我们感谢中国国家自然科学基金 (21703104)、江苏省科技计划 (SBK2017041514) 南京理工大学 (39837131) 的财政支持, 以及江苏国家协同 SICAM 奖学金。先进材料创新中心。

注意: 请检查化学品的材料安全数据表 (MSDS), 以详细处理和储存指示。请小心处理纳米材料, 因为可能有不明风险。请在通风罩内进行实验, 并佩戴适当的个人防护设备。
1. 种子纳米粒子的合成
注: 为避免在纳米粒子合成过程中过早成核造成的失败, 请用清水冲洗玻璃器皿和搅拌棒 , 并用水彻底冲洗。
<ol><li>3-5 纳米金纳米粒子的合成<ol>
<li>制备氢氯金酸 (III.) (HAuCl4) 溶液, 溶解10毫克 HAuCl4∙3H2O 在1毫升去离子水 (DI 水) 在4毫升瓶。吸管0.197 毫升的 HAuCl4溶液成50毫升的圆底烧瓶。</li>
		<li>将19.7 毫升的 DI 水添加到烧瓶中稀释 HAuCl4溶液。</li>
		<li>将10毫克柠檬酸钠溶于1毫升的 DI 水中, 再用4毫升的小瓶, 准备1% 柠檬酸钠溶液。添加0.147 毫升的1% 柠檬酸钠溶液的稀释 HAuCl4溶液中制备的步骤1.1.2。</li>
		<li>通过将2.3 毫克的 NaBH4溶解于0.1 米的硼氢化钠 (NaBH4) 溶液, 在0.6 毫升的 DI 水中溶化。</li>
		<li>快速注入0.6 毫升0.1 米 NaBH4溶液的混合物从步骤1.1.3 在剧烈搅拌。检查解决方案的直接颜色变化从淡黄色到明亮的橙色。</li>
		<li>将混合物搅拌10分钟, 等待溶液的渐变颜色变红橙。</li>
		<li>用紫外-可见光谱和扫描电镜 (SEM) 确定获得的 Au 纳米粒子的尺寸。</li>
	</ol>
</li>
	<li>15和40纳米 Au 纳米粒子的合成<ol>
<li>在250毫升的圆底烧瓶中加入100毫升的 DI 水。重10毫克的 HAuCl4∙3H2O 固体和溶解它在圆底烧瓶。</li>
		<li>在烧瓶中加入一个磁力搅拌棒, 并用冷凝器装备烧瓶。在油浴中搅拌并加热1.2.1 到100摄氏度的溶液。回流溶液10分钟。</li>
		<li>重40毫克柠檬酸钠, 并将其溶解在4毫升的 DI 水中, 以制备1% 柠檬酸钠溶液。</li>
		<li>合成15纳米 Au 纳米粒子, 加入3毫升的1% 柠檬酸钠溶液从步骤1.2.3 到煮沸的混合物与注射器。 注意: 溶液的颜色在1分钟内变成灰色, 然后逐渐变红。<ol>
<li>为了合成40纳米 Au 纳米粒子, 将1% 柠檬酸钠溶液中的1.5 毫升注入1.2.2 与注射器的沸点溶液中。保持溶液沸腾, 直到它在10分钟内变红。 注意: 溶液的颜色从透明变为深灰色, 然后变成黑色, 最后以紫色在1分钟左右。</li>
		</ol>
</li>
		<li>继续回流反应溶液30分钟, 冷却在室温下溶液的环境条件。</li>
		<li>用紫外-可见光谱和 SEM 表征了所得到的 Au 纳米粒子的大小和均匀性。</li>
	</ol>
</li>
</ol>2. 在硅 (硅) 晶片和各种基体上合成金纳米线 (长度 = ~ 500 nm)
<ol><li>制备种子吸附基材。<ol>
<li>将硅晶片切割成5毫米´5毫米片。在超声波浴中依次用 DI 水和乙醇清洁硅晶片, 每块15分钟。</li>
		<li>用 29.6 W 的 O2等离子 (操作在 220 V) 的硅晶片治疗20分钟。 注意: 晶片表面变得亲水性。</li>
		<li>5毫米 3-aminopropyltriethoxysilane (APTES) 溶液, 溶解11.1 毫克的 APTES, 以混合物的 DI 水 (5 毫升) 和乙醇 (5 毫升) 在20毫升瓶。</li>
		<li>在 APTES 溶液中浸泡一片硅晶片, 2.1.3 在20毫升的小瓶中制备30分钟。</li>
		<li>取出硅晶片, 用乙醇和底水彻底清洗。</li>
	</ol>
</li>
	<li>将种子纳米粒子吸附到基体上。<ol>
<li>在步骤1.1 中制备的3-5 纳米 Au 种子溶液中浸泡硅晶片2小时。<ol>
<li>从15纳米 au 种子中生长金纳米线, 在15纳米金纳米粒子溶液中浸泡硅晶片 2 h。</li>
			<li>从40纳米 au 种子中生长金纳米线, 在40纳米金纳米粒子溶液中浸泡硅晶片 2 h。</li>
		</ol>
</li>
		<li>取出硅晶片, 用50毫升的 DI 水冲洗, 除去未吸收金纳米粒子。</li>
	</ol>
</li>
	<li>生长基板绑定的 Au 纳米线。<ol>
<li>通过在4毫升乙醇中溶解2.5 毫克 10-mba, 准备1.65 毫米4巯基苯甲酸酸 (4-mba) 溶液。</li>
		<li>5.10 毫米 HAuCl4溶液溶解20.1 毫克的 HAuCl4∙3H2O 在混合物的5毫升乙醇和5毫升的 DI 水。</li>
		<li>在10毫升的 DI 水中溶解21.7 毫克 l-抗坏血酸, 制备12.3 毫米的 l-抗坏血酸溶液。</li>
		<li>混合0.5 毫升的5.10 毫米 HAuCl4溶液与0.5 毫升 1.65 mM 4-MBA 解决方案在10毫升瓶。</li>
		<li>在步进2.3.4 中制备的混合溶液中, 从步进2.2.2 中浸泡种子吸附硅晶片。</li>
		<li>将0.5 毫升的12.3 毫米 l-抗坏血酸溶液加入到晶片浸泡的混合溶液中。轻轻摇动瓶子, 均匀地混合溶液。</li>
		<li>离开晶片和解决方案不受干扰的15分钟. 检查在生长过程中气泡的形成, 以及硅晶片表面的颜色变化, 从闪亮的灰色到红褐色。</li>
		<li>取出硅晶片, 用乙醇和 DI 水冲洗。在环境条件下干燥硅晶片, 等待晶片表面转向黄金。</li>
		<li>用 SEM 表征了金纳米线的形貌。</li>
	</ol>
</li>
	<li>对于在玻璃滑轨上的 Au 纳米线的生长, Al2O3, SrTiO3, LaAlO3, 铟锡氧化物 (ITO) 和 F 掺杂的锡氧化物基板, 遵循相同的程序, 包括清洗过程。</li>
</ol>3. 不同配体的金纳米线的合成
<ol><li>用各种 thiolated 配体合成金纳米线林: 2-naphthalenethiol (2-NpSH), 4-mercaptophenylacetic 酸 (4-MPAA) 和 3-巯基苯甲酸酸 (3-MBA)。<ol>
<li>按照步骤 2.1-2.2 中的相同步骤处理硅晶片。</li>
		<li>在10毫升乙醇中溶解2.6 毫克的 2-NpSH, 制备1.65 毫米 2 NpSH 溶液。<ol>
<li>在10毫升乙醇中溶解2.8 毫克的 4-MPAA, 制备1.65 毫米 4 MPAA 溶液。</li>
			<li>通过在10毫升乙醇中溶解2.5 毫克 3-mba 课程, 准备 1.65 mM 3-mba 解决方案。</li>
		</ol>
</li>
		<li>5.10 毫米 HAuCl4溶液和12.3 毫米 l-抗坏血酸溶液在步骤 2.3. 1-2. 3.3 中遵循相同的步骤。</li>
		<li>在一个10毫升的小瓶, 混合0.5 毫升的 HAuCl4溶液与0.5 毫升的 2-NpSH 溶液, 并动摇混合物得到一个均匀的解决方案。<ol>
<li>在一个10毫升的小瓶, 混合0.5 毫升的 HAuCl4溶液与0.5 毫升的 4-MPAA 溶液, 并动摇混合物得到一个均匀的解决方案。</li>
			<li>在一个10毫升的小瓶, 混合0.5 毫升的 HAuCl4溶液与0.5 毫升 3-MBA 解决方案, 并动摇的混合物得到一个均匀的解决方案。</li>
		</ol>
</li>
		<li>添加0.5 毫升的12.3 毫米 l-抗坏血酸溶液的晶圆浸泡混合溶液。轻轻摇动瓶子, 得到一个均匀混合的溶液。</li>
		<li>离开晶片和解决方案不受干扰的15分钟. 观察硅晶片表面慢慢从闪亮的灰色变红棕色。</li>
		<li>取出硅晶片, 用乙醇和 DI 水冲洗, 在环境条件下干燥硅晶片, 直到晶片表面变成金色。</li>
		<li>用 SEM 对金纳米线森林结构进行了验证。</li>
	</ol>
</li>
	<li>混合配体的锥形金纳米线的合成。<ol>
<li>4-mba 与 3-mercaptopropanoic 酸 (3 兆帕) 混合配体增稠金纳米线的合成 (c4-mba/c3-mpa = 3:1)。<ol>
<li>在步骤 2.1-2.2 中, 除稀释种子溶液100次外, 对硅晶片进行相同的工序处理。</li>
			<li>通过在10毫升乙醇中溶解4.6 毫克 4-mba 课程, 准备 3 mM 4-mba 解决方案。</li>
			<li>在10毫升乙醇中溶解3.2 毫克3兆帕, 准备3毫米3兆帕斯卡溶液。</li>
			<li>混合0.75 毫升 3 mM 4-MBA 解决方案与0.25 毫升3毫米 3-MPA 解决方案 (在10毫升瓶。轻轻摇动, 得到一个均匀的溶液。</li>
			<li>5.10 毫米 HAuCl4溶液和12.3 毫米 l-抗坏血酸溶液在步骤 2.3. 2-2. 3.3 中遵循相同的步骤。</li>
			<li>在步骤3.2.1.4 中加入0.5 毫升的5.10 毫米 HAuCl4溶液, 并轻轻摇动以融汇溶液。</li>
			<li>在10毫升的小瓶中, 在混合溶液中浸泡3.2.1.1 的硅晶片。添加0.5 毫升的12.3 毫米 l-抗坏血酸溶液的混合溶液。</li>
			<li>10分钟后, 将硅晶片取出, 用乙醇和 DI 水冲洗。</li>
			<li>在环境条件下干燥晶片, 用 SEM 确认结构。</li>
		</ol>
</li>
		<li>合成 4-mba 和3兆帕混合配体的锥形金纳米线 (c4-mba/c3-mpa = 6:4)。在步骤3.2.1 中遵循相同的步骤, 0.6 毫升 3 mM 4-MBA 解决方案和0.4 毫升3毫米3兆帕解决方案。</li>
		<li>合成 4-mba 和3兆帕混合配体的锥形金纳米线 (c4-mba/c3-mpa = 1:1)。在步骤3.2.1 中遵循相同的步骤, 0.5 毫升 3 mM 4-MBA 解决方案和0.5 毫升3毫米3兆帕解决方案。</li>
	</ol>
</li>
</ol>4. 基于金纳米线的复合纳米结构的合成
<ol><li>厚薄厚薄段金纳米线的合成。<ol>
<li>按照步骤 2.1-2.2 中的相同步骤处理硅晶片。</li>
		<li>通过在10毫升乙醇中溶解2.5 毫克 4-mba 课程, 准备 1.65 mM 4-mba 解决方案。</li>
		<li>通过稀释 1.65 mm 4 mba 解决方案20次, 准备 0.0830 mm 4-mba 解决方案。</li>
		<li>按照步骤 2.3. 2-2. 3.3 中的相同步骤, 准备 HAuCl4和 l-抗坏血酸溶液。</li>
		<li>通过混合0.5 毫升 1.65 mm 4-MBA 解决方案, 0.5 毫升5.10 毫米 HAuCl4溶液和0.5 毫升 l-抗坏血酸溶液 (最终浓度: c12.3-mba = 4 毫米, cHAuCl4 = 0.550 毫米, 准备1.5 毫升的生长溶液 A, cl-抗坏血酸= 4.10 毫米)。</li>
		<li>通过混合0.5 毫升 0.0830 mM 4-MBA 解决方案, 准备1.5 毫升的生长溶液 B, 0.5 毫升5.10 毫米 HAuCl4溶液, 0.5 毫升12.3 毫米 l-抗坏血酸溶液 (最后浓度: c4-MBA = 0.0280 毫米, cHAuCl4 = 1.70 毫米, cL-抗坏血酸酸= 4.10 毫米)。</li>
		<li>将硅晶片浸入含有生长液 B 的10毫升瓶中, 约1分钟。</li>
		<li>迅速转移硅晶片不干燥到另一个10毫升的小瓶含有生长液 A, 并使其生长2分钟。</li>
		<li>重复步骤 4.1, 7-4, 1.8 再一次。</li>
		<li>将硅晶片取出, 用50毫升乙醇和50毫升的 DI 水冲洗。</li>
		<li>通过 SEM 验证了所得到的分段金纳米线的结构。</li>
	</ol>
</li>
	<li>nanoflowers 的合成<ol>
<li>在步骤 2.1-2.2 中, 除5分钟2等离子处理外, 对硅晶片进行相同的操作。</li>
		<li>将硅晶片浸泡在含有10000x 稀释3-5 纳米 Au 种子溶液的10毫升瓶中, 15 分钟。</li>
		<li>用4.2.2 彻底清洗硅晶片, 去除未吸收金纳米粒子。</li>
		<li>按照步骤4.1.5 中的相同步骤, 准备一个包含 0.550 mM 4-MBA, 1.70 毫米 HAuCl4, 4.10 毫米 l-抗坏血酸的生长溶液。</li>
		<li>将晶片浸泡在含有三十年代生长液的10毫升瓶中。</li>
		<li>从生长液中取出晶片, 在晶片上留下一层薄薄的溶液 (13-15 ul)。</li>
		<li>在室温下快速吹干晶片。</li>
		<li>通过 SEM 对 nanoflower 结构进行了验证。</li>
	</ol>
</li>
</ol>

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J., 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=Vapor-liquid-solid+Growth+of+Silicon+Nanowires+Using+Organosilane+as+Precursor.">Vapor-liquid-solid Growth of Silicon Nanowires Using Organosilane as Precursor.</a> Chemical Communications. 46, 6105-6107 (2010).</li><li>Xia, Y. N., 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=Ultrathin+Gold+Nanowires+Can+Be+Obtained+by+Reducing+Polymeric+Strands+of+Oleylamine&#8722;AuCl+Complexes+Formed+via+Aurophilic+Interaction.">Ultrathin Gold Nanowires Can Be Obtained by Reducing Polymeric Strands of Oleylamine&#8722;AuCl Complexes Formed via Aurophilic Interaction.</a> Journal of the American Chemical Society. 130, 8900-8901 (2008).</li><li>Miguel, J. Y., 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=Helical+Growth+of+Ultrathin+Gold-Copper+Nanowires.">Helical Growth of Ultrathin Gold-Copper Nanowires.</a> Nano Letters. 16, 1568-1573 (2016).</li><li>Sun, S. H., 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=Ultrathin+Au+Nanowires+and+Their+Transport+Properties.">Ultrathin Au Nanowires and Their Transport Properties.</a> Journal of the American Chemical Society. 130, 8902-8903 (2008).</li><li>Sun, S. H., 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=Growth+of+Au+Nanowires+at+the+Interface+of+Air/Water.">Growth of Au Nanowires at the Interface of Air/Water.</a> Journal of Physical Chemistry. C. 113, 15196-15200 (2009).</li><li>Wu, H. 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作者没有什么可透露的。

本文在前人工作19中全面讨论了这种活性表面生长治理纳米线合成的机理。此外, 还研究了种子大小和类型的影响以及配体类型和大小对20、21的影响。一般。纳米线的增长与以前报告的路线非常不同。不需要模板, 不对称生长是由配体上限的 au 表面与基体表面的金面之间的差异引起的。活性面在整个生长过程中保持活跃, 因为新沉积的?...

纳米线具有典型的一维纳米材料, 具有与体积相关的特性和由纳米结构的量子效应产生的独特性质。作为纳米尺度与块状材料之间的桥梁, 它们已广泛应用于各种催化、传感、纳米电子器件等领域。1,2,3。
然而, 纳米线的合成一直是一个巨大的挑战, 因为它通常需要打破晶体内在的对称性。传统上, 使用模板来调节材料的沉积。例如, 模板电沉积已被用于形成各种类型的纳米线, 如银纳米线和 CdS 纳米线4,5,6,7,8,9 ,10。另一种常见的方法是蒸气-液-固 (VLS) 的生长, 它采用熔融催化剂在高温下诱导基体上各向异性的生长11。合成金属纳米线的常用策略是银纳米线和油胺辅助超薄金纳米线12、13、14、15的多元醇方法。这两种方法都是材料特有的, 而纳米线参数在合成过程中不容易调整。此外, 金属纳米线也可以由压力驱动的方法, 其中组装金属纳米粒子被机械压缩和熔化成纳米线16,17,18。
最近, 我们报告了一个独特的方法合成金纳米线19。在 thiolated 小分子配体的协助下, 纳米线可以在环境条件下生长并形成垂直排列的硅晶片基底上的阵列。结果表明, 配体在对称断裂生长中起着重要作用。它强烈地与基体吸附的金种子的表面结合, 迫使 au 选择性地在种子和基质之间的配体缺陷界面上沉积。新沉积的金与基底之间的界面保持配体缺陷, 因此, 在整个生长过程中存在活性表面。通过对配体浓度、种子类型、浓度以及其它几个参数的调节, 可以合成一系列的金纳米线纳米结构。
在这项工作中, 我们将提供一个详细的协议, 为这种方便的 Au 纳米线合成。给出了合成方法, 包括用疏水性表面性质的金纳米线、其它基体上的 au 纳米线、混合两个配体的锥形金纳米线和通过调整生长而形成的纳米金纳米结构。条件。

<table border="0" cellpadding="0" cellspacing="0" width="846">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:256px;">Trisodium citrate dihydrate</td>
			<td style="width:209px;">Alfa Aesar</td>
			<td style="width:179px;">LoT: 5008F14U</td>
			<td style="width:203px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sodium borohydride</td>
			<td style="width:209px;">Fluka</td>
			<td style="width:179px;">LoT: STBG0330V</td>
			<td>NaBH4</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Hydrogen tetrachloroaurate(III) trihydrate</td>
			<td style="width:209px;">Alfa Aesar</td>
			<td style="width:179px;">LoT: T19C006</td>
			<td style="width:203px;">HAuCl4</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">3-aminopropyltriethoxysilane</td>
			<td style="width:209px;">J&#38;K Scientific</td>
			<td style="width:179px;">LoT: LT20Q102</td>
			<td style="width:203px;">APTES</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">L-ascorbic acid&#160;</td>
			<td>Sigma-Aldrich</td>
			<td style="width:179px;">LoT: SLBL9227V</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">4-mercaptobenzoic acid</td>
			<td>Sigma-Aldrich</td>
			<td style="width:179px;">LoT: MKBV5048V</td>
			<td style="width:203px;">4-MBA</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">2-Naphthalenethiol</td>
			<td>Sigma-Aldrich</td>
			<td style="width:179px;">LoT: BCBP4238V</td>
			<td>2-NpSH</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">4-Mercaptophenylacetic acid</td>
			<td style="width:209px;">Alfa Aesar</td>
			<td style="width:179px;">LoT: 10199160</td>
			<td>4-MPAA</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">3-mercaptobenzoic acid</td>
			<td style="width:209px;">Aladdin</td>
			<td style="width:179px;">LoT: G1213027</td>
			<td>3-MBA</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">3-Mercaptopropionic acid</td>
			<td style="width:209px;">Aladdin</td>
			<td style="width:179px;">LoT: E1618095</td>
			<td>3-MPA</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">absolute ethanol</td>
			<td style="width:209px;">Sinopharm chemical Reagent</td>
			<td style="width:179px;">20170802</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:256px;">Silicon wafer</td>
			<td style="width:209px;">Zhe Jiang lijing</td>
			<td style="width:179px;">P</td>
			<td>Si</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Scanning Electron Microscope</td>
			<td style="width:209px;">Quanta FEG 250</td>
			<td style="width:179px;"></td>
			<td>SEM</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Centrifuge&#160;</td>
			<td style="width:209px;">Eppendorf</td>
			<td style="width:179px;">5424</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Ultrasonic cleaner&#160;</td>
			<td style="width:209px;">Kun Shan hechuang</td>
			<td style="width:179px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:256px;">Ultra-pure water system</td>
			<td style="width:209px;">NanJing qianyan</td>
			<td style="width:179px;">UP6682-10-11</td>
			<td>for deionized water</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:256px;">Plasma cleaner</td>
			<td style="width:209px;">Harrick Plasma</td>
			<td style="width:179px;">PDC-002</td>
			<td>for oxygen plasma</td>
		</tr>
	</tbody>
</table>

synthesis of substrate-bound au nanowires via an active surface growth mechanism

提高合成能力对纳米和纳米技术的发展具有重要意义。纳米线的合成一直是一个挑战, 因为它需要对称晶体的不对称生长。在这里, 我们报告一个独特的合成基板绑定的 Au 纳米线。这种无模板合成采用 thiolated 配体和基材吸附法, 在环境条件下实现了 Au 在溶液中的连续不对称沉积。thiolated 配体在种子的暴露表面防止了 au 沉积, 因此在 au 种子和基体之间的界面上只发生 au 沉积。新沉积的金纳米线的一侧立即覆盖 thiolated 配体, 而底部面对基体保持无配体和活跃的下一轮 Au 沉积。进一步证明了该金纳米线的生长可以在各种基体上诱导, 不同的 thiolated 配体可以用来调节纳米丝的表面化学。纳米线的直径也可以用混合配体来控制, 而另一种 "坏" 配位则可以使侧向生长。通过对该机理的理解, 可以设计和合成金纳米线纳米结构。

用 sem 研究了金纳米粒种子、基片约束金纳米线和金纳米导线的衍生物纳米结构.图 1显示了3-5 纳米 au 纳米粒子、15纳米 au 纳米粒子和40纳米 au 的代表性 SEM 图像。纳米粒子吸附在硅晶片上, 确认其大小、吸附和分布。本文还介绍了在硅晶片基体上分别生长的金纳米线。典型的非晶金纳米线衬底表面的 SEM 图像,即玻璃基片等. <strong class="xfi...

Watch this Scientific Journal Video about Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism at JoVE.com

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

我们报告了一种基于溶液的方法合成基板束缚金纳米线。通过调整在合成过程中使用的分子配体, 可以从不同的表面性质的基体中生长出金纳米线。以金纳米线为基础的纳米结构也可以通过调整反应参数来合成。

通过活性表面生长机制合成基片束缚金纳米线

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

synthesis-substrate-bound-au-nanowires-via-an-active-surface-growth

Research

JoVE Journal

Chemistry

7.7K 次观看.  Nanjing Tech University. 我们报告了一种基于溶液的方法合成基板束缚金纳米线。通过调整在合成过程中使用的分子配体, 可以从不同的表面性质的基体中生长出金纳米线。以金纳米线为基础的纳米结构也可以通过调整反应参数来合成。

视频: Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

Synthesis of Antiviral Tetrahydrocarbazole Derivatives by Photochemical and Acid-catalyzed C-H Functionalization via Intermediate Peroxides (CHIPS)

The direct functionalization of C-H bonds is an important and long standing goal in organic chemistry. Such transformations can be very powerful in order to streamline synthesis by saving steps, time and material compared to conventional methods that require the introduction and removal of activating or directing groups. Therefore, the functionalization of C-H bonds is also attractive for green chemistry. Under oxidative conditions, two C-H bonds or one C-H and one heteroatom-H bond can be transformed to C-C and C-heteroatom bonds, respectively. Often these oxidative coupling reactions require synthetic oxidants, expensive catalysts or high temperatures. Here, we describe a two-step procedure to functionalize indole derivatives, more specifically tetrahydrocarbazoles, by C-H amination using only elemental oxygen as oxidant. The reaction uses the principle of C-H functionalization via Intermediate PeroxideS (CHIPS). In the first step, a hydroperoxide is generated oxidatively using visible light, a photosensitizer and elemental oxygen. In the second step, the N-nucleophile, an aniline, is introduced by Br&#248;nsted-acid catalyzed activation of the hydroperoxide leaving group. The products of the first and second step often precipitate and can be conveniently filtered off. The synthesis of a biologically active compound is shown.

Synthesis of Antiviral Tetrahydrocarbazole Derivatives by Photochemical and Acid-catalyzed C-H Functionalization via Intermediate Peroxides CHIPS

A two-step procedure for the synthesis of pharmaceutically active indole-derivatives by C-H functionalization with anilines is described, using photo- and Br&#248;nsted acid catalysis.

通过中级过氧化物的抗病毒四氢咔唑衍生物的合成光化学和酸催化CH官能（筹）

The direct functionalization of C-H bonds is an important and long standing goal in organic chemistry. Such transformations can be very powerful in order ...

科研

化学

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 Method to Manipulate Surface Tension of a Liquid Metal via Surface Oxidation and Reduction

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where interfacial tension is a dominant force. A variety of methods exist for controlling the interfacial tension of aqueous and organic liquids on this scale; however, these techniques have limited utility for liquid metals due to their large interfacial tension.
Liquid metals can form soft, stretchable, and shape-reconfigurable components in electronic and electromagnetic devices. Although it is possible to manipulate these fluids via mechanical methods (e.g., pumping), electrical methods are easier to miniaturize, control, and implement. However, most electrical techniques have their own constraints: electrowetting-on-dielectric requires large (kV) potentials for modest actuation, electrocapillarity can affect relatively small changes in the interfacial tension, and continuous electrowetting is limited to plugs of the liquid metal in capillaries.
Here, we present a method for actuating gallium and gallium-based liquid metal alloys via an electrochemical surface reaction. Controlling the electrochemical potential on the surface of the liquid metal in electrolyte rapidly and reversibly changes the interfacial tension by over two orders of magnitude ( &#820;500 mN/m to near zero). Furthermore, this method requires only a very modest potential (&#60; 1 V) applied relative to a counter electrode. The resulting change in tension is due primarily to the electrochemical deposition of a surface oxide layer, which acts as a surfactant; removal of the oxide increases the interfacial tension, and vice versa. This technique can be applied in a wide variety of electrolytes and is independent of the substrate on which it rests.

We present a method to control the interfacial energy of a liquid metal in an electrolyte via electrochemical deposition (or removal) of a surface oxide layer. This simple method can control the capillary behavior of gallium-based liquid metals by tuning the interfacial energy rapidly, significantly, and reversibly using modest voltages.

方法通过表面氧化还原操纵液态金属的表面张力

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the development of antibody drug conjugates (ADCs) and nanomedicine, fluorescent microscopy and systems chemistry. For many of these applications, specificity of the bioconjugation method used is of prime concern. The Michael addition of maleimides with cysteine(s) on the target proteins is highly selective and proceeds rapidly under mild conditions, making it one of the most popular methods for protein bioconjugation.
We demonstrate here the modification of the only surface-accessible cysteine residue on yeast cytochrome c with a ruthenium(II) bisterpyridine maleimide. The protein bioconjugation is verified by gel electrophoresis and purified by aqueous-based fast protein liquid chromatography in 27% yield of isolated protein material. Structural characterization with MALDI-TOF MS and UV-Vis is then used to verify that the bioconjugation is successful. The protocol shown here is easily applicable to other cysteine - maleimide coupling of proteins to other proteins, dyes, drugs or polymers.

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

This protocol details the important steps required for the bioconjugation of a cysteine containing protein to a maleimide, including reagent purification, reaction conditions, bioconjugate purification and bioconjugate characterization.

蛋白质生物缀合物的合成<em&gt;通过</em&gt;半胱氨酸马来酰亚胺化学

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and conformality by taking advantage of self-limiting reactions between vapor-phase precursors and the growing film. Perovskite oxides present potential for next-generation electronic materials, but to-date have mostly been deposited by physical methods. This work outlines a method for depositing SrTiO3 (STO) on germanium using ALD. Germanium has higher carrier mobilities than silicon and therefore offers an alternative semiconductor material with faster device operation. This method takes advantage of the instability of germanium's native oxide by using thermal deoxidation to clean and reconstruct the Ge (001) surface to the 2&#215;1 structure. 2-nm thick, amorphous STO is then deposited by ALD. The STO film is annealed under ultra-high vacuum and crystallizes on the reconstructed Ge surface. Reflection high-energy electron diffraction (RHEED) is used during this annealing step to monitor the STO crystallization. The thin, crystalline layer of STO acts as a template for subsequent growth of STO that is crystalline as-grown, as confirmed by RHEED. In situ X-ray photoelectron spectroscopy is used to verify film stoichiometry before and after the annealing step, as well as after subsequent STO growth. This procedure provides framework for additional perovskite oxides to be deposited on semiconductors via chemical methods in addition to the integration of more sophisticated heterostructures already achievable by physical methods.

This work details the procedures for the growth and characterization of crystalline SrTiO3 directly on germanium substrates by atomic layer deposition. The procedure illustrates the ability of an all-chemical growth method to integrate oxides monolithically onto semiconductors for metal-oxide semiconductor devices.

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

铂镍纳米线的合成及减氧性能优化

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

化学沉淀法合成铌2O5改性高比表面积镍催化剂

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

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

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

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

直接溶液还原法快速合成金、钯、铂气凝胶的研究

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

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) with a 4.6 nm pore size, and ordered silica porous matrix, SBA-15, with a 5.3 nm pore size. This work describes the surface properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the differently ordered porous materials with similar pore sizes. For this purpose, OMC and SBA-15 with highly ordered nanoporous structures are synthesized via impregnation of the silica matrix by applying a carbon precursor and by the sol-gel method, respectively. The porous structure of investigated systems is characterized by an N2 adsorption-desorption analysis at 77 K. To determine the electrochemical character of the surface of synthesized materials, potentiometric titration measurements are conducted; the obtained results for OMC shows a significant pHpzc shift toward the higher values of pH, relative to SBA-15. This suggests that investigated OMC has surface properties related to oxygen-based functional groups. To describe the surface properties of the materials, the contact angles of liquids penetrating the studied porous beds are also determined. The capillary rise method has confirmed the increased wettability of the silica walls relative to the carbon walls and an influence of the pore roughness on the fluid/wall interactions, which is much more pronounced for silica than for carbon mesopores. We have also studied the melting behavior of D2O confined in OMC and SBA-15 by applying the dielectric method. The results show that the depression of the melting temperature of D2O in the pores of OMC is about 15 K higher relative to the depression of the melting temperature in SBA-15 pores with a comparable 5 nm size. This is caused by the influence of adsorbate/adsorbent interactions of the studied matrices.

Here we report the synthesis and characterization of ordered nanoporous carbon (with a 4.6 nm pore size) and SBA-15 (with a 5.3 nm pore size). The work describes the surface and textural properties of nanoporous molecular sieves, their wettability, and the melting behavior of D2O confined in the materials.

合成纳米碳和二氧化硅矩阵的表面性能

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

Synthesis of Esters Via a Greener Steglich Esterification in Acetonitrile

The Steglich esterification is a widely-used reaction for the synthesis of esters from carboxylic acids and alcohols. While efficient and mild, the reaction is commonly performed using chlorinated or amide solvent systems, which are hazardous to human health and the environment. Our methodology utilizes acetonitrile as a greener and less hazardous solvent system. This protocol exhibits rates and yields that are comparable to traditional solvent systems and employs an extraction and wash sequence that eliminates the need for the purification of the ester product via column chromatography. This general method can be used to couple a variety of carboxylic acids with 1&#176; and 2&#176; aliphatic alcohols, benzylic and allylic alcohols, and phenols to obtain pure esters in high yields. The goal of the protocol detailed here is to provide a greener alternative to a common esterification reaction, which could serve useful for ester synthesis in both academic and industrial applications.

A modified Steglich esterification reaction was used to synthesize a small library of ester derivatives with primary and secondary alcohols. The methodology uses a non-halogenated and greener solvent, acetonitrile, and enables product isolation in high yields without the need for chromatographic purification.

乙腈绿色 Steglich 酯化合成酯的研究

The Steglich esterification is a widely-used reaction for the synthesis of esters from carboxylic acids and alcohols. While efficient and mild, the ...

通过活性表面生长机制合成基片束缚金纳米线

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