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.

注意:镉的前体是剧毒，必须非常小心处理。佩戴合适的防护设备，采用适当的工程控制，并咨询有关材料安全数据表（MSDS）。此外，纳米颗粒的生成可能存在额外的危害。本文所描述的反应是用标准真空气体歧管进行的，以便在惰性气氛中进行的实验。所有的化学品均商购并且原样使用。这个协议是基于一个先前开发的合成方法，这是我们最近别处所述。5 1.硫共聚物合成<ol><li> 熔火之元素硫的制备 <ol><li>地方元素硫（4克，124.8毫摩尔，S 8，99.5％）与一个附加冷凝器和温度探头50毫升三颈烧瓶中。用真空和氮气数次执行泵和吹扫循环。 </li><li>氮气下热至150℃，搅拌，这将导致硫成为黄色液体。 </li></ol></li><li> 硫共聚物的制备 <ol><li>一旦所有的硫的溶解到液体，立即注入α甲基苯乙烯（330微升，2.5毫摩尔，99％）到溶液中。 </li><li>热溶液至185℃，以500rpm搅拌10分钟。作为共聚物的形式，该解决方案将从黄色变色到橙色，终于产生深红色。 </li><li>除去从热溶液中，并冷却到室温。当其冷却时，共聚物会慢慢结晶，以形成一种橙色橡胶状固体。在此阶段，该共聚物可以在室温下保存用于随后的合成，或者可以立即使用。 </li></ol></li></ol> 2.硫化镉纳米粒子合成<ol><li>乙酰丙酮镉（Cd的（ACAC），900毫克，2.9毫摩尔99.9％）来自前面步骤添加到三颈烧瓶中，以使粉末放置均匀地涂在固体硫共聚物（4.0克，116毫摩尔）的顶部。 </li><li>上用氮气和真空几次烧瓶执行泵和吹扫循环。 </li><li>加热在氮气下将溶液至200℃，同时搅拌。硫共聚物会熔化并与镉前体混合，并在纳米颗粒成核和生长过程将开始。 </li><li>允许纳米颗粒中生长30分钟。 注:改变反应时间会影响纳米粒子的生长，所以有可能调整纳米颗粒的最终尺寸5所述的30分钟的反应时间将与7-10纳米的尺寸范围为5 </li><li>除去从热溶液中，并允许冷却到室温。 </li><li>一旦冷却，取出从烧瓶中并储存在室温下的固体纳米复合材料。 </li></ol> 3.除去硫共聚物和隔离纳米粒子<ol><li> 硫磺共聚物的去除 </s仲&gt; <ol><li>放置所述纳米复合材料（200毫克）在20毫升玻璃小瓶中，并添加氯仿（20毫升）中。 </li><li>在放置1小时超声波发生器和超声小瓶，打破了纳米复合材料，并暂停该解决方案中的纳米粒子。 </li><li>分离溶液进入两台30毫升离心管中，另外20毫升氯仿添加到每个。 </li><li>离心在8,736×g离心15分钟将溶液（相对离心力）。 </li><li>从离心管中倒出硫共聚物，确保不打扰解决纳米粒子。 </li></ol></li><li> 所述纳米粒子的隔离 <ol><li>加入氯仿至每个离心管（30ml）中，并超声处理15分钟，再分散安定纳米颗粒。 </li><li>重复部分3.1.4，3.1.5和3.2.1三次以上描述，以确保所有的硫共聚物的已被删除的步骤。一旦所有的硫共聚物被移除，滗析溶液将没有罗手指有一个橙色。 </li><li>加入氯仿（2ml）中于每个离心管中收集的最终纳米颗粒。 </li><li>结合所收集的纳米颗粒在一个20ml玻璃瓶（4 ml溶液总）和放置玻璃小瓶在真空下除去所有氯仿和干燥的纳米颗粒。在这个阶段，将所得的纳米粒子的质量可以被确定并以确定使用的起始原料和产物的摩尔比，反应的产率相比，前体的起始物质。 </li></ol></li></ol> 4.表征纳米CdS <ol><li> 透射电子显微镜 <ol><li>稀释在氯仿分离的纳米颗粒（20毫克）（20毫升）和ultrasonicate 1小时。 </li><li>稀释15分钟的氯仿该溶液（5滴/ 5毫升）和超声处理。 </li><li>放下最后的解决方案与上一个400多孔碳支持膜超薄碳薄膜基材目铜透射电子显微镜（TEM）栅格。 </li><li>放置TEM网格在玻璃小瓶中并在真空下保持过夜，以从样品中除去任何残留的溶剂。 </li><li>一旦干燥完成后，使用200千伏的加速电压，为3的光点尺寸和一个附加的能量色散X射线光谱（EDS）的检测器获得的TEM图像。 </li></ol></li><li> X射线衍射 <ol><li>稀释在氯仿中分离纳米颗粒（10毫克/毫升）。 </li><li>清洁镀钼的钠钙玻璃基片（1 平方厘米）通过超声处理在洗涤剂，去离子水，丙酮和异丙醇中，每个10分钟。最后，清洁的空气等离子清洗基板的下降铸造前10分钟。 </li><li>从跌落4.2.1 7μl递增投的解决方案在底材上的4.2.2。 </li><li>一旦电影已经干涸，获得X射线衍射（XRD）数据。在扫描速度收集使用7000个数据点的数据每秒1数据点用铜的KαX射线源和1.54059埃的入射波长。 </li></ol></li><li> 光谱解决方案 <ol><li>分散在氯仿中，声处理分离的纳米颗粒（0.1毫克/毫升）30分钟，发生的样品在密封的石英杯中。 </li><li>驱散从第2.6节所述纳米复合材料和从部分1.2.3中的甲酰胺的硫共聚物（1毫克/毫升），搅拌在700rpm，并加热至70℃，以促进该材料的悬浮液中。 </li><li>获得的光致发光（PL）和吸收光谱对所有三个样品。进行使用分光计光学吸收测量与横跨紫外线，可见光和近红外范围（UV-VIS-NIR）延伸的三检测器。使用荧光分光光度计以330nm的激发波长进行PL测量。 注:表征使用部分讨论了纳米技术的具体协议4.1.5，4.2.4，一ND 4.3.2变化很大，取决于所使用的特定设备的性质，所以我们在座的只是一般的特性参数。有兴趣的读者是针对几个综述文章使用这些分析技术的CdS纳米粒子有关的详细信息17 - 19 </li></ol></li></ol>

<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 use of methylstyrene and in the appropriate concentration is important to form the copolymer that can be stored as a powder at room temperature, and then be heated to produce a liquid to allow the nanoparticle synthesis to occur. During the synthesis, only some of the sulfur reacts with the cadmium precursor, while the remainder stays within the sulfur copolymer.5 Once the reaction solution is cooled and solidified, this procedure produces CdS nanoparticles suspended within a sulfur copolymer matrix.5 The copolymer can subsequently be removed, producing nanoparticles that do not have conventional organic ligands.5 A limitation of our method however, is that once the copolymer is removed, the nanoparticles are prone to aggregation, which can be prevented when conventional organic ligands are present. This makes it difficult to control the self-assembly of our nanoparticles during film formation. The nanoparticle size can be tuned by varying the reaction time, although another limitation is that this method produces nanoparticles with a higher level of polydispersity in size than conventional techniques,5,18 which broadens the absorption and emission spectra of our nanoparticles.
This nascent synthesis method can be useful in a range of fields where the presence of conventional aliphatic ligands diminishes the charge transfer or surface reaction properties of the nanoparticles. Furthermore, this synthesis method is relatively simple in comparison to other methods that require multistep ligand exchange or ligand stripping procedures to remove conventional aliphatic ligands.1-4 For example, one set of nanoparticles could be functionalized with a range of ligands to produce nanoparticles with a spectrum of different properties.9 In addition, this method could be used to produce nanoparticle based devices where the presence of organic ligands would otherwise introduce unwanted carbon impurities.10,12

虽然证明对合成是有用的，常规的脂族配位体存在许多用于纳米颗粒的光子和电化学装置的实施挑战。脂肪族配体高度绝缘，疏水性，并构成显著障碍电化学表面反应。1因此，一些研究已经开发了配体交换和配体剥离与功能部分或剥去配体取代这些脂肪族配体的协议，露出了光秃秃的纳米粒子表面1 - 3这些反应，但是，提出几个问题的内在。它们显著添加到合成过程的复杂性，不总是进行完全，并能恶化的纳米颗粒，使用这些技术时，器件制造过程中，可反过来强加显著问题的表面上。4 我们已经开发了硫共聚物，其可以用作硫化镉纳米粒子的合成过程中既高温溶剂和硫源。5该共聚物是基于由。Chung等人 ，使用元素硫和1,3-二异丙烯基苯（DIB）开发的网络共聚物。6在我们的情况下，甲基单体实现的，而不是DIB。的甲基单体限制交联反应，否则将产生一个高的分子量网络共聚物。5,6-只有一个乙烯基官能团的对甲基苯乙烯单体的存在促进形成低聚自由基一旦加热，这使得硫共聚物具体操作为并联纳米颗粒合成过程中的液体溶剂和硫源5，硫聚合物通过元素硫加热至150℃，这将导致在S 8环转变到线性结构液体硫双基形式产生。接下来，甲基注入我<html> n要在甲基分子与硫原子1:50摩尔比液体硫。5所述的甲基双键与硫链反应产生的共聚物，如在图1中。5硫共聚物，然后冷却和镉前体加入。然后将该混合物再加热到200℃，在此期间，硫共聚物熔化，并在纳米颗粒成核和生长过程发起的溶液内5 A 20:是用来硫镉前体的摩尔比为1:1，所以，只有某些硫在反应过程中消耗掉。5该共聚物由一旦反应已终止的固体聚合物基质中悬浮它们稳定纳米颗粒。5的共聚物可以在合成之后被去除，导致生产不具有的CdS纳米粒子的有机配位配体，如在图2 5所示内容】"&gt;在这项工作中提出的合成方法是比较简单的，在文献中提出的其它方法的比较。1 - 3,7在传统连接的纳米颗粒已被证明存在问题，或不希望的，适用于不同范围的应用这种技术可以打开大门更高吞吐量测试，其中一个批次纳米粒子可用于检查后续functionalizations的完整频谱，而不需要复杂且耗时的配位体剥离或交换过程。2,4,8,9这些未连接的纳米颗粒也提供机会通过消除碳源，以减少印刷纳米器件通常观察到的碳缺陷的数量。10 - 16本详细的协议旨在帮助他人实施这种新方法，并帮助推动各种会发现场的积极使用它具有特殊的意义。

<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.

在图3a的TEM图像显示了已硫共聚物内成核之前的硫共聚物已被完全除去小的CdS纳米粒子（3-4纳米）。在图3a中的图像通过取纳米颗粒溶液的等分试样后，立即将溶液达到200℃获得的。 图3b示出已在溶液中生长30分钟的硫共聚物已经完全以前大纳米颗粒（7-10纳米）除去。 图3c示出图3b中的突出显示区域的更高放大率的图像。在图3c一种纳米颗粒具有测得为3.3埃的特别清楚原子面间隔。 3.3埃的原子面间隔是具有闪锌矿硫化镉或纤锌矿的CdS的（002）面间距的（111）面间距是一致的。 图3D示出，一旦硫共聚物完全除去并溶解在氯仿中，纳米颗粒会聚集在一起。在图3d给出的EDS数据证实硫 ​​化镉的化学计量（接近1:1），并确认该硫共聚物已被有效去除。 在先前的出版物中，我们使用傅立叶变换红外光谱（FTIR）和质子核磁共振谱（1 H NMR）表明，一旦硫共聚物是完全除去，这些纳米颗粒不具有传统的有机配体。5一项研究通过纳格等。人发现，金属硫化物纳米颗粒可以与阴离子硫物质被有效地连接。7，我们断定，纳米颗粒使用这种方法也同样构成的纳米颗粒表面上的硫物种进行。在图3d给出的EDS数据表明有轻微的化学计量过量的硫，这是按照与硫物种对nanopar存在察员的表面。 为降铸纳米颗粒薄膜的X射线衍射图案示于图4，并与纤锌矿的形成相一致，还可能闪锌矿结构的CdS。设在26.6度的峰对应于3.3埃的原子面间隔，它与闪锌矿硫化镉或纤锌矿的CdS的（002）面间距的（111）面间距一致，证实了在TEM看到的平面间距图3c的图像。 使用UV-Vis光谱， 如图5中的硫共聚物和纳米复合材料进行了分析。由于每个分散体的浓度相等时，数据表明，该纳米复合材料显示出在比较的显著增强吸光度仅硫共聚物。在图6示出呈现的光致发光的数据，该纳米复合材料表现出峰，它是从散装蓝移硫化镉带隙（510纳米，2.4电子伏特），而硫共聚物峰是比较小的。 分离的纳米颗粒也使用紫外-可见-近红外和PL光谱一旦硫共聚物除去检验。 图7示出了既在UV-VIS-NIR和PL数据。在图6中，纳米颗粒具有在硫化镉的体材料带隙和小吸收边缘是在450-550纳米范围内的相应的宽吸收光谱为中心的广泛的PL峰。一旦硫聚合物被除去，所述纳米颗粒表面不再钝化并包含由于悬空键的存在表面缺陷。这导致新的表面介导的能量状态的存在是随后相比于在图5和6的纳米复合材料呈现的光谱拓宽和红移的PL及吸收光谱18,20 - 22另外，在显示出量子限制效应，这也拓宽了光谱的纳米颗粒群体的纳米颗粒的结果的多分散性。23因此，与我们以前的工作相结合，这个数据支持权利要求，这些纳米颗粒不具有传统的缺陷钝化一旦有机配体硫共聚物被除去。5此外，该数据表明，硫共聚物之前的去除钝化的CdS纳米粒子的表面上的缺陷。 <img alt="图1" src="/files/ftp_upload/54047/54047fig1.jpg" /> 图硫共聚物的合成1和结构，元素硫被加热产生线性结构的液态硫双基，其与甲基产生硫共聚物反应。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54047/54047fig1large.jpg" target="_blank">请点击此处查看大图</a>这一数字。 <img alt="图2" src="/files/ftp_upload/54047/54047fig2.jpg" /> 图2.纳米粒子生长和隔离。硫化镉纳米粒子核和硫共聚物内生长。一旦反应完成，硫共聚物被删除，产生无配体硫化镉纳米粒子。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54047/54047fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" src="/files/ftp_upload/54047/54047fig3.jpg" /> 图3孤立的CdS纳米粒子的TEM图像。 一个 ）3-4纳米的CdS纳米粒子开始共聚物内生长。B）7-10一旦终止反应纳米颗粒。小号共聚物仍然存在在这个阶段。 三 ）突出放大图像在B，D区）的去除量S共聚物后TEM照片。插图显示EDS数据。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54047/54047fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图4" src="/files/ftp_upload/54047/54047fig4.jpg" /> 图4.硫化镉纳米颗粒薄膜的XRD图。XRD图形与纤锌矿或闪锌矿的CdS的形成是一致的。钼峰由于基板。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54047/54047fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图5" src="/files/ftp_upload/54047/54047fig5.jpg" /> 图硫共聚物纳米复合材料5吸收光谱，纳米复合材料表现出signif相比于单独的硫共聚物icantly增强吸收峰。这两种材料具有相同浓度而分散。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54047/54047fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图6" src="/files/ftp_upload/54047/54047fig6.jpg" /> 图6.光致发光光谱硫共聚物和纳米复合材料。纳米复合材料表现出的峰值是蓝移从CD的大部分带隙（510纳米，2.4伏特），而硫共聚物呈现相对较少的光致发光。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54047/54047fig6large.jpg" target="_blank">请点击这里查看更大的版本这个数字。</a> <img alt="图7" src="/files/ftp_upload/54047/54047fig7.jpg" /> Figu7.重无配体的CdS纳米粒子的吸收和光致发光光谱。该PL数据显示，在510 nm处的宽峰。紫外-可见-近红外数据显示，在450-550纳米范围内的弱吸收肩膀较宽的吸收曲线。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54047/54047fig7large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

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.

a硫磺共聚物基质内的免费配体硫化镉纳米粒子的合成

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

Nanyang Technological University

Research

JoVE Journal

Chemistry

9.4K 次观看.  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.

视频: 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.

硒化镉/硫化镉棒和纳米四脚合成种子

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

科研

化学

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.

单金属和双金属前过渡金属碳化物和氮化物纳米粒子的反相微乳液介导的合成

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.

合成，表征和混合金/硫化镉和Au / ZnS核/壳纳米颗粒功能化

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.

根据环境条件的金纳米粒子的稳定低聚簇的大小控制合成的一种简便方法

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.

铱氧化物纳米颗粒对硒化镉硫化镉@纳米棒光化学氧化增长

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.

一个两亲性共聚物的阴离子聚合通过π-π堆积作用稳定嵌段共聚物胶束的制备

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.

半导体回转金属硫框架结晶的硫醇构建块的合成

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.

离子液体中双金属 Pt/锡基纳米粒子的合成

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.

复合金属氧化物纳米粒子的熔融盐合成

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.

两栖金纳米粒子的合成与表征

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