这项研究是由计划和预算委员会和以色列科学基金会（批准号:十一分之一百五十二）的I-CORE项目的支持。我们感谢化学的Schulich商学院与Technion工业 - 以色列理工学院的实验室装修和启动包。我们也感谢皇家化学学会的许可，从https://dx-doi-org.remotexs.ntu.edu.sg/10.1039/C4TA06164K适应材料在这个手稿中使用。 Kalisman博士感谢他们的支持Schulich商博士后研究。我们感谢亚龙考夫曼博士为他的HR-TEM和HAADF以及Kamira Weinfeld博士协助她与XPS表征援助。

1.量子点21的合成<ol><li> TOP的制备:Se前体<ol><li>在用隔膜小瓶结合58毫克硒粉末与0.360克三正辛基膦（TOP）中。 </li><li>超声振荡顶部:硒混合物，直到它是一个没有明确的固体。 </li></ol></li><li>硒化镉的合成<ol><li>结合3.0克三辛基氧化膦（TOPO），280毫克正 - 十八烷基酸（ODPA），和60毫克的CdO在装有热电偶25毫升三颈圆底烧瓶3毫米×8 mm的圆柱形搅拌棒（插入定制玻璃适配器），回流冷凝器用T型接头（中心颈），和橡胶隔膜。组装所有玻璃 - 玻璃接头高温真空润滑脂。 T型接头连接到一个端部的Schlenk线，可以清洁的惰性气体和真空之间进行切换，在连接的另一端，以鼓泡。 注意:氧化镉是非常有毒的，应称重并加入到圆底烧瓶中的封闭的env内ironment诸如手套箱。 </li><li>放置圆底烧瓶装置以加热套，并与惰性气体吹扫。 </li><li>加热该固体在圆底烧瓶至150℃，并确保以开始剧烈搅拌一次化合物熔化（约60-80℃）。为了避免超过目标温度，加热至100℃，然后150℃，一旦加热速度减慢或稳定。 </li><li>脱气在真空下将该混合物（在150℃）为至少1小时，同时仍然搅拌。确保T型接头是不对外开放的起泡或油会被吸进瓶中，舒伦克线。当从气体移动到真空小心地慢慢过渡，以避免超过沸腾了。 </li><li>重新填充有惰性气体的烧瓶（并继续流动气体在样品），并升高温度到350℃。该溶液应该打开清楚它加热，并在烧瓶壁过量固体可以通过在烧瓶小心旋流收集。 </LI&gt; <li>注入1.5克顶部进入通过隔膜烧瓶中。使溶液温度，然后再继续稳定。 注:尽量减少空气/湿气通过保持在惰性气氛下的隔膜小瓶的顶部，并尽可能快地注入其注入量。 </li><li>注入所有的TOP:硒混合物（在第1.1节中制备）进入通过隔膜的烧瓶中，使用宽针注入TOP:硒作为快速且均匀越好。 </li><li>来进行反应所需的时间，并从加热套除去。 <ol><li>对于非常小的种子刚刚注射前，离火。对于较大的种子取出注射TOP后，立即从热烧瓶:硒或等待长达3分钟后。再等导致更大的种子。 </li></ol></li><li>使反应冷却到约100℃，并注入大约5毫升脱气的甲苯中。转移溶液至小瓶惰性气氛下进行清洁。 没有德:为了简化此过程10ml甲苯可以放置在20ml的小瓶在惰性气体的恒定流动的隔片。使用大约一半的甲苯，注入到冷却的混合物，然后将冷却的混合物转移回该小瓶中。 </li><li>种子清洗<ol><li>放入50毫升的离心管中的溶液。 </li><li>加甲醇（约5毫升）以沉淀出从甲苯混合物的种子。 </li><li>离心3,400 XG 5分钟。 </li><li>滗澄清的上清液并再溶解在甲苯中沉淀（5-10）溶液中。 </li><li>重复步骤总通过1.2.10.2在1.2.10.4至少三次。 </li></ol></li><li>稀释在甲苯中的种子中的一小等分试样以测量350-800纳米之间紫外可见（UV-VIS）吸收。使用峰来确定，如在文献22中描述的硒化镉种子的浓度和大小。 </li></ol></li></ol> 2.去籽罗的合成DS 21 <ol><li> TOP的制备:•前兆<ol><li>用搅拌棒的小瓶结合1.2克的S用15g的顶部。 </li><li>搅拌至清无物（通常至少24小时）。 </li><li>测量0.62克该混合物与隔膜的小瓶。 </li></ol></li><li> TOP的制备:硒化镉前体<ol><li>测量从步骤1的CdSe种子的适当体积（基于紫外可见峰）与隔膜的小瓶。 注意:对于5×10计算浓度-5 2.25纳米的种子（从UV-Vis光谱22算出这两个值），使用300微升的溶液。 </li><li>使用真空线，直到种子干燥蒸发甲苯。真空下不要离开超过5-10分钟一次干，因为这会降低种子的质量。 </li><li>重新溶解所有的干种子的于0.5g TOP的。 </li></ol></li><li>硒化镉@ CDS的合成<ol><li>结合60毫克丙基酸（PPA），3.35克TOPO，1.080克O​​DPA和230毫克的CdO在装有热电偶（插在定制玻璃适配器）25毫升三颈圆底烧瓶3毫米×8 mm的圆柱形搅拌棒，回流冷凝器用T型接头（中心颈），以及橡胶隔膜。组装所有玻璃 - 玻璃接头高温真空润滑脂。 T型接头连接到一个端部的Schlenk线，可以清洁的惰性气体和真空之间进行切换，在连接的另一端，以鼓泡。 注意:氧化镉是非常有毒的，应称重并加入到圆底封闭的环境里，例如一个手套箱。 PPA在一些国家调节，并且可以通过丁基膦酸（BPA，72毫克），或己基膦酸（HPA，80毫克）代替，虽然双酚A和HP​​A通常导致较短的杆。 </li><li>放置圆底烧瓶装置以加热套，并与惰性气体吹扫。 </li><li>加热在圆底烧瓶中，以120℃的固体，并确保以开始剧烈搅拌一旦化合物 -DS熔体（约60-80℃）。为了避免超过目标温度，加热至90℃，然后120℃，一旦加热速度减慢或稳定。 </li><li>脱气在真空下将该混合物（在120℃）为至少半小时，同时仍然搅拌。 <ol><li>确保T型接头是不对外开放的起泡或油会被吸进瓶中，舒伦克线。当从气体移动到真空小心地慢慢过渡，以避免超过沸腾了。使用冷阱液氮（LN 2）较好的真空度。 </li></ol></li><li>重新填充有惰性气体的烧瓶（并继续流动气体在样品），并升高温度至320℃。该溶液应该打开清楚它加热，并在烧瓶壁过量固体可以通过在烧瓶小心旋流收集。 </li><li>冷却回落到120℃，并在真空下脱气如在步骤1.2.4。 </li><li>笔芯和再加热烧瓶步骤1.2.5。 </li><li>注入1.5克顶部进入通过隔膜烧瓶中。使溶液温度继续之前在340℃稳定。 注:尽量减少空气/湿气通过保持在惰性气氛下的隔膜小瓶的顶部，并尽可能快地注入其注入量。 </li><li>注入TOP:•混合物到烧瓶中通过隔膜，使用宽针注入TOP:作为快速且均匀š越好。启动计时器。 </li><li>注射后上方正好20秒:S，注入TOP:的CdSe混合物到烧瓶中通过隔膜，使用宽针注入TOP:的CdSe作为快速且均匀越好。 注:温度应该由这点低于330℃下降到由于加入的RT TOP溶液。 </li><li>设定温度至320℃，并让反应继续进行所需时间（8-15分钟），并从加热套除去。 </li><li>让反应从加热套的冷却程Ð当温度达到大约100℃注入约5毫升脱气的甲苯中。转移溶液至小瓶惰性气氛下进行清洁。 注意:为了简化此过程10ml甲苯可以放置在20ml的小瓶在惰性气体的恒定流动的隔片。使用大约一半的甲苯，注入到冷却的混合物，然后将冷却的混合物转移回该小瓶中。 </li><li>棒清洗<ol><li>放入50毫升的离心管中的溶液。 </li><li>加甲醇（约5毫升）以沉淀出从甲苯混合物的种子。 </li><li>离心3,400 XG 5分钟。 </li><li>倒出上层清液，并在大约10毫升己烷重新溶解沉淀。 </li><li>加1-2毫升每个正辛胺和壬酸的溶液。该解决方案应该是透明的。 </li><li>加入5毫升甲醇和离心3,400×g下5分钟。 </li><li>重复步骤2.3.13.4通过2.3.13.6至少两次以上。 </li><li>在10ml甲苯中再溶解沉淀。如果沉淀不容易溶解，有可能需要更多的清洗步骤，在这种情况下，重复步骤2.3.13.4通过2.3.13.6。 </li><li>加大约7毫升异丙醇，加入1ml的时间，直至溶液混合，即使稍微混浊。 </li><li>离心以便从一切分开较长杆为2200 xg离心30分钟。 </li><li>再溶于10-15毫升甲苯沉淀。 </li></ol></li><li>稀释在甲苯中的种子中的一小等分试样以测量杆的紫外 - 可见吸收和/或光致发光（PL）。 注意:任何等份体积是可接受的，只要该稀释因子是已知的，然而，典型的稀释因子将是20。PL，吸收应等于或低于0.1在选定的激发波长（通常使用450纳米）。 </li></ol></li></ol> 3.晶种棒转移到水溶液<ol><li>准备工作甲醇溶液定量<ol><li>倾约10毫升甲醇入离心管中。 </li><li>加约250毫克的巯基十一酸（MUA）和400毫克氢氧化四甲铵（TMAH）。 </li><li>涡或让坐在直到所有的固体完全溶解。 </li></ol></li><li>配体交换<ol><li>加甲醇（5-10毫升，或足以沉淀杆），以¼从步骤2中的离心管合成杆的半。 注意:用于将依赖于甲苯的量杆的体积用于溶解用于存储的棒。如果使用10-15毫升作为步骤2.3.13.11建议，然后3-6毫升杆溶液要适当。 </li><li>离心3,400 XG 5分钟。 </li><li>弃去上清液。 </li><li>从3.1节到颗粒加入所有的甲醇溶液。 </li><li>旋涡或震动用手充分溶解。让溶液坐至少1小时以允许发生最大配体交换。 ñOTE:该溶液应静置至少1小时，即使它似乎立即和完全溶解</li><li>分离溶液进入两个离心管两半。 注:保存用于步骤3.1的离心管中，转移一半溶液加入到那里。 </li><li> 20ml甲苯添加到每个一半。如果存在醇与甲苯之间的相分离加甲醇逐滴直到相复合。 </li><li>离心7700 XG 15分钟。 </li><li>非常小心地倒出从颗粒的上层清液。 </li><li>小心倒置离心管，以干燥样品。 </li><li> 5毫升超纯水加入沉淀和储存在小瓶中铝箔（或其他不透明覆盖物）缠好。 注意:一旦移动从甲苯到水，杆不耐光的，这就是为什么它们都包括在内。即使保持在黑暗中的棒应尽快使用，并且不建议存储棒在水中超过一个月。 </li></ol></li></ol> 4.成长铱纳米粒子<ol><li>氢氧化钠<ol><li>在一个塑料小瓶中称出1450毫克氢氧化钠。在20ml超纯水中溶解的NaOH。解决方案应该是无固体清楚。 </li></ol></li><li>过硫酸钠<ol><li>在一个塑料小瓶中称出950毫克的钠硫2 O 8。钠硫溶解2 O 8在20毫升超纯水。解决方案应该是无固体清楚。 </li></ol></li><li>硝酸钠<ol><li>在一个塑料小瓶中称出300毫克的亚硝酸钠3.溶解硝酸钠的18ml超纯水。解决方案应该是无固体清楚。 </li></ol></li><li>铱前体解决方案<ol><li>在一个塑料瓶中称出50毫克的Na 3 IrCl 6。溶解的Na 3 IrCl 6与5.0mL超纯水。解决方案应该是透明的棕色（如苏格兰威士忌），无固体。 </li></ol></li><li>预样品paration <ol><li>放置在一个标准聚苯乙烯比色皿的分光搅拌器。 注意:由于该解决方案是非常基本的，石英等玻璃试管，不应使用。 </li><li>添加从步骤4.4.10.20毫升铱前体溶液。 </li><li>加入0.50毫升硝酸盐溶液从步骤4.3.1。 </li><li>在水中加0.30ml接种棒从第3（跟踪从配体交换甲苯可能引起试管壁上的混浊）。 </li><li>从步骤4.2.1添加0.50毫升过的解决方案。 </li><li>从步骤4.1.1添加0.50毫升的氢氧化钠溶液中。 </li></ol></li><li>样品照明<ol><li>放置反应杯在搅拌能力的保持器。 </li><li> 450纳米的光在100毫瓦长达4小时的照明。该解决方案应该变绿后蓝色。 </li></ol></li><li>采集样品<ol><li>倾溶液（但不搅拌棒）到离心管中。 </li><li>离心7700 XG 10分钟。 </li><li>关心从粒料，这应该是绿色或蓝色根据所选择的反应时间充分倒出上清液。 注:沉淀现在可以收集或通过超声处理分散在极性溶剂中在其它实验。 </li></ol></li></ol>

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G., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultrafast+Electron-Hole+Dynamics+in+Core/Shell+CdSe/CdS+Dot/Rod+Nanocrystals.">Ultrafast Electron-Hole Dynamics in Core/Shell CdSe/CdS Dot/Rod Nanocrystals.</a> Nano Lett. 8 (12), 4582-4587 (2008).</li><li>Raino, G., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Probing+the+Wave+Function+Delocalization+in+CdSe/CdS+Dot-in-Rod+Nanocrystals+by+Time-+and+Temperature-Resolved+Spectroscopy.">Probing the Wave Function Delocalization in CdSe/CdS Dot-in-Rod Nanocrystals by Time- and Temperature-Resolved Spectroscopy.</a> ACS Nano. 5 (5), 4031-4036 (2011).</li><li>Talapin, D. V., Lee, J. S., Kovalenko, M. V., Shevchenko, E. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Prospects+of+Colloidal+Nanocrystals+for+Electronic+and+Optoelectronic+Applications.">Prospects of Colloidal Nanocrystals for Electronic and Optoelectronic Applications.</a> Chem. Rev. 110 (1), 389-458 (2010).</li><li>Kraus, R. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Room-Temperature+Exciton+Storage+in+Elongated+Semiconductor+Nanocrystals.">Room-Temperature Exciton Storage in Elongated Semiconductor Nanocrystals.</a> Phys. Rev. Lett. 98 (1), 017401 (2007).</li><li>She, C., Demorti&#232;re, A., Shevchenko, E. 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W., Qu, L., Guo, W., Peng, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Experimental+Determination+of+the+Extinction+Coefficient+of+CdTe,+CdSe,+and+CdS+Nanocrystals.">Experimental Determination of the Extinction Coefficient of CdTe, CdSe, and CdS Nanocrystals.</a> Chem. Mater. 15 (14), 2854-2860 (2003).</li><li>Miao, M. S., Seshadri, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rh2O3+versus+IrO2:+relativistic+effects+and+the+stability+of+Ir4.">Rh2O3 versus IrO2: relativistic effects and the stability of Ir4.</a> J. Phys. Condens. Matter. 24 (21), 215503 (2012).</li><li>Amirav, L., Alivisatos, A. 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作者什么都没有透露。

硒化镉种子和硒化镉硫化镉@播种棒的合成已得到很好的研究21,24,25。轻微的修改的量，温度和时间对这些基材颗粒的合成的步骤可用于调整其长度，直径和/或形态。本文所描述的合成方案产生均匀尺寸的高度发光种子棒。 该配体交换过程允许使用在极性环境中接种棒，在这种情况下的水。在配体交换，当正在收集溶解丸粒（由甲苯沉淀后）的最终阶段的沉淀往往较?...

光催化提出了可再生能源发电和其他环境的应用，如水处理和空气净化1-3的吸引力和有前景的解决方案。总体水分解，利用太阳能驱动，可能是清洁和可再生氢燃料的来源;然而，尽管数十年的研究，这是足够稳定和有效的，对实际使用的系统尚未实现。 既光化学淀积和半导体介导的光催化依靠分离光生电子 - 空穴对，并将它们驱动到表面在那里他们可以引发氧化还原反应的相同的机制。这两个过程之间的相似性使得光化学淀积为光催化4-6领域一个有吸引力的合成工具。这种方法有望采取光触媒生产新的未知领域。这也许可能提供纯净的控制空间布局在异质结构的不同组件，以及前进到构造复杂的纳米颗粒系统的能力。最终，该方法将使我们更接近了一步实现直接太阳能到燃料能量转换的高效光催化剂。 我们研究的IrO 2的生长作为助催化剂，因为它是已知可用于水氧化7-11的高效催化剂。嵌入在杆（硫化镉）12,13量子点（硒化镉）的可调结构作为我们的光触媒基板14,15。它是目前待定是否经由介导的途径发生氧化途径，或通过直接孔攻击。在这里，我们对半导体异质结构的光生空穴了解和控制，可以用来达到氧化反应的机理研究。这是通过在衬底结构，这有利于密闭小孔16,17和地层的本地化成为可能在杆不同的氧化反应部位。纳米材料的局限性电荷载体的使用可以利用用于由产品的简单检查的氧化还原反应的机理研究。以这种方式光化学淀积可以用作两个还原和氧化反应途径的独特探针。这是通过光化学淀积和尖端胶体合成18-20的结合所带来的新的和令人兴奋的可能性的一个例子。 制定水分解和可再生能源转化的高效催化剂的追求已成为材料界的重要推力。这促使在硫化镉世界范围的兴趣，这是已知的生产氢的高活性，尽管它是由光化学不稳定的阻碍。我们这里的工作把材料的阿喀琉斯之踵。 2的IrO装饰的CdSe @硫化镉棒展示纯延长光照下显着的光化学稳定性水。

<table border="0" cellpadding="0" cellspacing="0" width="822">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:304px;">Sulfur (S)</td>
			<td style="width:79px;">Sigma</td>
			<td style="width:119px;">84683</td>
			<td style="width:321px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Selenium (Se)</td>
			<td>Sigma</td>
			<td>229865</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Cadmium Oxide (CdO)</td>
			<td>Sigma</td>
			<td>202894</td>
			<td>Highly Toxic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">n-Octadecylphosphonic acid (ODPA)</td>
			<td>Sigma</td>
			<td>715166</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Propylphosphonic acid (PPA)</td>
			<td>Sigma</td>
			<td>305685</td>
			<td>Highly regulated in some countries and regions</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Butylphosphonic acid (BPA)</td>
			<td>Sigma</td>
			<td>737933</td>
			<td>Alternative to PPA</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Hexylphosphonic acid (HPA)</td>
			<td>Sigma</td>
			<td>750034</td>
			<td>Alternative to PPA</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Trioctylphosphonic oxide (TOPO)</td>
			<td>Sigma</td>
			<td>346187</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Tri-n-octylphosphine, 97% (TOP)</td>
			<td>Sigma</td>
			<td>718165</td>
			<td>Air sensitive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Spectrochemical Stirbar</td>
			<td>Sigma</td>
			<td><a href="http://www.sigmaaldrich.com/catalog/product/sigma/z363545?lang=en&amp;region=US">Z363545</a></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium Hydroxide</td>
			<td>Sigma</td>
			<td>S5881</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Methanol</td>
			<td>Sigma</td>
			<td>322415</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Toluene</td>
			<td>Sigma</td>
			<td>244511</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Hexane</td>
			<td>Sigma</td>
			<td>296090</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Octylamine</td>
			<td>Sigma</td>
			<td>74988</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Nonanoic Acid</td>
			<td>Sigma</td>
			<td>N5502</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Isopropanol</td>
			<td>Sigma</td>
			<td>278475</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Mercaptoundecanoic Acid (MUA)</td>
			<td>Sigma</td>
			<td>674427</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Tetramethylammonium Hydroxide (TMAH)</td>
			<td>Sigma</td>
			<td>T7505</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Apiezon H Grease (high temperature grease)</td>
			<td>Sigma</td>
			<td>Z273562</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium Persulfate</td>
			<td>Sigma</td>
			<td>216232</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium Nitrate</td>
			<td>Sigma</td>
			<td>229938</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium Hexachloroiridate(III) hydrate</td>
			<td>Sigma</td>
			<td>288160</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Mounted 455nm LED</td>
			<td>Thorlabs</td>
			<td>M455L3</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Cuvette Holder</td>
			<td>Thorlabs</td>
			<td>CVH100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">25mL 3-neck Round Bottom Flask</td>
			<td>Chemglass</td>
			<td>CG-1524-A-02</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Liebig Condensor</td>
			<td>Chemglass</td>
			<td>CG-1218-A-20</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">T-Joint Adapter</td>
			<td>Chemglass</td>
			<td>AF-0509-10</td>
			<td></td>
		</tr>
	</tbody>
</table>

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).

透射电子显微照片（TEM），以看到氧化铱的上引晶棒（图1）的分布收集。 TEM样品通过吹打溶解颗粒的下降到TEM网格制备。 X射线衍射（XRD， 图2）和 X射线光电子能谱（XPS，图3）被用来表征观察的生长结晶的IrO 2的混合和铱2 O 3等。 X射线衍射和XPS的样品的制备是通过在载玻片上的粒子的干燥完成。用足够的采?...

Watch this Scientific Journal Video about Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods at JoVE.com

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

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 ...

photochemical-oxidative-growth-iridium-oxide-nanoparticles-on-cdsecds

Universidad San Sebastian

Research

JoVE Journal

Chemistry

9.5K 次观看.  Technion – Israel Institute of Technology. A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

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

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

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

原子定义模板复合氧化物薄膜的外延生长

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Hydroquinone Based Synthesis of Gold Nanorods

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the synthetic methods for the preparation of gold nanorods are still not fully optimized. In this paper we describe a new, highly efficient, two-step protocol based on the use of hydroquinone as a mild reducing agent. Our approach allows the preparation of nanorods with a good control of size and aspect ratio (AR) simply by varying the amount of hexadecyl trimethylammonium bromide (CTAB) and silver ions (Ag+) present in the "growth solution". By using this method, it is possible to markedly reduce the amount of CTAB, an expensive and cytotoxic reagent, necessary to obtain the elongated shape. Gold nanorods with an aspect ratio of about 3 can be obtained in the presence of just 50 mM of CTAB (versus 100 mM used in the standard protocol based on the use of ascorbic acid), while shorter gold nanorods are obtained using a concentration as low as 10 mM.

This paper describes a protocol for the synthesis of gold nanorods, based on the use of hydroquinone as reducing agent, plus the different mechanisms for controlling their size and aspect ratio.

金纳米棒基于对苯二酚合成

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the ...

In Situ Detection and Single Cell Quantification of Metal Oxide Nanoparticles Using Nuclear Microprobe Analysis

Micro-analytical techniques based on chemical element imaging enable the localization and quantification of chemical composition at the cellular level. They offer new possibilities for the characterization of living systems and are particularly appropriate for detecting, localizing and quantifying the presence of metal oxide nanoparticles both in biological specimens and the environment. Indeed, these techniques all meet relevant requirements in terms of (i) sensitivity (from 1 up to 10 &#181;g.g-1 of dry mass), (ii) micrometer range spatial resolution, and (iii) multi-element detection. Given these characteristics, microbeam chemical element imaging can powerfully complement routine imaging techniques such as optical and fluorescence microscopy. This protocol describes how to perform a nuclear microprobe analysis on cultured cells (U2OS) exposed to titanium dioxide nanoparticles. Cells must grow on and be exposed directly in a specially designed sample holder used on the optical microscope and in the nuclear microprobe analysis stages. Plunge-freeze cryogenic fixation of the samples preserves both the cellular organization and the chemical element distribution. Simultaneous nuclear microprobe analysis (scanning transmission ion microscopy, Rutherford backscattering spectrometry and particle induced X-ray emission) performed on the sample provides information about the cellular density, the local distribution of the chemical elements, as well as the cellular content of nanoparticles. There is a growing need for such analytical tools within biology, especially in the emerging context of Nanotoxicology and Nanomedicine for which our comprehension of the interactions between nanoparticles and biological samples must be deepened. In particular, as nuclear microprobe analysis does not require nanoparticles to be labelled, nanoparticle abundances are quantifiable down to the individual cell level in a cell population, independently of their surface state.

In Situ Detection and Single Cell Quantification of Metal Oxide Nanoparticles Using Nuclear Microprobe Analysis

We describe a procedure for the detection of chemical elements present in situ in human cells as well as their in vitro quantification. The method is well-suited to any cell type and is particularly useful for quantitative chemical analyses in single cells following in vitro metal oxide nanoparticles exposure.

原位金属氧化物纳米粒子的核探针检测与单细胞定量研究

Micro-analytical techniques based on chemical element imaging enable the localization and quantification of chemical composition at the cellular level. ...

Ligand-Mediated Nucleation and Growth of Palladium Metal Nanoparticles

The size, size distribution and stability of colloidal nanoparticles are greatly affected by the presence of capping ligands. Despite the key contribution of capping ligands during the synthesis reaction, their role in regulating the nucleation and growth rates of colloidal nanoparticles is not well understood. In this work, we demonstrate a mechanistic investigation of the role of trioctylphosphine (TOP) in Pd nanoparticles in different solvents (toluene and pyridine) using in situ SAXS and ligand-based kinetic modeling. Our results under different synthetic conditions reveal the overlap of nucleation and growth of Pd nanoparticles during the reaction, which contradicts the LaMer-type nucleation and growth model. The model accounts for the kinetics of Pd-TOP binding for both, the precursor and the particle surface, which is essential to capture the size evolution as well as the concentration of particles in situ. In addition, we illustrate the predictive power of our ligand-based model through designing the synthetic conditions to obtain nanoparticles with desired sizes. The proposed methodology can be applied to other synthesis systems and therefore serves as an effective strategy for predictive synthesis of colloidal nanoparticles.

The main goal of this work is to elucidate the role of capping agents in regulating the size of palladium nanoparticles by combining in situ small angle x-ray scattering (SAXS) and ligand-based kinetic modeling.

配体介导成核与钯金属纳米粒子的生长

The size, size distribution and stability of colloidal nanoparticles are greatly affected by the presence of capping ligands. Despite the key contribution ...

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven effective in gas adsorption, separations, and catalysis. MOFs are most commonly synthesized as bulk powder, requiring additional processes to adhere them to functional devices and fabrics that risk decreasing the powder porosity and adsorption capacity. Here, we demonstrate a method of first coating fabrics with metal oxide films using atomic layer deposition (ALD). This process creates conformal films of controllable thickness on each fiber, while providing a more reactive surface for MOF nucleation. By submerging the ALD coated fabric in solution during solvothermal MOF synthesis, the MOFs create a conformal, well-adhered coating on the fibers, resulting in a MOF-functionalized fabric, without additional adhesion materials that may block MOF pores and functional sites. Here we demonstrate two solvothermal synthesis methods. First, we form a MIL-96(Al) layer on polypropylene fibers using synthetic conditions that convert the metal oxide to MOF. Using initial inorganic films of varying thicknesses, diffusion of the organic linker into the inorganic allows us to control the extent of MOF loading on the fabric. Second, we perform a solvothermal synthesis of UiO-66-NH2 in which the MOF nucleates on the conformal metal oxide coating on polyamide-6 (PA-6) fibers, thereby producing a uniform and conformal thin film of MOF on the fabric. The resulting materials can be directly incorporated into filter devices or protective clothing and eliminate the maladroit qualities of loose powder.

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks are effective in gas storage and heterogeneous catalysis, but typical synthesis methods result in loose powders that are difficult to incorporate into smart materials. We demonstrate a method of first coating fabrics with ALD metal oxides, resulting in conformal films of MOF on the fabrics during solvothermal synthesis.

溶剂热合成 MIL-96 和 UiO-66-NH2在纤维垫上原子层沉积金属氧化物涂层上的合成

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven ...

Chemoselective Preparation of 1-Iodoalkynes, 1,2-Diiodoalkenes, and 1,1,2-Triiodoalkenes Based on the Oxidative Iodination of Terminal Alkynes

We present the chemoselective synthesis of 1-(iodoethynyl)-4-methylbenzene, 1-(1,2-diiodovinyl)-4-methylbenzene, and 1-methyl-4-(1,2,2-triiodovinyl)benzene as representative examples for the practical chemoselective preparation of 1-iodoalkynes, 1,2-diiodoalkenes, and 1,1,2-triiodoalkenes from the chemoselective iodination of terminal alkynes mediated by hypervalent-iodine reagents. The chemoselectivity was confirmed by using p-tolylethyne as a model substrate to screen a variety of iodine sources and/or the hypervalent-iodine reagents. A combination of tetrabutylammonium iodide (TBAI) and (diacetoxyiodo)benzene (PIDA) selectively generates 1-iodoalkynes, while a combination of KI and PIDA generates 1,2-diiodoalkenes. A one-pot synthesis based on both TBAI-PIDA and KI-PIDA yields the corresponding 1,1,2-triiodoalkenes. These protocols were subsequently applied to the synthesis of synthetically important aromatic and aliphatic 1-iodoalkynes, 1,2-diiodoalkenes, and 1,1,2-triiodoalkenes, which were obtained in good yield with excellent chemoselectivity.

Herein, detailed protocols for the oxidative iodination of terminal alkynes using hypervalent-iodine reagents are presented, which chemoselectively afford 1-iodoalkynes, 1,2-diiodoalkenes, and 1,1,2-triiodoalkenes.

基于末端碘氧化炔烃的 1-Iodoalkynes、12-Diiodoalkenes、11、2 Triiodoalkenes 的 Chemoselective 制备

We present the chemoselective synthesis of 1-(iodoethynyl)-4-methylbenzene, 1-(1,2-diiodovinyl)-4-methylbenzene, and ...

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. ...

Growth of Gold Dendritic Nanoforests on Titanium Nitride-coated Silicon Substrates

In this study, a high-power impulse magnetron sputtering system is used to coat a flat and firm titanium nitride (TiN) film on silicon (Si) wafers, and a fluoride-assisted galvanic replacement reaction (FAGRR) is employed for the rapid and easy deposition of gold dendritic nanoforests (Au DNFs) on the TiN/Si substrates. Scanning electron microscopy (SEM) images and energy-dispersive X-ray spectroscopy patterns of TiN/Si and Au DNFs/TiN/Si samples validate that the synthesis process is accurately controlled. Under the reaction conditions in this study, the thickness of the Au DNFs increases linearly to 5.10 &#177; 0.20 &#181;m within 15 min of the reaction. Therefore, the employed synthesis procedure is a simple and rapid approach for preparing Au DNFs/TiN/Si composites.

This study presents a feasible procedure for synthesizing gold dendritic nanoforests on titanium nitride/silicon substrates. The thickness of gold dendritic nanoforests increases linearly within 15 min of a synthesis reaction.

氮化钛涂层硅基板上金石榴石的生长

In this study, a high-power impulse magnetron sputtering system is used to coat a flat and firm titanium nitride (TiN) film on silicon (Si) wafers, and a ...

Design, Synthesis, and Photochemical Properties of Clickable Caged Compounds

Caged compounds enable the photo-mediated manipulation of the cell physiology with high spatiotemporal resolution. However, the limited structural diversity of currently available caging groups and the difficulties in synthetic modification without sacrificing their photolysis efficiencies are obstacles to expanding the repertoire of caged compounds for live cell applications. As the chemical modification of coumarin-type photo-caging groups is a promising approach for the preparation of caged compounds with diverse physical and chemical properties, we report a method for the synthesis of clickable caged compounds that can be modified easily with various functional units via the copper(I)-catalyzed Huisgen cyclization. The modular platform molecule contains a (6-bromo-7-hydroxycoumarin-4-yl)methyl (Bhc) group as a photo-caging group, which exhibits a high photolysis efficiency compared to those of the conventional 2-nitrobenzyls. General procedures for the preparation of clickable caged compounds containing amines, alcohols, and carboxylates are presented. Additional properties such as the water solubility and cell targeting ability can be readily incorporated into clickable caged compounds. Furthermore, the physical and photochemical properties, including the photolysis quantum yield, were measured and were found to be superior to those of the corresponding Bhc caged compounds. The described protocol could therefore be considered a potential solution for the lack of structural diversity in the available caged compounds.

A protocol for the synthesis and measurement of the photochemical properties of modular caged compounds with clickable moieties is presented.