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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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, 因为新沉积的金表面总是新鲜的, 配体缺乏。在这里, 我们将集中讨论的实验操作, 以执行这一综合。反应发生在环境条件之下;然而, 还需要强调一些要点, 以便更好地控制合成这些纳米结构。
金纳米线的合成始于种子纳米粒子的制备。一般而言, 任何 Au 纳米结构都可以作为生长纳米线的种子使用。然而, 基体上种子的密度对于以下的 Au 沉积和纳米线的生长过程是很重要的。种子密度决定了活性部位的密度, 而非盟将存入。如果配体、HAuCl4和 l-抗坏血酸的浓度保持不变, 则单位时间内的 Au 减少量将保持不变。因此, 在每个活性部位上生长的 Au 纳米线将会更快, 如果种子密度降低, 得到的纳米丝将会更长。另一种可能的情况是, 非盟纳米线束的外观和扩展, 因为在一个活动场所太多的 Au 沉积会导致膨胀和分裂活动表面。基质中种子的密度可以通过两种方法来控制: 种子孵化时间和种子溶液的浓度, 用于孵化基质。值得一提的是, 这里描述的每种非盟纳米粒子溶液的浓度都不一样, 而差异可能是在数量级上。因此, 种子溶液的浓度有时是必要的。如 3-5 nm 和15纳米 au 纳米粒子的代表性结果所示, 从非浓缩的40纳米 au 纳米粒子中生长的 Au 纳米线要长得多, 形成束。另一方面, 在制备具有混合配体的厚纳米线时, 有针对性地减少了种子密度。这是为了避免纳米线的融合, 因为在厚纳米丝生长过程中, 横向生长与纵向伸长同时发生。致密种子吸附会导致金籽在一开始阶段与连续的 au 膜融合, 防止纳米线的进一步生长。
基材对种子表面的吸附是造成非晶种的系统不对称的重要因素。我们使用含胺的硅氧烷来获得 Au 种子的附着物。一般认为, 金籽由胺基团与纳米粒子表面的静电相互作用吸附22。在某些情况下, 种子颗粒有正电荷, 也可以使用浇铸和干法。在水/乙醇溶液水解后, APTES 通过硅 O 键与晶片和玻璃片表面相连。理论上, 任何能与 APTES 凝结的表面都能促进金纳米线的生长。在这项工作中, 我们用几个氧化物表面来证明这一点。O2等离子处理是必要的部分氧化的基质表面和植入的 OH 组, 可以凝聚与 APTES。O2等离子处理是由于其清洁和简单的操作程序而选择的;否则, 食人鱼的解决方案也可以用来创建-OH 组。基体制备的另一个关键点是-NH2的表面浓度对种子吸附也有显著的影响。虽然不能直接表征表面处理的结果, 但应尽可能精确地完成操作过程。
每步后的承印物的洗涤有时是关键的, 特别是在 APTES 处理之后。自由 APTES 分子也可以吸附在 Au 纳米粒子表面上。如果没有彻底清洗, 种子溶液在浸泡过程中会有显著的聚合。聚合种子仍可吸附在基体上, 并诱导金纳米线的生长。然而, 由于聚合会大大减少种子的浓度, 活跃的站点密度也会呈指数递减。因此, 最终的纳米线区域的顶端将是 Au 纳米粒子团聚, 而纳米线成为备用丛而不是森林。
典型的 Au 纳米线的生长发生在混合溶剂的水和乙醇 (v/v = 1:1)。由于配体 4-MBA 不溶于乙醇, 它应该首先溶解在乙醇溶液中, 然后与生长溶液的结果混合。除溶解度问题外, 溶剂比本身也在决定纳米线的生长过程中起着重要作用。活性面面积由配体吸附比和金的沉积速率决定。l-抗坏血酸的还原能力在不同的溶剂和不同的 pH 环境下变化23。改变溶剂比会立即改变金的还原率和沉积速率。增加水的比值会导致快速的金还原和可能的均匀成核, 从而防止基体束缚金纳米线的生长。
与溶剂比一样, 配体的浓度也直接影响纳米线的形成, 因为它不仅钝化了 au 表面, 而且稳定了 au, 防止了均匀成核。过量的配体会大大减慢非盟的还原。例如, 增加配体浓度5倍至2.5 毫米, 将导致基板上没有 Au 沉积物21。降低配体浓度将导致纳米线直径和有时均匀成核的增加, 后者由无色到灰或带红色的溶液变化所表示。均匀成核与非均相金纳米线在 au 原料中的生长有一定的竞争。根据均匀成核的程度, 金纳米线的生长可能是完全或部分关闭的非金饲料库存。
最后, 我们展示了一种新的方法来制备基板束缚金纳米线在不同的基底上。Au 纳米线在平坦的基板表面形成一个阵列。通过改变反应参数, 可方便地调整宽度、长度和密度。纳米线的表面化学可以通过配体进行调节, 通过混合两种不同的配位, 可以形成增厚的纳米线。另外, 结合几种不同的生长条件, 可以形成金纳米线衍生的复合 au 纳米结构。

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><tbody><tr><td>Trisodium citrate dihydrate</td><td>Alfa Aesar</td><td>LoT: 5008F14U</td><td></td></tr><tr><td>Sodium borohydride</td><td>Fluka</td><td>LoT: STBG0330V</td><td>NaBH4</td></tr><tr><td>Hydrogen tetrachloroaurate(III) trihydrate</td><td>Alfa Aesar</td><td>LoT: T19C006</td><td>HAuCl4</td></tr><tr><td>3-aminopropyltriethoxysilane</td><td>J&amp;amp;K Scientific</td><td>LoT: LT20Q102</td><td>APTES</td></tr><tr><td>L-ascorbic acid&amp;nbsp;</td><td>Sigma-Aldrich</td><td>LoT: SLBL9227V</td><td></td></tr><tr><td>4-mercaptobenzoic acid</td><td>Sigma-Aldrich</td><td>LoT: MKBV5048V</td><td>4-MBA</td></tr><tr><td>2-Naphthalenethiol</td><td>Sigma-Aldrich</td><td>LoT: BCBP4238V</td><td>2-NpSH</td></tr><tr><td>4-Mercaptophenylacetic acid</td><td>Alfa Aesar</td><td>LoT: 10199160</td><td>4-MPAA</td></tr><tr><td>3-mercaptobenzoic acid</td><td>Aladdin</td><td>LoT: G1213027</td><td>3-MBA</td></tr><tr><td>3-Mercaptopropionic acid</td><td>Aladdin</td><td>LoT: E1618095</td><td>3-MPA</td></tr><tr><td>absolute ethanol</td><td>Sinopharm chemical Reagent</td><td>20170802</td><td></td></tr><tr><td>Silicon wafer</td><td>Zhe Jiang lijing</td><td>P</td><td>Si</td></tr><tr><td>Scanning Electron Microscope</td><td>Quanta FEG 250</td><td></td><td>SEM</td></tr><tr><td>Centrifuge&amp;nbsp;</td><td>Eppendorf</td><td>5424</td><td></td></tr><tr><td>Ultrasonic cleaner&amp;nbsp;</td><td>Kun Shan hechuang</td><td></td><td></td></tr><tr><td>Ultra-pure water system</td><td>NanJing qianyan</td><td>UP6682-10-11</td><td>for deionized water</td></tr><tr><td>Plasma cleaner</td><td>Harrick Plasma</td><td>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. 如图 2所示。图 3给出了由各种配体和混合配体合成的增厚纳米线的代表性 SEM 图像。图 4给出了分段纳米线和 nanoflower 结构的代表性 SEM 图像。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/57808/57808fig1.jpg"> 图 1: 在纳米线生长前的金纳米粒种子的 SEM 图像: (a) 3-5 nm, (b) 15 nm, (c) 40 纳米 Au 纳米粒子.金纳米线从(d) 3-5 毫微米, (e) 15 毫微米和(f) 40 毫微米种子在硅片基体。<a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57808/57808fig1large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/57808/57808fig2.jpg"> 图 2: 在硅晶片以外的基板上生长的 Au 纳米线的 SEM 图像.纳米线生长于: (a)Al 2O3, (b) SrTiO3, (c) LaAlO3 (d) 玻璃滑动, (e) ITO 和 (f) 基板。<a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57808/57808fig2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 3" class="xfigimg" src="/files/ftp_upload/57808/57808fig3.jpg"> 图 3: 与其它配体合成的 SEM 图像.超薄纳米线阵列形成与 (a) MPAA, (b) 2-Naphthalenethiol, (c) 3-MBA 配体。4-MBA 和3兆帕混合配体形成的锥形金纳米线:(d)c 4-mba :c 3-MPA = 3: 1, (e) c4-MBA : c3-MPA = 6: 4 和 (f) c4-mba : c3-MPA = 1: 1。<a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57808/57808fig3large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 4" class="xfigimg" src="/files/ftp_upload/57808/57808fig4.jpg"> 图 4: 复杂的 Au NW 基纳米结构的 SEM 图像.(a) 带厚薄厚薄段的分段纳米线;(b) 通过干燥基质上的生长液 nanoflowers。<a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57808/57808fig4large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

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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

Nanyang Technological University

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

Ultrahigh Density Array of Vertically Aligned Small-molecular Organic Nanowires on Arbitrary Substrates

In recent years &pi;-conjugated organic semiconductors have emerged as the active material in a number of diverse applications including large-area, low-cost displays, photovoltaics, printable and flexible electronics and organic spin valves. Organics allow (a) low-cost, low-temperature processing and (b) molecular-level design of electronic, optical and spin transport characteristics. Such features are not readily available for mainstream inorganic semiconductors, which have enabled organics to carve a niche in the silicon-dominated electronics market. The first generation of organic-based devices has focused on thin film geometries, grown by physical vapor deposition or solution processing. However, it has been realized that organic nanostructures can be used to enhance performance of above-mentioned applications and significant effort has been invested in exploring methods for organic nanostructure fabrication.	
A particularly interesting class of organic nanostructures is the one in which vertically oriented organic nanowires, nanorods or nanotubes are organized in a well-regimented, high-density array. Such structures are highly versatile and are ideal morphological architectures for various applications such as chemical sensors, split-dipole nanoantennas, photovoltaic devices with radially heterostructured "core-shell" nanowires, and memory devices with a cross-point geometry. Such architecture is generally realized by a template-directed approach. In the past this method has been used to grow metal and inorganic semiconductor nanowire arrays. More recently &pi;-conjugated polymer nanowires have been grown within nanoporous templates. However, these approaches have had limited success in growing nanowires of technologically important &pi;-conjugated small molecular weight organics, such as tris-8-hydroxyquinoline aluminum (Alq3), rubrene and methanofullerenes, which are commonly used in diverse areas including organic displays, photovoltaics, thin film transistors and spintronics.	
Recently we have been able to address the above-mentioned issue by employing a novel "centrifugation-assisted" approach. This method therefore broadens the spectrum of organic materials that can be patterned in a vertically ordered nanowire array. Due to the technological importance of Alq3, rubrene and methanofullerenes, our method can be used to explore how the nanostructuring of these materials affects the performance of aforementioned organic devices. The purpose of this article is to describe the technical details of the above-mentioned protocol, demonstrate how this process can be extended to grow small-molecular organic nanowires on arbitrary substrates and finally, to discuss the critical steps, limitations, possible modifications, trouble-shooting and future applications.

We report a simple method for fabricating an ultrahigh density array of vertically ordered small-molecular organic nanowires. This method allows for synthesis of complex heterostructured hybrid nanowire geometries, which can be inexpensively grown on arbitrary substrates. These structures have potential applications in organic electronics, optoelectronics, chemical sensing, photovoltaics and spintronics.

超高密度垂直对齐的任意基质的小分子有机纳米线阵列

In  recent years &pi;-conjugated  organic semiconductors have emerged as the active material in a number of  diverse applications including large-area, ...

科研

工程学

Monolayer Contact Doping of Silicon Surfaces and Nanowires Using Organophosphorus Compounds

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra shallow and sharp doping profiles at the nanometer scale. In MLCD process the dopant source is a monolayer containing dopant atoms.
In this article a detailed procedure for surface doping of silicon substrate as well as silicon nanowires is demonstrated. Phosphorus dopant source was formed using tetraethyl methylenediphosphonate monolayer on a silicon substrate. This monolayer containing substrate was brought to contact with a pristine intrinsic silicon target substrate and annealed while in contact. Sheet resistance of the target substrate was measured using 4 point probe. Intrinsic silicon nanowires were synthesized by chemical vapor deposition (CVD) process using a vapor-liquid-solid (VLS) mechanism; gold nanoparticles were used as catalyst for nanowire growth. The nanowires were suspended in ethanol by mild sonication. This suspension was used to dropcast the nanowires on silicon substrate with a silicon nitride dielectric top layer. These nanowires were doped with phosphorus in similar manner as used for the intrinsic silicon wafer. Standard photolithography process was used to fabricate metal electrodes for the formation of nanowire based field effect transistor (NW-FET). The electrical properties of a representative nanowire device were measured by a semiconductor device analyzer and a probe station.

A detailed procedure for surface doping of Silicon interfaces is provided. The ultra-shallow surface doping is demonstrated by using phosphorus containing monolayers and rapid annealing process. The method can be used for doping of macroscopic area surfaces as well as nanostructures.

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra ...

Evaluating Plasmonic Transport in Current-carrying Silver Nanowires

Plasmonics is an emerging technology capable of simultaneously transporting a plasmonic signal and an electronic signal on the same information support1,2,3. In this context, metal nanowires are especially desirable for realizing dense routing networks4. A prerequisite to operate such shared nanowire-based platform relies on our ability to electrically contact individual metal nanowires and efficiently excite surface plasmon polaritons5 in this information support. In this article, we describe a protocol to bring electrical terminals to chemically-synthesized silver nanowires6 randomly distributed on a glass substrate7. The positions of the nanowire ends with respect to predefined landmarks are precisely located using standard optical transmission microscopy before encapsulation in an electron-sensitive resist. Trenches representing the electrode layout are subsequently designed by electron-beam lithography. Metal electrodes are then fabricated by thermally evaporating a Cr/Au layer followed by a chemical lift-off. The contacted silver nanowires are finally transferred to a leakage radiation microscope for surface plasmon excitation and characterization8,9. Surface plasmons are launched in the nanowires by focusing a near infrared laser beam on a diffraction-limited spot overlapping one nanowire extremity5,9. For sufficiently large nanowires, the surface plasmon mode leaks into the glass substrate9,10. This leakage radiation is readily detected, imaged, and analyzed in the different conjugate planes in leakage radiation microscopy9,11. The electrical terminals do not affect the plasmon propagation. However, a current-induced morphological deterioration of the nanowire drastically degrades the flow of surface plasmons. The combination of surface plasmon leakage radiation microscopy with a simultaneous analysis of the nanowire electrical transport characteristics reveals the intrinsic limitations of such plasmonic circuitry.

Silver nanowires can simultaneously transport electrons and optical information in the form of surface plasmons. A procedure is described here to realize such a shared circuitry and the limitations at propagating both information carriers are evaluated.

Plasmonics is an emerging technology capable of simultaneously transporting a plasmonic signal and an electronic signal on the same information ...

Gold Nanostar Synthesis with a Silver Seed Mediated Growth Method

The physical, chemical and optical properties of nano-scale colloids depend on their material composition, size and shape 1-5. There is a great interest in using nano-colloids for photo-thermal ablation, drug delivery and many other biomedical applications 6. Gold is particularly used because of its low toxicity 7-9. A property of metal nano-colloids is that they can have a strong surface plasmon resonance 10. The peak of the surface plasmon resonance mode depends on the structure and composition of the metal nano-colloids. Since the surface plasmon resonance mode is stimulated with light there is a need to have the peak absorbance in the near infrared where biological tissue transmissivity is maximal 11, 12.
We present a method to synthesize star shaped colloidal gold, also known as star shaped nanoparticles 13-15 or nanostars 16. This method is based on a solution containing silver seeds that are used as the nucleating agent for anisotropic growth of gold colloids 17-22. Scanning electron microscopy (SEM) analysis of the resulting gold colloid showed that 70 % of the nanostructures were nanostars. The other 30 % of the particles were amorphous clusters of decahedra and rhomboids. The absorbance peak of the nanostars was detected to be in the near infrared (840 nm). Thus, our method produces gold nanostars suitable for biomedical applications, particularly for photo-thermal ablation.

We synthesized star shaped gold nanostars using a silver seed mediated growth method. The diameter of the nanostars ranges from 200 to 300 nm and the number of tips vary from 7 to 10. The nanoparticles have a broad surface plasmon resonance mode centered in the near infrared.

黄金Nanostar合成银种子介导的生长方法

The physical, chemical and optical properties of nano-scale colloids depend on their material composition, size and shape 1-5. There is a great interest ...

生物工程

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 ...

化学

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 ...

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 ...

Iron Nanowire Fabrication by Nano-Porous Anodized Aluminum and its Characterization

Magnetic nanowires possess unique properties that have attracted the interest of different fields of research, including basic physics, biomedicine, and data storage. We demonstrate a fabrication method for iron (Fe) nanowires&#160;via electrochemical deposition into anodic&#160;alumina oxide (AAO) templates. The templates are fabricated by anodization of aluminum (Al) discs, and the pore length and diameter are controlled by changing the anodizing conditions. Pores with an average diameter of around 120 nm are created using oxalic acid as the electrolyte. Using this method, cylindrical nanowires are synthesized, which are released by dissolving the alumina using a selective chemical etchant.

In this work, we describe a&#160;protocol to fabricate iron nanowires, including the formation of the porous alumina membrane that is used as the template, electrodeposition into templates using electrolyte solution, and the release of the nanowires into the solution.

纳米孔阳极氧化铝的铁纳米线制造及其特性

Magnetic nanowires possess unique properties that have attracted the interest of different fields of research, including basic physics, biomedicine, and ...

Microscopic Visualization of Porous Nanographenes Synthesized through a Combination of Solution and On-Surface Chemistry

On-surface synthesis has recently been regarded as a promising approach for the generation of new molecular structures. It has been particularly successful in the synthesis of graphene nanoribbons, nanographenes and intrinsically reactive and instable, yet attractive species. It is based on the combination of solution chemistry aimed at preparation of appropriate molecular precursors for further ultra-high vacuum surface assisted transformations. This approach also owes its success to an incredible development of characterization techniques, such as scanning tunneling/atomic force microscopy and related methods, which allow detailed, local characterization at atomic scale. While the surface-assisted synthesis can provide molecular nanostructures with outstanding precision, down to single atoms, it suffers from basing on metallic surfaces and often limited yield. Therefore, the extension of the approach away from metals and the struggle to increase productivity seem to be significant challenges toward wider applications. Herein, we demonstrate the on-surface synthesis approach for generation of non-planar nanographenes, which are synthesized through a combination of solution chemistry and sequential surface-assisted processes, together with the detailed characterization by scanning probe microscopy methods.

<meta charset="utf8"></head><body>通过溶液和表面化学相结合合成的多孔纳米石墨烯的微观可视化

A combination of solution and surface assisted synthesis opens new directions in the atomically precise synthesis of nanostructures. Scanning tunneling microscopy (STM) supplemented by non-contact atomic force microscopy (nc-AFM) enables detailed characterization of newly designed and generated carbon-based nano-objects.