The authors would like to acknowledge the State of Washington for supporting this research through the University of Washington Clean Energy Institute Exploratory Fellowship Program, and National Science Foundation (NSF) Sustainable Energy Pathway (SEP) Award CHE-1230615.

Dikkat: Kadmiyum öncüleri son derece zehirlidir ve büyük bir dikkatle ele alınması gerekir. Uygun koruyucu kıyafet giyiniz uygun mühendislik kontrollerini kullanın ve danışmak ilgili malzemeler güvenlik veri sayfaları (MSDS). Buna ek olarak, nanopartiküller oluşumu ilave tehlikeleri olabilir. Burada tarif edilen reaksiyonların eylemsiz bir atmosfer içinde deneyleri yürütmek üzere, standart bir vakum gaz manifoldu ile yürütülmektedir. Tüm kimyasallar ticari olarak alındı ​​ve alındığı şekilde kullanıldı. Bu protokol, kısa bir süre önce başka bir yerde tarif edilen daha önce geliştirilmiş sentezleme yöntemi, dayanmaktadır. 5 1. Kükürt Kopolimer Sentezi <ol><li> Erimiş element kükürt hazırlanması <ol><li> Talep element kükürt bağlı bir kondansatör ve ısı sondası ile 50 ml&#39;lik bir üç boyunlu bir şişe içinde (4 g, 124.8 mmol, S 8,% 99.5). Vakum ve azot birkaç kez pompa ve boşaltma çevrimi gerçekleştirin. </li><li> nitrojen altında ısıKükürt san renkli sıvı hale gelmesine neden olur karıştırılarak 150 ° C,. </li></ol></li><li> Kükürt Kopolimerin Hazırlanması <ol><li> Bir kez kükürt, tüm sıvı içine çözününceye, hemen çözüm α-metilstiren (330 ul, 2.5 mmol,% 99) enjekte edilir. </li><li> 10 dakika boyunca 500 rpm&#39;de karıştırılarak 185 ° C&#39;ye kadar ısı çözeltisi. kopolimer formları gibi, çözüm nihayet koyu kırmızı bir renk üreten, turuncu, sarı rengi değişecektir. </li><li> ısı çözelti alınır ve oda sıcaklığına soğumaya bırakın. soğur, kopolimer yavaş yavaş lastik katı bir portakal oluşturmak için kristalize olur. Bu aşamada, kopolimer, bir sonraki sentez için oda sıcaklığında saklanabilir ya da hemen kullanılabilir. </li></ol></li></ol> 2. CdS Nanoparçacık Sentezi <ol><li> , Önceki adımda elde edilen üç boyunlu bir şişeye kadmiyum asetilasetonat (Cd (AcAc), 900 mg, 2.9 mmol,% 99.9) ilave böyleceToz eşit bir katı kükürt kopolimer (4.0 g, 116 mmol) üstüne yerleştirilir. </li><li> azot ve vakum birkaç kez balona pompa ve tasfiye çevrimi gerçekleştirin. </li><li> azot altında karıştırılarak 200 ° C&#39;ye kadar çözelti ısıtılır. kükürt kopolimer eritmek ve kadmiyum öncüsü ile karıştırın ve nanoparçacık çekirdeklenme ve büyüme süreçleri başlayacak olacaktır. </li><li> nanopartiküller 30 dakika boyunca büyümeye olanak sağlar. Not:.. Nanopartiküller büyümesini etkileyecektir reaksiyon süresi değiştirilerek, bu nedenle ayarlamak için nanopartiküllerin son boyutu mümkündür 5 30 dakika reaksiyon süresi 7-10 nm arası bir boyuta aralığı 5 </li><li> ısı çözelti alınır ve oda sıcaklığına soğumaya bırakın. </li><li> Soğuduktan sonra, oda sıcaklığında, şişe ve mağaza katı nanokompozit çıkarın. </li></ol> 3. Kükürt Kopolimeri çıkarın ve Nanoparçacıklar izole <ol><li> Kükürt Kopolimer çıkarılması </strong&gt; <ol><li> 20 ml&#39;lik bir cam şişe içinde nanokompozitinin (200 mg), koyun ve kloroform (20 mi) ilave edin. </li><li> nanokompositlerin kırmak ve çözüm içinde nanopartiküller askıya, 1 saat için bir ultrasonikatör ve sonikasyon flakon yerleştirin. </li><li> İki adet 30 ml&#39;lik santrifüj tüplerine aynlır ve her bir kloroform diğer 20 ilave edin. </li><li> 15 dakika boyunca 8736 xg solüsyonu (göreceli merkezkaç kuvveti) santrifüj. </li><li> yerleşmiş nanopartiküller rahatsız değil emin olun, santrifüj tüplerine gelen kükürt kopolimer süzün. </li></ol></li><li> Nanopartiküller izolasyonu <ol><li> 15 dakika boyunca her santrifüj tüpünün (30 mi) ve sonikasyon kloroformun eklenmesi yerleşmiş nano-tanecikleri yeniden dağıtılır. </li><li> kükürt kopolimer tüm kaldırıldı sağlamak için bölümler 3.1.4, 3.1.5 ve 3.2.1 üç kez daha açıklanan adımları tekrarlayın. Bir kez kükürt kopolimerin tüm kaldırılır boşaltıldı Çözelti No lo olacaknger turuncu bir renge sahiptir. </li><li> Her bir santrifüj tüpüne kloroform (2 mi) eklenerek nihai nano partikülleri toplamak. </li><li> Bir 20 ml&#39;lik bir cam şişeye (4 ml çözelti toplam) toplanan nano parçacıkları birleştirilir ve kloroform kaldırmak için vakum altında cam şişe yerleştirin ve nano-parçacıkları kuru. Bu aşamada elde edilen nanopartiküllerin kitle belirlenebilir ve başlatıcı madde ile ürünün mol oranları kullanılarak reaksiyonun verimi tespit etmek için öncüler başlangıç ​​kütlesine göre. </li></ol></li></ol> CdS Nanoparçacıkları karakterize 4. <ol><li> Transmisyon Elektron Mikroskobu <ol><li> 1 saat boyunca izole edilmiş kloroform içinde nano-tanecikleri (20 mg), (20 mi) ve ultrasonicate seyreltilir. </li><li> 15 dakika için bu kloroform içinde çözelti (5/5 ml damla) ve sonikasyon ile seyreltilir. </li><li> 400 üzerinde holey karbon destek filmleriyle bir ultra ince karbon filmi alt tabaka üzerine nihai çözüm BırakBakır Transmisyon Elektron Mikroskobu (TEM) ızgara örgü. </li><li> bir cam şişede TEM ızgara yerleştirin ve örnek herhangi bir kalan solventin çıkması için, bir gece boyunca vakum altında tutun. </li><li> Kurutma işlemi tamamlandıktan sonra, 200 kV hızlandırma gerilimi, 3 spot boyutu ve ekli Enerji Dağılımı X-ışını spektroskopisi (EDS) detektörü kullanılarak TEM görüntüleri kazanır. </li></ol></li><li> X-ışını difraksiyon <ol><li> kloroform içinde izole edilmiş nano parçacıkları (10 mg / ml) ile seyreltilir. </li><li> 10 dakika boyunca her biri, deterjan, iyonu giderilmiş su, aseton ve izopropil alkol içinde sonike temizleyin molibden kaplanmış soda camı alt-tabakalar (1 cm2). Son olarak, döküm damla önce 10 dakika için bir hava plazma temizleyici yüzeyin temizlenmesi. </li><li> Bırak 7 ul artışlarla 4.2.2 den substratlar üzerine 4.2.1 den çözüm attı. </li><li> filmler kuruduktan sonra, X-ışını difraksiyonu (XRD) veri elde. bir tarama hızında 7,000 veri noktalarını kullanarak veri toplamakbir Cu-Ka X-ışını kaynağı ve 1,54059 Â bir dalga boyu ile saniyede 1 veri noktası. </li></ol></li><li> çözüm Spektroskopisi <ol><li> kapalı bir kuartz küvet içinde 30 dakika ve yeri örnekleri için kloroform ve sonikasyon izole nano-tanecikleri (0.1 mg / ml) dağıtılır. </li><li> malzeme süspansiyonunun kolaylaştıran 70 ° C&#39;ye kadar bölüm 2.6 nanokompozit ve formamid bölüm 1.2.3&#39;de sülfür kopolimeri (1 mg / ml), 700 rpm&#39;de karıştırılmıştır ve ısıyı dağıtmak. </li><li> Her üç numune için fotolüminesans (PL) ve absorbans spektrumlarını kazanır. ultraviyole, görünür ve kızıl ötesine yakın aralık (UV-Vis NIR) boyunca uzanan bir üç dedektörü ile bir spektrometre kullanılarak optik absorbans ölçümleri yürütün. 330 nm&#39;lik bir eksitasyon dalga boyunda bir flüoresan spektrofotometre kullanılarak PL ölçümlerini. NOT: bölümlerde tartışılan teknikleri kullanarak nanopartikülleri tanımlamak için özel bir protokol 4.1.5, 4.2.4, birnd 4.3.2 yaygın olarak kullanılan özel ekipman doğasına bağlı olarak değişir, bu yüzden biz burada sadece genel karakterizasyon parametreleri sunuyoruz. İlgilenen okuyucu CdS nanopartiküller bu analiz teknikleri kullanılarak ilgili daha fazla bilgi için birçok yorum kağıtları yöneliktir 17 -. 19 </li></ol></li></ol>

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The authors disclose no competing financial interests.

We have developed a method to synthesize CdS nanoparticles within a sulfur copolymer matrix. This sulfur copolymer is composed of elemental sulfur and methylstyrene.5 An important feature of this method is that the copolymer can be used as both a high-temperature solvent and a sulfur source that reacts with a cadmium precursor to produce CdS nanoparticles in solution.5 The critical step in the procedure is the synthesis of the sulfur copolymer with a suitable ratio of methylstyrene and sulfur. The u...

sentezi için yararlı olduğu kanıtlanmıştır rağmen, geleneksel alifatik ligandlar fotonik ve elektrokimyasal cihazlarda nanopartiküllerin uygulanması için bir takım zorluklar mevcut. Alifatik ligandlar son derece hidrofobik yalıtım ve elektrokimyasal yüzey reaksiyonları önemli bir engel teşkil etmektedir. 1 Buna göre, çeşitli çalışmalar geliştirdik ligand değişimi ve ligand çıplak nanoparçacık ortaya çıkarmak için fonksiyonel parçalarının veya kaldırdığını ligandlarla Bu alifatik ligandları yerini protokolleri sıyırma vardır yüzey 1 -. 3 Bu reaksiyonlar, ancak birkaç içsel sorunlar oluşturmaktadır. Onlar önemli ölçüde zaman tamamlanması gitmeyin, sentetik sürecin karmaşıklığı ekleyin ve bu teknikleri kullanırken sırayla cihaz üretim sırasında önemli sorunlar empoze edebilirsiniz nanopartiküller, yüzeyini kötüleşmesine neden olabilir. 4 Bir kükürt kopolimeri geliştirdikCdS nanopartiküllerin sentezi sırasında yüksek sıcaklık, çözücüye ve kükürt kaynağı hem de kullanılabilir. 5 bu kopolimer Chung ve diğ. element kükürt ve 1,3-benzeni (DIB) kullanan tarafından geliştirilen bir ağ kopolimerine dayanmaktadır. 6&#39;da bizim davamız, bir metilstiren monomer yerine DIB uygulanmaktadır. Aksi takdirde, yüksek moleküler ağırlıklı ağ kopolimeri üretecek çapraz bağlama reaksiyonları metilstiren monomer sınırlar. 5,6 metilstiren monomer sadece bir vinilik fonksiyonel grubun varlığı kükürt kopolimer sağlar ısıtılmış ve oligomerik radikallerin oluşumunu teşvik nanoparçacık sentezi sırasında paralel olarak sıvı çözücü ve kükürt kaynağı olarak faaliyet göstermektedir. 5 Spesifik olarak, kükürt, polimer doğrusal yapılı sıvı sülfür diradikal forma geçiş S 8 halka olur, 150 ° C, kükürt elementi ısıtılması ile elde edilir. Daha sonra, metilstiren i enjekte edilir<html> 5 metilstiren çift bağ, Şekil 1 &#39;de gösterildiği gibi, kopolimer üretmek üzere kükürt zincirleri ile reaksiyona giren kükürt atomu metilstiren moleküllerinin 1:50 mol oranında sıvı sülfür nBu.. 5 kükürt kopolimeri daha sonra soğutuldu ve kadmiyum ön-madde olan eklendi. Bu karışım daha sonra çözelti içinde, 200 ° C&#39;ye ısıtılmış bu süre boyunca, kükürt kopolimeri erir ve nanoparçacık çekirdeklenme ve büyüme prosesleri başlatılmış olan 5 A 20:. Kadmiyum ön kükürt 1 mol oranı kullanıldığında, sadece bazı şekilde kükürt reaksiyon sırasında tüketilir. 5 bu kopolimer, reaksiyon sona erdiğinde, katı bir polimer matrisi içinde süspansiyon haline getirilerek nano partikülleri stabilize eder. 5 kopolimer sentezden sonra çıkarılabilir olmayan CdS nanopartiküllerin üretimi ile sonuçlanan Şekil 2&#39;de tasvir edildiği gibi, organik koordine ligandlar. 5 ontent &quot;&gt; Bu çalışmada sunulan sentetik yöntem literatürde diğer yöntemlerle karşılaştırıldığında nispeten basit 1 -.. 3,7 geleneksel bağlandı nanopartiküller sorunlu ya da istenmeyen kanıtlanmıştır nerede uygulamaların çeşitli bir yelpazede için geçerli olan bu teknik can nanopartiküllerin bir serisi, karmaşık ve zaman işlemleri soyma veya değişim ligand alıcı gerek kalmadan takip eden functionalizations tam bir spektrumunun incelemek için kullanılabilir daha yüksek verim test açık kapı. 2,4,8,9 Bu bağlanmamış nanopartiküller imkanı da sunmaktadır karbon kaynağı ortadan kaldırarak yaygın basılı nanoparçacık cihazlarda görülen karbon kusurları sayısını azaltmak için - 10. 16 Bu ayrıntılı bir protokol diğerleri bu yeni yöntemi uygulamak yardımcı olmak ve bulacaksınız alanlarda çeşitli aktif kullanımını teşvik yardımcı olmak için tasarlanmıştır özel önem bu.

<table>
	<tbody>
		<tr>
			<td>Sulfur (S8), 99.5%</td>
			<td>Sigma Aldrich</td>
			<td>84683</td>
			<td></td>
		</tr>
		<tr>
			<td>&#945;-methylstyrene, 99%</td>
			<td>Sigma Aldrich</td>
			<td>M80903</td>
			<td></td>
		</tr>
		<tr>
			<td>Cadmium acetylacetonate (Cd(acac)), 99.9%</td>
			<td>Sigma Aldrich</td>
			<td>517585</td>
			<td>Highly Toxic</td>
		</tr>
		<tr>
			<td>Chloroform (CHCl3), 99.5%</td>
			<td>Sigma Aldrich</td>
			<td>C2432</td>
			<td></td>
		</tr>
		<tr>
			<td>Hotplate / magnetic stirrer</td>
			<td>IKA RCT&#160;</td>
			<td>3810001</td>
			<td></td>
		</tr>
		<tr>
			<td>Temperature controller with probe and heating mantle</td>
			<td>Oakton Temp 9000</td>
			<td>WD-89800</td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifuge</td>
			<td>Beckman Coulter Allegra X-22</td>
			<td>392186</td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifuge Tubes</td>
			<td>Thermo Scientific</td>
			<td>3114</td>
			<td>Teflon for resistance to chlorinated solvents</td>
		</tr>
		<tr>
			<td>TEM with attached EDS detector</td>
			<td>FEI Tecnai G2 F-20 with EDAX detector</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>TEM Sample Grid</td>
			<td>Ted Pella</td>
			<td>1824</td>
			<td>Ultrathin carbon film substrate with holey carbon support films on a 400 mesh copper grid</td>
		</tr>
		<tr>
			<td>XRD</td>
			<td>Bruker F-8 Focus Diffractometer</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Molybdenum coated soda lime glass substrates</td>
			<td></td>
			<td></td>
			<td>750 nm thick sputtered molybdenum layer</td>
		</tr>
		<tr>
			<td>Quartz Fluorescence Cuvettes</td>
			<td>Sigma Aldrich</td>
			<td>Z803073</td>
			<td>10 mm by 10 mm, 4 polished sides with screw top</td>
		</tr>
		<tr>
			<td>UV-Vis-NIR</td>
			<td>Perkin Elmer Lambda 1050 Spectrometer</td>
			<td></td>
			<td>With 3D WB Detector Module</td>
		</tr>
		<tr>
			<td>PL</td>
			<td>Horiba FL3-21tau Fluorescence Spectrophotometer</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

synthesis of ligand-free cds nanoparticles within a sulfur copolymer matrix

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature solvents. These coordinating ligands help solubilize and stabilize the nanoparticles while in solution, and can influence the resulting size and reactivity of the nanoparticles during their formation. Despite the ubiquity of using ligands during synthesis, the presence of aliphatic ligands on the nanoparticle surface can result in a number of problems during the end use of the nanoparticles, necessitating further ligand stripping or ligand exchange procedures. We have developed a way to synthesize cadmium sulfide (CdS) nanoparticles using a unique sulfur copolymer. This sulfur copolymer is primarily composed of elemental sulfur, which is a cheap and abundant material. The sulfur copolymer has the advantages of operating both as a high temperature solvent and as a sulfur source, which can react with a cadmium precursor during nanoparticle synthesis, resulting in the generation of ligand free CdS. During the reaction, only some of the copolymer is consumed to produce CdS, while the rest remains in the polymeric state, thereby producing a nanocomposite material. Once the reaction is finished, the copolymer stabilizes the nanoparticles within a solid polymeric matrix. The copolymer can then be removed before the nanoparticles are used, which produces nanoparticles that do not have organic coordinating ligands. This nascent synthesis technique presents a method to produce metal-sulfide nanoparticles for a wide variety of applications where the presence of organic ligands is not desired.

Şekil 3a TEM görüntüsü kükürt kopolimeri tamamen kaldırılmıştır önce kükürt kopolimer içinde çekirdekli olan küçük CdS nanopartiküller (3-4 nm) gösterir. Şekil 3a&#39;da görüntü çözeltisi 200 ° C&#39;ye ulaştığında hemen sonra nanopartikül çözeltisinin bir bölümü alınarak elde edildi. Şekil 3b, kükürt kopolimeri tamamen olmuştur önce 30 dakika süre ile çözelti içinde büyüdü büyük nano-tanecikleri (7-10 nm) göstermek...

Watch this Scientific Journal Video about Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix at JoVE.com

Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix

Herein we present a method to synthesize ligand-free cadmium sulfide (CdS) nanoparticles based on a unique sulfur copolymer. The sulfur copolymer operates as a high temperature solvent and a sulfur source during the nanoparticle synthesis and stabilizes the nanoparticles after the reaction.

Bir Kükürt Kopolimer Matrix içinde ligand-serbest CdS Nanopartiküller Sentezi

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature ...

synthesis-ligand-free-cds-nanoparticles-within-sulfur-copolymer

Research

JoVE Journal

Chemistry

9.4K Görüntüleme.  University of Washington. Herein we present a method to synthesize ligand-free cadmium sulfide (CdS) nanoparticles based on a unique sulfur copolymer. The sulfur copolymer operates as a high temperature solvent and a sulfur source during the nanoparticle synthesis and stabilizes the nanoparticles after the reaction.

Video: Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix

Seeded Synthesis of CdSe/CdS Rod and Tetrapod Nanocrystals

We demonstrate a method for the synthesis of multicomponent nanostructures consisting of CdS and CdSe with rod and tetrapod morphologies. A seeded synthesis strategy is used in which spherical seeds of CdSe are prepared first using a hot-injection technique. By controlling the crystal structure of the seed to be either wurtzite or zinc-blende, the subsequent hot-injection growth of CdS off of the seed results in either a rod-shaped or tetrapod-shaped nanocrystal, respectively. The phase and morphology of the synthesized nanocrystals are confirmed using X-ray diffraction and transmission electron microscopy, demonstrating that the nanocrystals are phase-pure and have a consistent morphology. The extinction coefficient and quantum yield of the synthesized nanocrystals are calculated using UV-Vis absorption spectroscopy and photoluminescence spectroscopy. The rods and tetrapods exhibit extinction coefficients and quantum yields that are higher than that of the bare seeds. This synthesis demonstrates the precise arrangement of materials that can be achieved at the nanoscale by using a seeded synthetic approach.

A protocol for the seeded synthesis of rod-shaped and tetrapod-shaped multicomponent nanostructures consisting of CdS and CdSe is presented.

We demonstrate a method for the synthesis of multicomponent nanostructures consisting of CdS and CdSe with rod and tetrapod morphologies. A seeded ...

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 ...

A Simple Method for the Size Controlled Synthesis of Stable Oligomeric Clusters of Gold Nanoparticles under Ambient Conditions

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like oligomeric clusters of these yellow nanoparticles of narrow size distribution are synthesized under ambient conditions via two methods. The delay-time method controls the number of subunits in the oligoclusters by varying the time between the addition of HAuCl4 to alkaline solution and the subsequent addition of reducing agent, NaSCN. The yellow oligoclusters produced range in size from ~3 to ~25 nm. This size range can be further extended by an add-on method utilizing hydroxylated gold chloride (Na+[Au(OH4-x)Clx]-) to auto-catalytically increase the number of subunits in the as-synthesized oligocluster nanoparticles, providing a total range of 3 nm to 70 nm. The crude oligocluster preparations display narrow size distributions and do not require further fractionation for most purposes. The oligoclusters formed can be concentrated &#62;300 fold without aggregation and the crude reaction mixtures remain stable for weeks without further processing. Because these oligomeric clusters can be concentrated before derivatization they allow expensive derivatizing agents to be used economically. In addition, we present two models by which predictions of particle size can be made with great accuracy.

We describe a simple method for producing highly stable oligomeric clusters of gold nanoparticles via the reduction of chloroauric acid (HAuCl4) with sodium thiocyanate (NaSCN). The oligoclusters have a narrow size distribution and can be produced with a wide range of sizes and surface coats.

Ortam Koşullarında Altın Nanopartiküller Kararlı Oligomerik Kümeleri Boyut Kontrollü Sentezi için Basit Bir Yöntem

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like ...

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

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

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

CdSe @ CdS nanorods üzerinde İridyum Oksit Nanopartiküller Fotokimyasal Oksidatif Büyüme

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

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &#960;-&#960; Stacking Interactions

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE). Characterization of the copolymer revealed a narrow molecular distribution (PDI &#60; 1.03) and confirmed the degree of polymerization of mPEG122-b-(PheGE)15. The critical micelle concentration of the copolymer was evaluated using an established fluorescence method with the aggregation behavior evaluated by dynamic light scattering and transmission electronic microscopy. The potential of the copolymer for use in drug delivery applications was evaluated in a preliminary manner including in vitro biocompatibility, loading and release of the hydrophobic anti-cancer drug doxorubicin (DOX). A stable micelle formulation of DOX was prepared with drug loading levels up to 14% (wt%), drug loading efficiencies &#62; 60% (w/w) and sustained release of drug over 4 days under physiologically relevant conditions (acidic and neutral pH, presence of albumin). The high drug loading level and sustained release is attributed to stabilizing &#960;-&#960; interactions between DOX and the core-forming block of the micelles.

The key steps of living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE) are described. The resulting block copolymer micelles (BCMs) were loaded with doxorubicin 14% (wt%) and sustained release of drug over 4 days under physiologically relevant conditions was obtained.

π-π İstifleme etkileşimlerle Stabilize blok kopolimer miselleri hazırlanması için bir amfifilik kopolimerin anyonik polimerizasyonu

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl ...

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 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 ...

Molten-Salt Synthesis of Complex Metal Oxide Nanoparticles

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. Here, we introduce the molten-salt synthesis (MSS) method for making metal oxide nanomaterials. Advantages over other methods include its simplicity, greenness, reliability, scalability, and generalizability. Using pyrochlore lanthanum hafnium oxide (La2Hf2O7) as a representative, we describe the MSS protocol for the successful synthesis of complex metal oxide nanoparticles (NPs). Furthermore, this method has the unique ability to produce NPs with different material features by changing various synthesis parameters such as pH, temperature, duration, and post-annealing. By fine-tuning these parameters, we are able to synthesize highly uniform, non-agglomerated, and highly crystalline NPs. As a specific example, we vary the particle size of the La2Hf2O7&#160;NPs by changing the concentration of the ammonium hydroxide solution used in the MSS process, which allows us to further explore the effect of particle size on various properties. It is expected that the MSS method will become a more popular synthesis method for nanomaterials and more widely employed in the nanoscience and nanotechnology community in the upcoming years.

Here, we demonstrate a unique, relatively low-temperature, molten-salt synthesis method for preparing uniform complex metal oxide lanthanum hafnate nanoparticles.

Karmaşık Metal Oksit nano tanecikleri erimiş tuz sentezi

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of their interactions with cell membranes, lipid bilayers, and viruses. The hydrophilic ligands make these particles colloidally stable in aqueous solutions and the combination with hydrophobic ligands creates an amphiphilic particle that can be loaded with hydrophobic drugs, fuse with the lipid membranes, and resist nonspecific protein adsorption. Many of these properties depend on nanoparticle size and the composition of the ligand shell. It is, therefore, crucial to have a reproducible synthetic method and reliable characterization techniques that allow the determination of nanoparticle properties and the ligand shell composition. Here, a one-phase chemical reduction, followed by a thorough purification to synthesize these nanoparticles with diameters below 5 nm, is presented. The ratio between the two ligands on the surface of the nanoparticle can be tuned through their stoichiometric ratio used during synthesis. We demonstrate how various routine techniques, such as transmission electron microscopy (TEM), nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA), and ultraviolet-visible (UV-Vis) spectrometry, are combined to comprehensively characterize the physicochemical parameters of the nanoparticles.

Amphiphilic gold nanoparticles can be used in many biological applications. A protocol to synthesize gold nanoparticles coated by a binary mixture of ligands and a detailed characterization of these particles is presented.

Amphiphilik altın nanopartiküller sentezi ve karakterizasyonu

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...