This research was supported by the Natural Sciences and Engineering Research Council (NSERC) of Canada, the Canada Research Chairs Program, and Simon Fraser University. This work made use of 4D LABS shared facilities supported by the Canada Foundation for Innovation (CFI), British Columbia Knowledge Development Fund (BCKDF) and Simon Fraser University.

NaYF 4 / Yb 3+ / Er 3+ upconverting Nanopartiküller (UCNP) 1. sentezi <ol><li> Olarak takip cihazı ayarlayın: <ol><li> Düzenli karıştırma plaka üzerinde 250 ml&#39;lik bir ısıtma manto yerleştirin ve termal çift üzerine manto takın. </li><li> Uygun olarak tespit ısıtma mantosu üzerine bir manyetik karıştırma çubuğu ile donatılmış bir 250 ml&#39;lik yuvarlak tabanlı bir şişeye koyun. </li><li> Yuvarlak dipli sol boyun hava adaptörünü ve plastik boru ile savurma hattına bu hava adaptörünü bağlayın. </li><li> Yuvarlak dipli sağ boyun cam adaptörünü ve cam adaptör üzerine bir termometre adaptörünü sabitleyin. Termometre adaptörü ile balona sıcaklık probu yerleştirin ve termokupl içine bu takın. </li><li> Yuvarlak tabanlı şişenin orta boynunun bir damıtma kafası takın. Damıtma kafası üzerine bir stoper yerleştirin. Bir vakum distillat ardından bir kondansatör kafa bağlayınİyon adaptörü ve 50 ml&#39;lik yuvarlak tabanlı bir şişeye. Plastik boru aracılığıyla kabarcık Vakum damıtma adaptörünü bağlayın. </li></ol></li><li> Itriyum asetat 1.17 g (3.9 mmol), iterbiyum asetat 0.439 g ve erbiyum asetat 0,0727 g (0.1 mmol) tartılır ve yuvarlak dipli bir deney kabına reaksiyona koyun. </li><li> Oleik asit 30 ml ve bir dereceli silindir kullanarak şişeye -oktadesene 75 ml ekleyin. </li><li> 5 ml metanol herhangi bir oleik asit, ve oktadesen reaksiyon şişesine kenarlarına yapışmış olduğundan emin olmak için, kullanılarak yuvarlak tabanlı reaksiyonun yan durulayın. </li><li> Çift manifoldu Schlenk hattına tepki şişeyi bağlayın ve azot hattına bağlı reaksiyon şişesi tutmak için gelen vanayı çevirin. </li><li> , Termokupl açın 80 ° C sıcaklığı ayarlamak ve yavaş yavaş, bu sıcaklıkta, sistemi ısıtın. Tüm başlangıç ​​materyalleri eritilir sonra 80 ° C&#39;de ve, ısıtma gömleğinin kaldırmak ve reaksiyona olanak vermek30 ° C&#39;ye kadar soğutun. </li><li> Sıcaklık 30 ° C&#39;ye ulaştığında, damıtma kafasını çıkarmak orta boyun sol boyun hava adaptörünü geçiş ve bir tıpa ile sol boyun kapatmaktadır. Yavaşça vakum hattına azot hattından savurma hattında vana çevirerek reaksiyon balonuna vakum tanıtmak. Düşük kaynama noktalı bileşenlerin tümü, bu noktada reaksiyondan üzerinden çekilir. </li><li> Çözelti köpüren durduğunda, 5 ° C / dk bir hızda, 115 ° C sıcaklık yükseltmek. </li><li> Sıcaklık 115 ° C&#39;ye ulaştığında, 15 dakika boyunca bu sıcaklıkta muhafaza daha sonra ısıtma mantosu çıkarın ve 50 ° C&#39;de reaksiyonun soğuması. Daha sonra, hızlı bir şekilde orta boyun ve sol baş hava adaptörü damıtma kafa reattaching geri orijinal formuna kurmak geçin. </li><li> Soğutma işlemi sırasında NaOH 0.74 g (12.5 mmol) ve NH4 F 0.50 g (20.0 mmol) tartılır ve bunları çözmeksonikasyon ile metanol içinde 50 ml. </li><li> Sonikasyon sonrasında, yuvarlak tabanlı reaksiyona girerek çözelti dökün ve 5 ml MeOH ile Şişenin yanlarının yıkayın. </li><li> 30 dakika boyunca 50 ° C de karıştırılarak çözelti bırakın. </li><li> Metanol damıtmak için 75 ° C sıcaklık artırır. </li><li> Gerektiğinde damıtma sırasında, toplama şişesi boşaltın. Damıtma işlemi bittikten sonra, mümkün olduğunca hızlı azot koruması altında 300 ° C&#39;ye tepki ısınır. </li><li> Sıcaklık 300 ° C&#39;ye ulaştığında, 1 saat boyunca bu sıcaklıkta muhafaza. Gerekirse, sıcaklık korumaya yardımcı olmak için alüminyum folyo ile setup kapsamaktadır. Daha sonra ısı kaynağı çıkarın ve reaksiyon, oda sıcaklığına kadar soğumaya bırakın. </li><li> Bu sırada oda sıcaklığına kadar soğutuldu sonra üç santrifüj tüpleri (50 mi borular, her bir tüp başına yaklaşık 35 ml solüsyon) içinde eşit bir şekilde çözelti ayrıldı ve 50 ml üst borusunu, susuz etanol kullanılarak ölçek. Santrifüj tüm tO 15 dakika 3400 xg&#39;de borular. Santrifüj işleminden sonra, beyaz bir çökelti UCNPs tüplerin tarafında gözlenmelidir. </li><li> Süpernatant atılır ve heksan (her tüp için heksan 7.5 ml) &#39;de UCNPs pelet yeniden disperse, daha sonra 50 ml ölçekli etanol ile tüp doldurun. Santrifüj tüpleri tekrar 15 dakika 3400 xg&#39;de. </li><li> Santrifüj işlemi tamamlandıktan sonra, süpernatan atılır ve daha sonra kullanılmak üzere CHCI3 30 ml bir katı UCNPs yeniden disperse. </li></ol> Organik boya molekülünü ve upconverting Nanopartiküller İçeren 2. Montaj suda dağılabilir Nanoassemblies <ol><li> Bir manyetik karıştırma çubuğu ile donatılmış bir ışıldama şişesine boşaltıldı CHCI3 3 ml poli (stiren-alt -maleik anhidrid), 25 mg (0,0147 mmol), (PSMA) içinde çözülür. Bu miktar birden denemeden sonra optimize edilmiş miktardır. </li><li> Upconverting 250 ul (47 mg / ml) ilave edilir taraması yapmak üzere kloroform stok solüsyonu nanopartiküllerillation şişe. </li><li> Kapatılır ve manyetik bir karıştırma levhasının üzerine yerleştirin ve 2 saat boyunca oda sıcaklığında çözelti karıştırılır. </li><li> 2070 amin polieter 160 mg (0,0773 mmol) tartılır ve CHCI3 1 ml içinde çözülür. Daha sonra, bir pipet kullanılarak, bir kısım halinde sintilasyon şişesine, bu çözüm ekleyin. Çözelti PSMA üzerinde anhidrit grupları ile 2070 amin polieter tepkisini gösteren sarı soluk dönecek. </li><li> Gece boyunca oda sıcaklığında çözelti karıştırılmaya devam edin. </li><li> 1 saat süre ile karıştırıldı, elde edilen çözeltinin, daha sonra organik boya moleküllerinin uygun miktarda ölçün bir kısım halinde sintilasyon şişesine içine dağıtın. <ol><li> Örnek TPP-NP (nanoassembly polimer kabuk, tetrafenil porfirin ve upconverting nanopartikülleri içeren) için, doğrudan olarak ışıldama şişesine tetrafenil porfirinin 1 mg ekleyin. Örnek DAE-UCNP (nanoassembly için polimer kabuk, diarylethene molekülleri ve upconverting nanoparçacık içerens), her bir diarylethene moleküllerinin miktarı 2 x 10 -7 mol. Reaksiyon çözeltisi içine, iki diarylethene molekülleri ekleyin. İki diarylethene moleküller için hacimleri: DAE-1o (1.8 mM), 111 ul ve DAE-2O (1.6 mM), 125 ul. </li></ol></li><li> Bir döner buharlaştırıcı kullanılarak indirgenmiş basınç altında çözücüyü çıkarın CHCI3, sonra sütümsü süspansiyon meydana getirilinceye kadar, sonra flakon sonikasyon, sintilasyon şişesine 3 mL (11 pH ≈) M sulu NaOH 0,001 ekleyin. </li><li> Geri dönüşlü buharlaştırıcı ile şişe yerleştirin ve süspansiyon daha berrak bir solüsyona dönüştü kadar dikkatlice geri kalan CHCl3 çıkarın. </li><li> Daha sonra 25 dakika boyunca 20.600 xg&#39;de çözüm santrifüj, iki adet 1,5 ml&#39;lik konik santrifüj tüplerine sintilasyon şişeden çözüm aktarın. </li><li> Süpernatant atılır, daha sonra, iki tüp (tüp başına 1,5 mi) içine deiyonize H2O 3 ml toplam eklemek peletler yeniden dağıtmak için tüpler sonikasyondeiyonize H 2 O. </li><li> 25 dakika boyunca 20.600 x g hızında tekrar santrifüj iki boruyu. </li><li> Süpernatant atılır, daha sonra iki tüp (tüp başına 1.5 mi) içinde deiyonize H2O 3 ml toplam ekleyin. Deiyonize H2O pelet yeniden dağıtmak için tüpler sonikasyon </li><li> Ileri testler için son örneği elde etmek için bir 0.2 mikron bir şırınga filtreden geçirilmiştir sulu bir dispersiyon örneği nanopartiküller filtre. </li></ol>

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The authors have nothing to disclose.

Bu protokole uygun olarak sentez nanopartiküller Bir α-NaYF 4 ev sahibi kafes yapısı ile küresel parçacıklar olarak sınıflandırılabilir yaklaşık 22,5 nm. 26,27 merkezli 20 25 nm arasında bir boyut dağılımına sahiptir. Bu protokolde iki kritik adımlar vardır. UCNP sentezinde, bu parçacık boyutunun dar bir dağılımı sağlamak için mümkün olduğu kadar kesin bir ısıtma sıcaklığı ve zamanı sağlamak için çok önemlidir. Iyi dağıtılmış boyut ve iyi bir morfoloji...

Bugün biyo-görüntüleme ajanları yeni türleri geliştirmek için acil ihtiyaç duyulmaktadır. Birçok roman floresan probları iyi belgelenmiştir. 1-6 Ancak, görüntü çözünürlüğü önemli gelişmeler bir sorun olmaya devam etmektedir. 7 Tek pratik yöntem, doğrudan bir &#39;hafif&#39; yayan devlet ve &#39;karanlık&#39; söndürüldü devlet arasındaki floresan probları modüle etmektir. 8-12 Bu özel yöntem, uyarılmış emisyon tükenmesi gibi teknolojileri geliştirmek için uygulanmıştır (STED) mikroskopi 13 ve stokastik optik rekonstrüksiyon mikroskobu (FIRTINA). 14 Floresan modüle için başka bir yaklaşım, floresan probları ile birlikte bir çift ışığa cevap kromoforlar etmektir. 15,16 izomerlerden sadece birisinin etkin bir enerji aktarma alıcısı olarak hareket edebilen iki izomer arasındaki ışığa cevap kromofor geçiş yapılması, th flüoresanının söndürülmesi üzerinde kontrole olanak sağlamaktadırFörster Rezonans Enerji Transferi (FRET) ve diğer mekanizmalar aracılığıyla e prob. Sonuç bir emisyonlu devleti oluşturma ve ışığın farklı dalga boylarında ışığa cevap kromoforun maruz kalarak dönüşümlü edilebilir söndürüldü devlettir. Işığa diarylethene kromoforlar tersine çevrilebilir renksiz halka açık izomeri ve UV ve görünür ışık ile ışınlama üzerine renkli halka kapalı izomeri arasında geçiş yapılabilir. 17-19 halka kapalı izomer make iki izomer ve ayarlanabilir emme spektrumları termal stabilitesi diarylethenes çok iyi aday kontrol FRET alıcıları olarak. 20-23 lantanid katkılı NaYF 4 upconverting nanopartiküller biyo-görüntüleme için faydalıdır. 24 Bu nanopartiküller yakın kızılötesi ışık emer ve görünür spektrum çeşitli bölgelerinde ışık yayar. Işığa cevap diarylethene kromoforları ve nano-parçacıkları birleştirerek floresans modülasyon örnekleri önceden edilmiştirbir önce grubumuz tarafından rapor edilmiştir. 25-27 Bununla birlikte, her örnek için tarif sistemler daha çeşitli sistemlerin geliştirilmesini zorlaştırmaktadır nanopartiküllerin yüzeyine diarylethenes takmak için bir ek sentetik modifikasyon gerekli. Bu yazıda kendi kendine montaj stratejisi kullanılarak suda dağılabilir organik boya molekülleri ve ışığa cevap upconverting nanopartiküller hazırlamak için basit bir &#39;tak-çalıştır&#39; yöntemini göstermektedir. Polimerlerin seçimi; 2070 amin poli (stiren-alt -maleik anhidrid) ve polieter hidrofobik ve hidrofilik bir ortam hem de sağlar. Polimerin hidrofilik bölgesi suda çözünürlüğe muhafaza edilmesi için önemli ise, polimer yardımıyla hidrofobik bölümler, birbirine normal suda çözünür olmayan organik moleküller ve upconverting nanopartikülleri tutun. Biz ilk termal çekirdeklenme yöntemiyle upconverting nanopartiküllerin sentezi gösterecektir. Sonra, biz ho ispat edecektirOrganik moleküller ve upconverting nanopartiküller polimer kabuk hidrofobik bölgeler içinde kapsüllenmiş ve basit uygun bir çalışma prosedüreüne ardından upconverting nanopartiküller, polimer ve farklı organik boya molekülleri ihtiva eden bir çözelti, co-karıştırılarak sulu ortam içinde sabit kalması w. Biz de dış ışık ışıması kullanılarak meclislerinin floresan emisyonunu modüle nasıl gösterilmektedir. Biz suda dağılabilir nanoassemblies genişletmeye devam edeceğiz yapmak için bu &#39;tak-çalıştır&#39; yöntemini kullanarak kapsamını tahmin.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>yttrium acetate</td>
			<td>sigma</td>
			<td>326046</td>
			<td>Yttrium(III) acetate hydrate</td>
		</tr>
		<tr>
			<td>ytterbium acetate</td>
			<td>sigma</td>
			<td>544973</td>
			<td>&#160;Ytterbium(III) acetate hydrate&#160;</td>
		</tr>
		<tr>
			<td>erbium acetate</td>
			<td>sigma</td>
			<td>325570</td>
			<td>Erbium(III) acetate hydrate</td>
		</tr>
		<tr>
			<td>oleic acid</td>
			<td>sigma</td>
			<td>75096</td>
			<td>analytical standard</td>
		</tr>
		<tr>
			<td>octadecene</td>
			<td>sigma</td>
			<td>O806&#160;</td>
			<td>Technical grade&#160;</td>
		</tr>
		<tr>
			<td>NaOH</td>
			<td></td>
			<td>S5881&#160;</td>
			<td>reagent grade</td>
		</tr>
		<tr>
			<td>NH4F</td>
			<td></td>
			<td>216011</td>
			<td>ACS reagent</td>
		</tr>
		<tr>
			<td>poly(styrene-alt-maleic anhydride)</td>
			<td>sigma</td>
			<td>4422699</td>
			<td>Average Mn= 1700</td>
		</tr>
		<tr>
			<td>JeffAmine 2070</td>
			<td>Huntsman</td>
			<td>M-2070</td>
			<td></td>
		</tr>
		<tr>
			<td>Varian Carry 300</td>
			<td>Agilent</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>JDSU NIR laser</td>
			<td>JSDU</td>
			<td>L4-9897510-100M</td>
			<td>980 nm diode laser</td>
		</tr>
	</tbody>
</table>

a 'plug and play' method to create water-dispersible nanoassemblies containing an amphiphilic polymer, organic dyes and upconverting nanoparticles

In this protocol, we first describe a procedure to synthesize lanthanide doped upconverting nanoparticles (UCNPs). We then demonstrate how to generate amphiphilic polymers in situ, and describe a protocol to encapsulate the prepared UCNPs and different organic dye molecules (porphyrins and diarylethenes) using polymer shells to form stable water-dispersible nanoassemblies. The nanoassembly samples containing both the UCNPs and the diarylethene organic dyes have interesting photochemical and photophysical properties. Upon 365 nm UV irradiation, the diarylethene group undergoes a visual color change. When the samples are irradiated with visible light of another specific wavelength, the color fades and the samples return to the initial colorless state. The samples also emit visible light from the UCNPs upon irradiation with 980 nm near-infrared light. The emission intensity of the samples can be tuned through alternate irradiation with UV and visible light. Modulation of fluorescence can be performed for many cycles without observable degradation of the samples. This versatile encapsulation procedure allows for the transfer of hydrophobic molecules and nanoparticles from an organic solvent to an aqueous medium. The polymer helps to maintain a lipid-like microenvironment for the organic molecules to aid in preservation of their photochemical behavior in water. Thus this method is ideal to prepare water-dispersible photoresponsive systems. The use of near-infrared light to activate upconverting nanoparticles allows for lower energy light to be used to activate photoreactions instead of more harmful ultraviolet light.

Absorpsiyon spektrumları ve fotoluminesans spektrumları numune DAE-UCNP için toplanmıştır. Emme spektrumları kapalı diarylethene kromoforlar ve upconverting nano-tanecikleri arasındaki spektral örtüşme karşılaştırılması için kullanılır. Örneklerde (TPP-UCNP hem de DAE-UCNP) fotoğrafları, sulu faz içinde amfifilik polimer kabukları içinde bulunan organik boya molekülleri ile upconverting nanopartiküller, başarılı bir şekilde kapsülleme göstermek için dahil edilmiştir. Fotokimyada ve f...

Watch this Scientific Journal Video about A 'Plug and Play' Method to Create Water-dispersible Nanoassemblies Containing an Amphiphilic Polymer, Organic Dyes and Upconverting Nanoparticles at JoVE.com

A 'Plug and Play' Method to Create Water-dispersible Nanoassemblies Containing an Amphiphilic Polymer, Organic Dyes and Upconverting Nanoparticles

Organic dye molecules and oleic acid coated upconverting nanoparticles are not water-soluble. This protocol describes a &#8216;plug and play&#8217; method that enables the transfer of organic dye molecules and upconverting particles from their initial hydrophobic solvent to water.

A &#39;Tak ve&#39; Yöntem, bir Amfifilik Polimer, Organik maddeler ve upconverting Nanopartiküller İçeren Su dağılabilir Nanoassemblies oluşturma

In this protocol, we first describe a procedure to synthesize lanthanide doped upconverting nanoparticles (UCNPs). We then demonstrate how to generate ...

a-plug-play-method-to-create-water-dispersible-nanoassemblies

Research

JoVE Journal

Chemistry

9.8K Görüntüleme.  Simon Fraser University. Organic dye molecules and oleic acid coated upconverting nanoparticles are not water-soluble. This protocol describes a ‘plug and play’ method that enables the transfer of organic dye molecules and upconverting particles from their initial hydrophobic solvent to water. 

Video: A 'Plug and Play' Method to Create Water-dispersible Nanoassemblies Containing an Amphiphilic Polymer, Organic Dyes and Upconverting Nanoparticles

Analysis of Volatile and Oxidation Sensitive Compounds Using a Cold Inlet System and Electron Impact Mass Spectrometry

This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The analysis of volatile and oxidation sensitive compounds by mass spectrometry is not easily achieved, as all state-of-the-art mass spectrometric methods require at least one sample preparation step, e.g., dissolution and dilution of the analyte (electrospray ionization), co-crystallization of the analyte with a matrix compound (matrix-assisted laser desorption/ionization), or transfer of the prepared samples into the ionization source of the mass spectrometer, to be conducted under atmospheric conditions. Here, the use of a sample inlet system is described which enables the analysis of volatile metal organyls, silanes, and phosphanes using a sector field mass spectrometer equipped with an electron impact ionization source. All sample preparation steps and the sample introduction into the ion source of the mass spectrometer take place either under air-free conditions or under vacuum, enabling the analysis of compounds highly susceptible to oxidation. The presented technique is especially of interest for inorganic chemists, working with metal organyls, silanes, or phosphanes, which have to be handled using inert conditions, such as the Schlenk technique. The principle of operation is presented in this video.

This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The presented technique is especially of interest for inorganic chemists, working with metal organyls, silanes, or phosphanes which have to be handled using inert conditions, such as the Schlenk technique.

Soğuk Giriş Sistemi ve Electron Impact Kütle Spektrometresi kullanarak Uçucu ve Oksidasyon Hassas Bileşiklerin Analizi

This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The ...

Kimya

Synthesis and Characterization of Functionalized Metal-organic Frameworks

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy.

Synthesis, activation, and characterization of intentionally designed metal-organic framework materials is challenging, especially when building blocks are incompatible or unwanted polymorphs are thermodynamically favored over desired forms. We describe how applications of solvent-assisted linker exchange, powder X-ray diffraction in capillaries and activation via supercritical CO2 drying, can address some of these challenges.

Fonksiyonlu Sentezi ve Karakterizasyonu Metal-organik Altyapıları

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ethylene-propylene rubber, grafted with maleic anhydride, is thermo-reversibly cross-linked in two steps. The pending anhydride moieties are first modified with furfurylamine to graft furan groups to the rubber backbone. These pendant furan groups are then cross-linked with a bis-maleimide via a Diels-Alder coupling reaction. Both reactions can be performed under a broad range of experimental conditions and can easily be applied on a large scale. The material properties of the resulting Diels-Alder cross-linked rubbers are similar to a peroxide-cured ethylene/propylene/diene rubber (EPDM) reference. The cross-links break at elevated temperatures (&#62; 150 &#176;C) via the retro-Diels-Alder reaction and can be reformed by thermal annealing at lower temperatures (50-70 &#176;C). Reversibility of the system was proven with infrared spectroscopy, solubility tests and mechanical properties. Recyclability of the material was also shown in a practical way, i.e., by cutting a cross-linked sample into small parts and compression molding them into new samples displaying comparable mechanical properties, which is not possible for conventionally cross-linked rubbers.

A simple two-step approach involving rubber modification and cross-linking yields fully reworkable, elastic rubber products.

Termo-tersinir Çapraz bağlı Lastik Via Diels-Alder Kimya hazırlanması ve Özellikleri

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

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

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

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

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

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

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables the silk proteins to be compact and ordered by shearing and elongation forces. Here, a biomimetic microfluidic channel was designed to mimic the specific geometry of the spinning duct of the silkworm. Regenerated silk fibroin (RSF) spinning doped with high concentration, was extruded through the microchannel to dry-spin fibers at ambient temperature and pressure. In the post-treated process, the as-spun fibers were drawn and stored in ethanol aqueous solution. Synchrotron radiation wide-angle X-ray diffraction (SR-WAXD) technology was used to investigate the microstructure of single RSF fibers, which were fixed to a sample holder with the RSF fiber axis normal to the microbeam of the X-ray. The crystallinity, crystallite size, and crystalline orientation of the fiber were calculated from the WAXD data. The diffraction arcs near the equator of the two-dimensional WAXD pattern indicate that the post-treated RSF fiber has a high orientation degree.

A protocol for the microfluidic spinning and microstructure characterization of regenerated silk fibroin monofilament is presented.

Mikrosıvısal kuru-iplik ve rejenere ipek Fibroin lifleri karakterizasyonu

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

Elektrokimyasal empedans spektroskopisi elektrokimyasal oranı sürekli tahmini için bir araç olarak

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

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

Zaman karar vermek Photophysical karakterizasyonu üçlüsü-hasat organik bileşikler bir oksijensiz ortamı kullanarak bir ICCD kamera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...

Raman and IR Spectroelectrochemical Methods as Tools to Analyze Conjugated Organic Compounds

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule on the vibrational level of energy. Raman and IR spectroelectrochemistry can be used for advanced characterization of the structural changes in the organic electroactive compounds. Here, the step-by-step analysis by means of Raman and IR spectroelectrochemistry is shown. Raman and IR spectroelectrochemical techniques provide complementary information about structural changes occurring during an electrochemical process, i.e. allows for the investigation of redox processes and their products. The examples of IR and Raman spectroelectrochemical analysis are presented, in which the products of the redox reactions, both in solution and solid state, are identified.

A protocol of step-by-step Raman and IR spectroelectrochemical analysis is presented.

Raman ve IR spektroelektrokimyasal yöntemleri araçları olarak konjuge organik bileşikler çözümlemek için

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule ...

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

Here, we describe an effective protocol that combines photoredox Ni/Ir catalysis with the use of a Zn-alkoxide for efficient ring-opening polymerization, allowing for the synthesis of isotactic poly(&#945;-hydroxy acids) with expected molecular weights (&#62;140 kDa) and narrow molecular weight distributions (Mw/Mn &#60; 1.1). This ring-opening polymerization is mediated by Ni and Zn complexes in the presence of an alcohol initiator and a photoredox Ir catalyst, irradiated by a blue LED (400 - 500 nm). The polymerization is performed at a low temperature (-15 &#176;C) to avoid undesired side reactions. The complete monomer consumption can be achieved within 4 - 8 hours, providing a polymer close to the expected molecular weight with narrow molecular weight distribution. The resulted number-average molecular weight shows a linear correlation with the degree of polymerization up to 1000. The homodecoupling 1H NMR study confirms that the obtained polymer is isotactic without epimerization. This polymerization reported herein offers a strategy for achieving rapid, controlled O-carboxyanhydrides polymerization to prepare stereoregular poly(&#945;-hydroxy acids) and its copolymers bearing various functional side-chain groups.

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

A protocol for the controlled photoredox ring-opening polymerization of O-carboxyanhydrides mediated by Ni/Zn complexes is presented.

Photoredox yüzük-açılış polimerizasyon O- Carboxyanhydrides Ni/Zn kompleksleri tarafından aracılı ile kontrol

Here, we describe an effective protocol that combines photoredox Ni/Ir catalysis with the use of a Zn-alkoxide for efficient ring-opening polymerization, ...

Using Cyclic Voltammetry, UV-Vis-NIR, and EPR Spectroelectrochemistry to Analyze Organic Compounds

Cyclic voltammetry (CV) is a technique used in the analysis of organic compounds. When this technique is combined with electron paramagnetic resonance (EPR) or ultraviolet-visible and near-infrared (UV-Vis-NIR) spectroscopies, we obtain useful information such as electron affinity, ionization potential, band-gap energies, the type of charge carriers, and degradation information that can be used to synthesize stable organic electronic devices. In this study, we present electrochemical and spectroelectrochemical methods to analyze the processes occurring in active layers of an organic device as well as the generated charge carriers.

In this article, we describe electrochemical, electron paramagnetic resonance, and ultraviolet-visible and near-infrared spectroelectrochemical methods to analyze organic compounds for application in organic electronics.

Çevrimsel Voltammetry, UV-VIS-NIR ve EPR Spectroelectrochemistry organik bileşikleri analiz kullanarak

Cyclic voltammetry (CV) is a technique used in the analysis of organic compounds. When this technique is combined with electron paramagnetic resonance ...