tersini tüp defalarca sallayarak tarafından örnek karıştırın. </li><li> üretici tarafından sağlanan NMR protokolü tarafından belirlenen yönergeleri izleyerek NMR içine yerleştirin örnek tüpü. 1000 taramaların bir yukarı doğru res için gerekli olabilirBir 1H Proton NMR darbe programında züm. Not: NMR tüp duvarları temiz olmalıdır. Borunun dış duvarı önce spektrumları netlik için analize bir mikrofiber veya bezle silinmesi tavsiye edilir. </li><li> Bittiğinde örnek atın. Üst çözümüne örnek iade etmeyin. </li></ol> 4. Fourier Infrared (FTIR) Spektroskopisi Numune Hazırlama Transform <ol><li> Küçük bir cam kap içine nanopartikül örnek 2 ml yerleştirin. Bir 3 mi borusu ya da 1 dirhemlik cam şişe iyi çalışır. </li><li> Bir durdurma musluğu takılmış bir vakum kurutucu içinde cam kap yerleştirerek örnekleri kurutun. </li><li> Vakum pompası cihazına desikatörde takın. Numunelerin Kurutma vakum gücüne bağlı olarak birkaç saat sürebilir. kapta hiçbir görünür bir sıvı olduğunu sonra düşünün numuneler kurulayın. </li><li> Temiz bir spatula ile örnek aşağı Pençe ve katı malzemeler toplamak. </li><li> Bir ZnSe cryst ile donatılmış ATR-FTIR spectroscope üzerine katı malzemeyi yerleştirinal diyot lazer. </li><li> 4,000-500 cm arasında 32 tarama entegre FTIR spektrumları elde -1 2.0 bir spektral çözünürlükle. Hava arka plan 23 kullanın. </li></ol> 5. UV-Vis Spektroskopisi Numune Hazırlama <ol><li> doygunluk spektrometre analizi oluşmaz, böylece su nanopartikül örnek bir ila on seyreltme nanopartikül örnekleri üzerinde UV-Vis spektroskopisi yürütün. </li><li> Reaksiyon yarım saat aralıklarla çalışırken UV-Vis nanoparçacık örnekleri kaldırın. </li><li> hassas bir pipet kullanarak, nanopartikül malzeme 100 ul çıkarın ve bir plastik küvet içine yerleştirin. </li><li> Aynı küvete ultra saf su 1 ml ekleyin ve pipet birkaç kez yıkama ile iyice karıştırın. </li><li> 250-800 nm arasında rekor UV-Vis absorbans spektrumu. </li><li> Analizden sonra, reaksiyona örnek dönmez. uygun bir şekilde analitin imha edin. </li></ol>

<ol>
	<li>Corriu, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Organosilicon+Chemistry+and+Nanoscience.">Organosilicon Chemistry and Nanoscience.</a> J Organomet Chem. 686, 32-41 (2003).</li><li>Chou, L. Y., Ming, K., Chan, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Strategies+for+the+intracellular+delivery+of+nanoparticles.">Strategies for the intracellular delivery of nanoparticles.</a> Chem. Soc. Rev. 40 (1), 233-245 (2011).</li><li>Richards, R., B&#246;nnemann, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthetic+Approaches+to+Metallic+Nanomaterials.">Synthetic Approaches to Metallic Nanomaterials.</a> Nanofabrication towards Biomedical Applications. , 4-9 (2005).</li><li>Bradley, J., Schmid, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chapter+6,+Unit+6.2.2,+The+Chemistry+of+Transition+Metal+Colloids:+Synthetic+Methods+for+the+Preparation+of+Colloidal+Transition+Metals.">Chapter 6, Unit 6.2.2, The Chemistry of Transition Metal Colloids: Synthetic Methods for the Preparation of Colloidal Transition Metals.</a> Clusters and Colloids. , 469-473 (1994).</li><li>Paterer, 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=Investigation+on+the+formation+of+copper+zinc+tin+sulphide+nanoparticles+from+metal+salts+and+dodecanethiol.">Investigation on the formation of copper zinc tin sulphide nanoparticles from metal salts and dodecanethiol.</a> Mater. Chem. Phys. 149-150, 94-98 (2015).</li><li>Yi, D. K., Lee, S. S., Ying, J. Y. <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+Applications+of+Magnetic+Nanocomposite+Catalysts.">Synthesis and Applications of Magnetic Nanocomposite Catalysts.</a> Chem. Mater. 18, 2459-2461 (2006).</li><li>Piepenbrock, M. M., Lloyd, G. O., Clarke, N., Steed, J. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Metal-+and+Anion-Binding+Supramolecular+Gels.">Metal- and Anion-Binding Supramolecular Gels.</a> Chem. Rev. 110, 1960-2004 (2010).</li><li>Wu, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+and+Structural+Characterization+of+Novel+Nanohybrids+by+Cationic+3D+Silica+Nanoparticles+Sandwiched+between+2D+Anionic+Montmorillonite+Clay+through+Electrostatic+Attraction.">Preparation and Structural Characterization of Novel Nanohybrids by Cationic 3D Silica Nanoparticles Sandwiched between 2D Anionic Montmorillonite Clay through Electrostatic Attraction.</a> J. Phys. Chem. C. 113 (30), 13036-13044 (2009).</li><li>Spitalsky, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Carbon+nanotube-polymer+composites:+Chemistry,+Processing,+Mechanical+and+Electrical+Properties.">Carbon nanotube-polymer composites: Chemistry, Processing, Mechanical and Electrical Properties.</a> Prog. Polym. Sci. 35, 357-401 (2010).</li><li>Link, S., El-Sayed, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spectral+Properties+and+Relaxation+Dynamics+of+Surface+Plasmon+Electronic+Oscillations+in+Gold+and+Silver+Nanodots+and+Nanorods.">Spectral Properties and Relaxation Dynamics of Surface Plasmon Electronic Oscillations in Gold and Silver Nanodots and Nanorods.</a> J. Phys. Chem. B. 103 (40), 8410-8426 (1999).</li><li>Fau, 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=Monitoring+the+Coordination+of+Amine+Ligands+on+Silver+Nanoparticles+Using+NMR+and+SERS.">Monitoring the Coordination of Amine Ligands on Silver Nanoparticles Using NMR and SERS.</a> Langmuir. 31 (4), 1362-1367 (2015).</li><li>Patil, H. B., Borse, S. V., Patil, D. R., Patil, U. K., Patil, H. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+silver+nanoparticles+by+microbial+method+and+their+characterization.">Synthesis of silver nanoparticles by microbial method and their characterization.</a> Arch. Phys. Res. 2 (3), 153-158 (2011).</li><li>Ghosh, S., Sarma, N., Mandal, M., Kundu, S., Esumi, K., Pal, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evolution+of+gold+nanoparticles+in+micelle+by+UV-irradiation:+A+conductometric+study.">Evolution of gold nanoparticles in micelle by UV-irradiation: A conductometric study.</a> Curr. Sci. 84 (6), 791-795 (2003).</li><li>Paul, B., Bhuyan, B., Purkayastha, D. D., Dey, M., Dhar, S. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Green+synthesis+of+gold+nanoparticles+using+Pogestemon+benghalensis+(B)+O.+Ktz+leaf+extract+and+studies+of+their+photocatalytic+activity+in+degradation+of+methylene.">Green synthesis of gold nanoparticles using Pogestemon benghalensis (B) O. Ktz leaf extract and studies of their photocatalytic activity in degradation of methylene.</a> Mater. Lett. 148, 37-40 (2015).</li><li>Chauhan, B. P. S., Rathore, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Regioselective+Synthesis+of+Multifunctional+Hybrid+Polysiloxanes+Achieved+by+Pt-Nanocluster+Catalysis.">Regioselective Synthesis of Multifunctional Hybrid Polysiloxanes Achieved by Pt-Nanocluster Catalysis.</a> J. Am. Chem. Soc. 127, 5790-5791 (2005).</li><li>Chauhan, B. P. S., Rathore, S., Bandoo, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=&#34;Polysiloxane-Pd&#34;+Nanocomposites+as+Recyclable+Chemoselective+Hydrogenation+Catalysts.">&#34;Polysiloxane-Pd&#34; Nanocomposites as Recyclable Chemoselective Hydrogenation Catalysts.</a> J. Am. Chem. Soc. 126, 8493-8500 (2004).</li><li>Chauhan, B. P. S., Rathore, S., Chauhan, M., Krawicz, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+Polysiloxane+Stabilized+Palladium+Colloids+and+Evidence+of+Their+Participation+in+Silaesterification+Reactions.">Synthesis of Polysiloxane Stabilized Palladium Colloids and Evidence of Their Participation in Silaesterification Reactions.</a> J. Am. Chem. Soc. 125, 2876-2877 (2003).</li><li>Chauhan, B. P. S., Sardar, R., Tewari, P., Sharma, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> , 23-25 (2003).</li><li>Pouchert, C. J., Pouchert, C. .. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Non-Aromatic+Amines.">Non-Aromatic Amines.</a> The Aldrich Library of Infrared Spectra. , (1983).</li><li>Arkles, B., 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=Infrared+Analysis+of+Organosilicon+Compounds:+Spectra-Structure+Correlations.">Infrared Analysis of Organosilicon Compounds: Spectra-Structure Correlations.</a> Silicon Compounds Register and Review. , (1987).</li><li>Corriu, R. J. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hypervalent+Species+of+Silicon-structure+and+Reactivity.">Hypervalent Species of Silicon-structure and Reactivity.</a> J. Organomet. Chem. 400, 81-106 (1990).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Basic Instruction Manual: Hitachi HT7700 TEM. , 1-28 (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> OMNIC User's Guide Version 7.3: Thermo Electron Corporation. , 151-216 (2006).</li></ol>

Çakışan mali çıkarları vardır.

Bu yazıda bildirilen tuzlar o metalden test edildi ancak tuzlardır. Bunun bir sonucu olarak, bu reaksiyon, bir strateji metallerin tüm tuzlar, özellikle de altın çalışmak olduğu belirsizdir. bu tuzların su içinde çözünürlüğü, bu reaksiyon süresi, morfoloji ve verimi açısından reaksiyon sonuçlarını etkileyebilir. Tüm reaksiyonlar, silan önceden eritilmiş metal tuzu solüsyonuna ilave edildi. Bu reaksiyonlar higroskopik veya 18 eriyip olabilir metal tuzla...

talep ve tasarımcı nano artar uygulamaları, böylece sentez çeşitli yöntemler yapmak. Böyle lazer ablasyon veya kimyasal aşındırma olarak &quot;yukarıdan aşağıya&quot; yöntemleri, onların mükemmel kontrol edilebilirlik ve güvenilir alt mikron seviyesine kadar malzeme çözme yeteneği için kullanılmıştır. Bu yöntemler, istenen nano boyutu azaldıkça, tipik olarak üretim maliyetini arttıracaktır ince parçaların işlendikten dökme malzeme kullanır. Buna sentez alternatif bir yöntem moleküler düzeyde sentezini kontrol eder ve istenen nano kurar &quot;aşağıdan yukarıya&quot; yaklaşımıdır. Bu durum, bu nano yapılı malzemelerin 1 nesil istenen öz-montaj, fonksiyonellik, pasiflik ve istikrarına bir kontrol önemli derecede kazandırır. Moleküler seviyede çalışarak, hibrid nanokompozitler aynı birleşik yapılarda olan her iki malzemenin fayda sağlayan oluşturulabiliryeniden. Nano aşağıdan yukarıya strateji ile sentezlenir gibi yöntemler partikül büyüklüğü, şekli, doku, hidrofobiklik, porozite, ücret ve işlevsellik 2 kontrol istihdam edilmesi gerekir. Metal temel nanopartikül sentezi, başlangıç ​​metal tuzu daha sonra diğer parçacık çekirdeklenmesinin doğrudan sıfır değerlikli parçacıkları üretmek için bir otokatalitik işlemde azalır. Bu kümeleme yol açar ve nihayet nanoparçacık üretimi 3. Oluşturulan nanopartiküllerin büyüklüğü kontrol çözeltiden çökmesini önlemek amacıyla, bu tür ligandlar, yüzey aktif maddeler, iyonik şarj ve büyük polimerler stabilize fazla yığılma 4-10 den nano-tanecikleri bloke etme yetenekleri açısından yararlanılmaktadır. Bu malzemeler nedeniyle büyük grupların varlığı veya sterik iğrenmeyle 3 boyunca, sterik engelleme yoluyla, ya da nanopartiküllerin van der Waals çekimi inhibe eder. tçalışmaları, silan kullanılarak, çeşitli metal çekirdek nanopartiküllerin üretimi için, basit bir, tek kaplı bir sentetik strateji, N- (2-aminoetil) -3-aminosilanetriol (2-AST) (Şekil 1) sunulmuştur. Bu bileşik üzerinde ligandlar, nispeten yüksek bir etki ile, metal nano-tanecikleri, metal öncülleri azaltılması ve stabilize edebilmektedir. Bu üç silanol yarımları da çapraz bağlama yeteneğine sahip olan ve matris (Şekil 2) olan nanopartiküller ile emprenye organosilan polimerin birbirine ağı oluşturur. Suda mevcudiyetinde hidrolize çok silanlar, farklı olarak, bu bileşik, hidrofobisite amacıyla, stabilite, ve kontrol için yararlı olan su içinde stabilize edilir.

<table><tbody><tr><td>n-(2-aminoethyl)-3-aminosilanetriol (2-AST)</td><td>Gelest</td><td>SIA0590.0</td><td>25% in H&lt;sub&gt;2&lt;/sub&gt;O</td></tr><tr><td>Silver nitrate</td><td>Sigma Aldrich</td><td>S6506</td><td></td></tr><tr><td>Gold(III) chloride trihydrate</td><td>Sigma Aldrich</td><td>520918</td><td></td></tr><tr><td>Palladium(II) Nitrate</td><td>Alfa Aesar</td><td>11035</td><td></td></tr><tr><td>Deuterium Dioxide</td><td>Cambridge Isotope Laboratories</td><td>DLM-4-100</td><td></td></tr></tbody></table>

generation of zerovalent metal core nanoparticles using n-(2-aminoethyl)-3-aminosilanetriol

In this work, a facile one-pot reaction for the formation of metal nanoparticles in a water solution through the use of n-(2-aminoethyl)-3-aminosilanetriol is presented. This compound can be used to effectively reduce and complex metal salts into metal core nanoparticles coated with the compound. By controlling the concentrations of salt and silane one is able to control reaction rates, particle size, and nanoparticle coating. The effects of these changes were characterized through transmission electron microscopy (TEM), UV-Vis spectrometry (UV-Vis), Nuclear Magnetic Resonance spectroscopy (NMR) and Fourier Transform Infrared spectroscopy (FTIR). A unique aspect to this reaction is that usually silanes hydrolyze and cross-link in water; however, in this system the silane is water-soluble and stable. It is known that silicon and amino moieties can form complexes with metal salts. The silicon is known to extend its coordination sphere to form penta- or hexa-coordinated species. Furthermore, the silanol group can undergo hydrolysis to form a Si-O-Si silica network, thereby transforming the metal nanoparticles into a functionalized nanocomposites.

nanoparçacık oluşumu her metal nanoparçacık için karakteristik zirveleri üretmek gerektiği gibi reaksiyon UV-Vis spektrometresi ile takip edildi. Sentezlenen malzemelerin son tahlilde TEM ve FTIR ile gerçekleştirildi. FTIR spektrumu örneklerinin kuru toz elde edildi. Partikül büyüklüğü analizi TEM ve ortalama sonuçları ile elde edilen görüntü ile ilgili nanopartikül çapının ölçülmesiyle gerçekleştirilebilmektedir. <p class="jove_content" fo:keep-togethe...

Watch this Scientific Journal Video about Generation of Zerovalent Metal Core Nanoparticles Using n-2-aminoethyl-3-aminosilanetriol at JoVE.com

Generation of Zerovalent Metal Core Nanoparticles Using n-2-aminoethyl-3-aminosilanetriol

A novel method for metal core nanoparticle synthesis using a water stable silanol is described.

Sıfır değerlikli metal çekirdek Nanopartiküller Üretimi N- (2-aminoetil) -3-aminosilanetriol

In this work, a facile one-pot reaction for the formation of metal nanoparticles in a water solution through the use of ...

generation-zerovalent-metal-core-nanoparticles-using-n-2-aminoethyl-3

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Generation of Zerovalent Metal Core Nanoparticles Using n-(2-aminoethyl)-3-aminosilanetriol

7.6K Görüntüleme.  William Paterson University. A novel method for metal core nanoparticle synthesis using a water stable silanol is described.

Video: Generation of Zerovalent Metal Core Nanoparticles Using n-2-aminoethyl-3-aminosilanetriol

Using Polystyrene-block-poly(acrylic acid)-coated Metal Nanoparticles as Monomers for Their Homo- and Co-polymerization

We present a template-free method for &#8220;polymerizing&#8221; nanoparticles into long chains without side branches. A variety of nanoparticles are encapsulated in polystyrene-block-poly(acrylic acid) (PSPAA) shells and then used as monomers for their self-assembly. Spherical PSPAA micelles upon acid treatment are known to assemble into cylindrical micelles. Exploiting this tendency, the core-shell nanoparticles are induced to aggregate, coalesce, and then transform into long chains. When more than one type of nanoparticles are used, random and block &#8220;copolymers&#8221; of nanoparticles can be obtained. Detailed procedures are reported for the PSPAA encapsulation of nanoparticles, homo- and co-polymerization of the core-shell nanoparticles, separation and purification of the resulting nanoparticle chains. Transformations of single-line chains into double- and triple-line chains are also presented. The synergy between the polymer shell and the embedded nanoparticles leads to an unusual chain-growth polymerization mode, giving long nanoparticle chains that are distinct from the products of the traditional step-growth aggregation process.

Using Polystyrene-block-polyacrylic acid-coated Metal Nanoparticles as Monomers for Their Homo- and Co-polymerization

We report protocols for &#8220;polymerizing&#8221; various types of polymer-encapsulated metal nanoparticles into long chains of &#8220;homo-&#8220; and &#8220;co-polymers&#8221;.

Polistiren kullanma<em&gt; Bloğu</em&gt; -poli (Akrilik asit) Bunların homo- ve ko-polimerizasyon için monomer olarak metal Nanopartiküller -kaplı

We present a template-free method for &#8220;polymerizing&#8221; nanoparticles into long chains without side branches. A variety of nanoparticles are ...

Kimya

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 ...

Synthesis, Characterization, and Functionalization of Hybrid Au/CdS and Au/ZnS Core/Shell Nanoparticles

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large extinction coefficients which can be tuned across the visible spectrum. Research into the plasmonic enhancement of optical transitions has become popular, due to the possibility of altering and in some cases improving photo-absorption or emission properties of nearby chromophores such as molecular dyes or quantum dots. The electric field of the plasmon can couple with the excitation dipole of a chromophore, perturbing the electronic states involved in the transition and leading to increased absorption and emission rates. These enhancements can also be negated at close distances by energy transfer mechanism, making the spatial arrangement of the two species critical. Ultimately, enhancement of light harvesting efficiency in plasmonic solar cells could lead to thinner and, therefore, lower cost devices. The development of hybrid core/shell particles could offer a solution to this issue. The addition of a dielectric spacer between a gold nanoparticles and a chromophore is the proposed method to control the exciton plasmon coupling strength and thereby balance losses with the plasmonic gains. A detailed procedure for the coating of gold nanoparticles with CdS and ZnS semiconductor shells is presented. The nanoparticles show high uniformity with size control in both the core gold particles and shell species allowing for a more accurate investigation into the plasmonic enhancement of external chromophores.

The synthesis of uniform gold nanoparticles coated with semiconductor shells of CdS or ZnS is performed. The semiconductor coating is conducted by first depositing a silver sulfide shell and exchanging the silver cations for zinc or cadmium cations.

Sentezi, Karakterizasyonu ve Hibrid Au / CdS ve Au / ZnS Çekirdek / Shell Nanopartiküller işlevselleştirilmesi

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large ...

Synthesis and Characterization of Supramolecular Colloids

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

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

Supramoleküler Kolloidlerin Sentezi ve Karakterizasyonu

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

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various precursor noble metal ions with reducing agents in a 1:1 (v/v) ratio results in the formation of metal gels within seconds to minutes compared to much longer synthesis times for other techniques such as sol-gel. Conducting the reduction step in a microcentrifuge tube or small volume conical tube facilitates a proposed nucleation, growth, densification, fusion, equilibration model for gel formation, with final gel geometry smaller than the initial reaction volume. This method takes advantage of the vigorous hydrogen gas evolution as a by-product of the reduction step, and as a consequence of reagent concentrations. The solvent accessible specific surface area is determined with both electrochemical impedance spectroscopy and cyclic voltammetry. After rinsing and freeze drying, the resulting aerogel structure is examined with scanning electron microscopy, X-ray diffractometry, and nitrogen gas adsorption. The synthesis method and characterization techniques result in a close correspondence of aerogel ligament sizes. This synthesis method for noble metal aerogels demonstrates that high specific surface area monoliths may be achieved with a rapid and direct reduction approach.

A rapid, direct solution-based reduction synthesis method to obtain Au, Pd, and Pt aerogels is presented.

Otomatik Güncelleştirmeler, Pd ve Pt Aerogels üzerinden doğrudan çözüm tabanlı azaltma için hızlı sentez yöntemi

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...

Synthesis of Bimetallic Pt/Sn-based Nanoparticles in Ionic Liquids

We demonstrate a method for the synthesis of bimetallic nanoparticles consisting of Pt and Sn. A synthesis strategy is used in which the particular physico-chemical properties of ionic liquids (ILs) are exploited to control both nucleation and growth processes. The nanoparticles form colloidal sols of very high colloidal stability in the IL, which is particularly interesting in view of their use as quasi-homogeneous catalysts. Procedures for both nanoparticle extraction in conventional solvents and for nanoparticle precipitation are presented. The size, structure and composition of the synthesized nanocrystals are confirmed using inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray diffraction analysis (XRD) and transmission electron microscopy (TEM) with energy-dispersive X-ray spectroscopy (EDX). By this, we show that the nanocrystals are random-type alloy and of small (2-3 nm) size. The catalytic activity and selectivity in the hydrogenation of &#945;,&#946;-unsaturated aldehydes is tested in a semi-continuous batch-type reactor. In this context, the bimetallic Pt/Sn-based nanoparticles reveal a high selectivity towards the unsaturated alcohol.

A protocol for the synthesis of bimetallic nanoparticles in ionic liquids and the procedure of their catalytic testing in the selective hydrogenation of unsaturated aldehydes are described.

Bimetal Pt/Sn tabanlı nano tanecikleri İyonik Sıvılar içinde sentezi

We demonstrate a method for the synthesis of bimetallic nanoparticles consisting of Pt and Sn. A synthesis strategy is used in which the particular ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared according to the methodology developed by surface organometallic chemistry (SOMC). In this framework, catalytic cycles can be determined by isolating crucial intermediates. All air-sensitive materials are handled under inert atmosphere (using gloveboxes or a Schlenk line) or high vacuum lines (HVLs, &#60;10-5 mbar). The preparation of SiO2-700 (silica dehydroxylated at 700 &#176;C) and subsequent applications (the grafting of complexes and catalytic runs) requires the use of HVLs and double-Schlenk techniques. Several well-known characterization methods are used, such as Fourier-transform infrared spectroscopy (FTIR), elemental microanalysis, solid-state nuclear magnetic resonance spectroscopy (SSNMR), and state-of-the-art dynamic nuclear polarization surface enhanced NMR spectroscopy (DNP-SENS). FTIR and elemental microanalysis permit scientists to establish the grafting and its stoichiometry. 1H and 13C SSNMR allows the structural determination of the hydrocarbon ligands coordination sphere. DNP SENS is an emerging powerful technique in solid characterization for the detection of poorly sensitive nuclei (15N, in our case). SiO2-700 is treated with about one equivalent of the metal precursor compared to the amount of surface silanol (0.30 mmol&#183;g-1) in pentane at room temperature. Then, volatiles are removed, and the powder samples are dried under dynamic high vacuum to afford the desired materials [(&#8801;Si-O-)Hf(&#951;2&#960;-MeNCH2)(&#951;1-NMe2)(&#951;1-HNMe2)]. After a thermal treatment under high vacuum, the grafted complex is converted into metal imido silica complex [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)]. [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] effectively promotes the metathesis of imines, using the combination of two imine substrates, N-(4-phenylbenzylidene)benzylamine, or N-(4-fluorobenzylidene)-4-fluoroaniline, with N-benzylidenetert-butylamine as substrates. A significantly lower conversion is observed with the blank runs; thus, the presence of the imido group in [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is correlated to the catalytic performance.

A new group IV metal catalyst for imine metathesis is prepared by grafting amine metal complex onto dehydroxylated silica. Surface metal fragments are characterized using FT-IR, elemental microanalysis, and solid-state NMR spectroscopy. Further dynamic nuclear polarization surface enhanced NMR spectroscopy experiments complement the determination of the coordination sphere.

Yüzey Organometalik Kimya metodolojisini kullanan Silika Destekli Katalizörler tarafından Imine Metatez

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...

Preparation of Silver-Palladium Alloyed Nanoparticles for Plasmonic Catalysis under Visible-Light Illumination

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular transformations. This opens possibilities for the use of visible or near-IR light as a sustainable input to drive and control reactions when plasmonic nanoparticles supporting LSPR excitation in these ranges are employed as catalysts. Unfortunately, this is not the case for several catalytic metals such as palladium (Pd). One strategy to overcome this limitation is to employ bimetallic NPs containing plasmonic and catalytic metals. In this case, the LSPR excitation in the plasmonic metal can contribute to accelerate and control transformations driven by the catalytic component. The method reported herein focuses on the synthesis of bimetallic silver-palladium (Ag-Pd) NPs supported on ZrO2 (Ag-Pd/ZrO2) that acts as a plasmonic-catalytic system. The NPs were prepared by co-impregnation of corresponding metal precursors on the ZrO2 support followed by simultaneous reduction leading to the formation of bimetallic NPs directly on the ZrO2 support. The Ag-Pd/ZrO2 NPs were then used as plasmonic catalysts for the reduction of nitrobenzene under 425 nm illumination by LED lamps. Using gas chromatography (GC), the conversion and selectivity of the reduction reaction under the dark and light irradiation conditions can be monitored, demonstrating the enhanced catalytic performance and control over selectivity under LSPR excitation after alloying non-plasmonic Pd with plasmonic metal Ag. This technique can be adapted to a wide range of molecular transformations and NPs compositions, making it useful for the characterization of the plasmonic catalytic activity of different types of catalysis in terms of conversion and selectivity.

Presented here is a protocol for the synthesis of silver-palladium (Ag-Pd) alloy nanoparticles (NPs) supported on ZrO2 (Ag-Pd/ZrO2). This system allows for harvesting energy from visible light irradiation to accelerate and control molecular transformations. This is illustrated by nitrobenzene reduction under light irradiation catalyzed by Ag-Pd/ZrO2 NPs.

Görünür-Işık Aydınlatması Altında Plazmonik Kataliz için Gümüş-Paladyum Alaşımlı Nanopartiküllerin Hazırlanması

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular ...

Gold Nanoparticle Synthesis

Gold nanoparticles (Au nanoparticles) that are ~12 nm in diameter were synthesized by rapidly injecting a solution of 150 mg (0.15 mmol) of tetrachloroauric acid in 3.0 g (3.7 mmol, 3.6 mL) of oleylamine (technical grade) and 3.0 mL of toluene into a boiling solution of 5.1 g (6.4 mmol, 8.7 mL) of oleylamine in 147 mL of toluene. While boiling and mixing the reaction solution for 2 hours, the color of the reaction mixture changed from clear, to light yellow, to light pink, and then slowly to dark red. The heat was then turned off, and the solution was allowed to gradually cool down to room temperature for 1 hour. The gold nanoparticles were then collected and separated from the solution using a centrifuge and washed three times; by vortexing and dispersing the gold nanoparticles in 10 mL portions of toluene, and then precipitating the gold nanoparticles by adding 40 mL portions of methanol and spinning them in a centrifuge. The solution was then decanted to remove any remaining byproducts and unreacted starting materials. Drying the gold nanoparticles in a vacuum environment produced a solid black pellet; which could be stored for long periods of time (up to one year) for later use, and then redissolved in organic solvents such as toluene.

A protocol for synthesizing ~12 nm diameter gold nanoparticles (Au nanoparticles) in an organic solvent is presented. The gold nanoparticles are capped with oleylamine ligands to prevent agglomeration. The gold nanoparticles are soluble in organic solvents such as toluene.

Altın Nanopartikül Sentezi

Gold nanoparticles (Au nanoparticles) that are ~12 nm in diameter were synthesized by rapidly injecting a solution of 150 mg (0.15 mmol) of ...

Triplet Fusion Upconversion Nanocapsule Synthesis

Triplet fusion upconversion (UC) allows for the generation of one high energy photon from two low energy input photons. This well-studied process has significant implications for producing high energy light beyond a material's surface. However, the deployment of UC materials has been stymied due to poor material solubility, high concentration requirements, and oxygen sensitivity, ultimately resulting in reduced light output. Toward this end, nanoencapsulation has been a popular motif to circumvent these challenges, but durability has remained elusive in organic solvents. Recently, a nanoencapsulation technique was engineered to tackle each of these challenges, whereupon an oleic acid nanodroplet containing upconversion materials was encapsulated with a silica shell. Ultimately, these nanocapsules (NCs) were durable enough to enable triplet fusion upconversion-facilitated volumetric three-dimensional (3D) printing. By encapsulating upconversion materials with silica and dispersing them in a 3D printing resin, photopatterning beyond the surface of the printing vat was made possible. Here, video protocols for the synthesis of upconversion NCs are presented for both small-scale and large-scale batches. The outlined protocols serve as a starting point for adapting this encapsulation scheme to multiple upconversion schemes for use in volumetric 3D printing applications.

This protocol details the synthesis of upconversion nanocapsules for subsequent use in photopolymerizable resins for triplet fusion upconversion-facilitated volumetric 3D printing.

Üçlü Füzyon Yukarı Dönüşüm Nanokapsül Sentezi

Triplet fusion upconversion (UC) allows for the generation of one high energy photon from two low energy input photons. This well-studied process has ...