Name: a salt-templated synthesis method for porous platinum-based macrobeams and macrotubes
Uploaded: 2020-05-18T15:00:00
Description: Watch this Scientific Journal Video about A Salt-Templated Synthesis Method for Porous Platinum-based Macrobeams and Macrotubes at JoVE.com

这项工作由美国军事学院学院发展研究基金赠款资助。作者感谢美国陆军战斗力发展指挥部的克里斯托弗·海恩斯博士的帮助。作者还要感谢约书亚·莫勒博士在纽约沃特夫利特的美国陆军CCDC-军备中心使用FIB-SEM。

注意：使用前请咨询所有相关的化学品安全数据表 （SDS）。在进行化学反应时，请使用适当的安全做法，包括使用烟罩和个人防护设备。电化学还原过程中氢气的快速演化会导致反应管中产生高压，导致瓶盖弹出，溶液喷出。确保反应管盖保持协议中指定的打开状态。在烟罩中进行所有电化学还原。
1. 马格努斯的盐衍生物模板制备
注：由于长时间储存会?...

<ol>
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这种合成方法演示了一种简单、相对快速的方法，实现了高表面积铂基大管和宏光带，具有可调谐纳米结构和元素成分，无需任何结合材料，可压入无固定薄膜。使用Magnus的盐衍生物作为高纵横比针形模板，通过盐模板的化学测量控制产生的金属成分，并结合选择还原剂，控制大管和宏波孔多孔侧壁和横截面结构的纳米结构。合成方法可以通过更改用于形成模板的盐比而变化：Pt2+:P（t 2-，Pt</...

已开发出多种合成方法，以获得高表面积、多孔铂基材料，主要用于催化应用，包括燃料电池1。实现这种材料的一个策略是合成球体、立方体、电线和管2、3、4、5等形式的单分散纳米粒子。为了将离散纳米粒子集成到功能装置的多孔结构中，聚合物粘结剂和碳添加剂通常需要6，7。此策略需要额外的处理步骤、时间，并可能导致质量特定性能下降，以及在扩展设备使用8期间聚集纳米粒子。另一种策略是推动合成纳米粒子的合合成金属凝胶，随后超临界干燥9，10，11。虽然贵金属的溶胶凝胶合成方法的进步将凝胶时间从数周缩短到数小时或几分钟，但由此产生的单体往往在机械上脆弱，妨碍了其在装置12中的实际应用。
铂合金和多金属三维多孔纳米结构为催化特异性提供可调谐性，并解决铂金13、14的高成本和相对稀缺性问题。虽然有许多关于铂铂15、16和铂铜17、18、19离散纳米结构以及其他合金组合20的报道，但用于实现三维铂合金和多金属结构解决方案技术的综合策略很少。
最近，我们展示了使用高浓度盐溶液和还原剂，以迅速产生黄金，铂，和铂金属凝胶21，22。高浓度盐溶液和还原剂也用于合成生物聚合物贵金属复合材料使用明胶，纤维素，和丝绸23，24，25，26。不溶性盐是可减少的离子浓度最高的，肖和同事用来证明二维金属氧化物27、28的合成。在高浓度盐溶液中对多孔贵金属气凝胶和复合材料进行示范，并利用不溶性盐的高密度，我们利用马格努斯的盐和衍生物作为形状模板，合成多孔贵金属大管和微孔29、30、31、32。
马格努斯的盐组装从添加相反充电的方形平面铂离子 [PtCl4]2 - 和[Pt（NH3]4=2 = 33。以类似的方式，Vauquelin的盐从相反充电的铂离子组合中形成[PdCl4]2- 和[Pd（NH3）4=2= 34。前体盐浓度为100 mM，产生的盐晶体形成10至100微米的针，平方宽度约为100纳米至3μm。虽然盐模板是电荷中性，改变马格努斯的盐衍生物在离子物种之间的测量，包括[Cu（NH3）4+2]，允许控制由此产生的金属比率降低。离子的组合，以及化学还原剂的选择，导致宏管或宏束与方形横截面和多孔纳米结构组成的融合纳米粒子或纳米纤维。磁管和宏光纳米也被压入自由立立膜，电化学活性表面积通过电化学阻抗光谱和循环电压测量确定。盐模板方法用于合成铂金大管29，铂金-铂宏波带31，并努力降低材料成本，并调整催化活性，结合铜，铜铂巨管32。盐模板方法也演示了Au-Pd和Au-Pd-Cu二进制和三元金属宏管和纳米泡30。
在这里，我们提出了一种方法，从不溶性马格努斯的盐针模板29，31，32合成铂金，铂金，铜-铂，和铜-铂双金属多孔宏管和宏波。盐针模板中离子组测定的控制可控制化学还原后产生的金属比，并可以通过 X 射线衍射测量和 X 射线光电子光谱法进行验证。由此产生的宏管和宏带可以组装并形成具有手压的立式薄膜。所得薄膜表现出高电化学活性表面积 （ECSA），由 H2SO4和 KCl 电解质中的电化学阻抗光谱和环伏测量测定。此方法提供了一种合成途径，以快速和可扩展的方式控制铂基金属成分、孔隙度和纳米结构，这些方法可推广到更广泛的盐模板中。

<table>
	<tbody>
		<tr>
			<td>50 mL Conical Tubes</td>
			<td>Corning Costar Corp.</td>
			<td>430290</td>
			<td></td>
		</tr>
		<tr>
			<td>Ag/AgCl Reference Electrode</td>
			<td>BASi</td>
			<td>MF-2052</td>
			<td></td>
		</tr>
		<tr>
			<td>Cu(NH3)4SO4&#159;&#8226;H2O</td>
			<td>Sigma-Aldrich</td>
			<td>10380-29-7</td>
			<td></td>
		</tr>
		<tr>
			<td>dimethylamine borane (DMAB)</td>
			<td>Sigma-Aldrich</td>
			<td>74-94-2</td>
			<td></td>
		</tr>
		<tr>
			<td>K2PtCl4</td>
			<td>Sigma-Aldrich</td>
			<td>10025-99-7</td>
			<td></td>
		</tr>
		<tr>
			<td>Miccrostop Lacquer</td>
			<td>Tober Chemical Division</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr>
			<td>Na2PdCl4</td>
			<td>Sigma-Aldrich</td>
			<td>13820-40-1</td>
			<td></td>
		</tr>
		<tr>
			<td>NaBH4</td>
			<td>Sigma-Aldrich</td>
			<td>16940-66-2</td>
			<td></td>
		</tr>
		<tr>
			<td>Polarized Optical Microscope</td>
			<td>AmScope</td>
			<td>PZ300JC</td>
			<td></td>
		</tr>
		<tr>
			<td>Potentiostat</td>
			<td>Biologic-USA</td>
			<td>VMP-3</td>
			<td>Electrochemical analysis-EIS, CV</td>
		</tr>
		<tr>
			<td>Pt wire electrode</td>
			<td>BASi</td>
			<td>MF-4130</td>
			<td></td>
		</tr>
		<tr>
			<td>Pt(NH3)4Cl2&#159;&#8226;H2O</td>
			<td>Sigma-Aldrich</td>
			<td>13933-31-8</td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning Electron Microscope</td>
			<td>FEI</td>
			<td>Helios 600</td>
			<td>EDS performed with this SEM</td>
		</tr>
		<tr>
			<td>Shelf Rocker</td>
			<td>Thermo Scientific</td>
			<td>Vari-Mix&#8482; Platform Rocker</td>
			<td></td>
		</tr>
		<tr>
			<td>Snap Cap Microcentrifuge Tubes, 1.7 mL</td>
			<td>Cole Parmer</td>
			<td>UX-06333-60</td>
			<td></td>
		</tr>
		<tr>
			<td>X-ray diffractometer</td>
			<td>PanAlytical</td>
			<td>Empyrean</td>
			<td>X-ray diffractometry</td>
		</tr>
		<tr>
			<td>X-ray photoelectron spectrometer</td>
			<td>ULVAC PHI - Physical Electronics</td>
			<td>VersaProbe III</td>
			<td></td>
		</tr>
	</tbody>
</table>

a salt-templated synthesis method for porous platinum-based macrobeams and macrotubes

高表面积多孔贵金属纳米材料的合成通常依赖于预制纳米粒子的耗时结合，然后是冲洗和超临界干燥步骤，往往导致机械易碎材料。本文提出了一种从不溶性盐针模板中合成纳米结构多孔多孔铂基宏管和宏波带的方法。相反带电的铂、铂和铜方形平面离子的组合导致不溶性盐针的快速形成。根据盐模板中金属离子的计量比和化学还原剂的选择，大管或宏束形成由熔融纳米粒子或纳米纤维组成的多孔纳米结构。通过X射线衍射和X射线光电子光谱确定，宏管和大束的元素组成由盐模板中金属离子的测量比控制。宏管和宏光纳米可压入自由立地薄膜中，电化学活性表面积通过电化学阻抗光谱和循环电压测量确定。这种合成方法演示了一种简单、相对快速的方法，实现了高表面积铂基大管和宏光带，具有可调谐纳米结构和元素成分，无需任何结合材料，可压入无固定薄膜。

添加相反带电的方形平面贵金属离子，导致高纵横比盐晶体几乎瞬时形成。在图1中，方形平面离子的线性堆叠以示意图显示，偏振光学显微镜图像显示盐针的细米长为10到100秒。所有铂、铂和铜盐溶液的浓度为 100 mM。虽然盐针模板是电荷中性，因为总阳离子和阳离子电荷相等，但结果盐针的测定度可以随离子的三级组合而变化。例如，铂金铂盐模板的计量与Pt2+:P d<s...

Watch this Scientific Journal Video about A Salt-Templated Synthesis Method for Porous Platinum-based Macrobeams and Macrotubes at JoVE.com

A Salt-Templated Synthesis Method for Porous Platinum-based Macrobeams and Macrotubes

提出了一种合成方法，通过化学还原不溶性盐针模板，获得多孔铂基大管和宏波带的方形横截面。

多孔铂基微波和宏管的盐模板合成方法

The synthesis of high surface area porous noble metal nanomaterials generally relies on time consuming coalescence of pre-formed nanoparticles, followed ...

该协议提供了一种简单、较快的方法，用于合成铂合金宏带和具有方形横截面的宏管中的高表面积、高纵横比铂金。盐和电镀方法允许控制模板金属离子比和由此产生的质量组成，以及宏效应和宏管纳米结构。宏光带和微管压膜可以满足催化和传感应用对整体三维电极的需求。麦格纳盐衍生物在化学上被减少形成宏带和大管的能力表明，盐模板合成方法可以应用于更广泛的金属盐。要将马格努斯盐以1比0至1铂2正到铂两负比，将0.5毫升100毫摩尔钾四氯酸酸加入微烟管中，并强力移液0.5毫升100毫四甲胺质（II）氯化水合物入水管。由此产生的一毫升体积盐针模板解决方案将呈现不透明如绿色。要准备一至零铂金盐针模板，在水中加入0.5毫升四胺铂（II）氯化水合物到微离心管中，并强力移液器0.5毫升100毫升四氯硅酸钠到管中。要准备2至1至1铂金-铂盐针模板，将0.25毫升100毫摩尔四氯硅酸钠和0.25毫升100毫摩尔钾四氯四酸酯加入微富管。在用力将0.5毫升的100毫升四甲酸胺（II）氯化水水向管子中移液之前，将管子旋转三到五秒钟。为了准备三至一至两个铂金盐针模板，移液器0.167毫升100毫升四氯硅钠和0.333毫升100毫升四氯酸钾到微烟管。涡旋后，用力移液器 0.5 毫升 100 毫摩尔四甲苯胺（II）氯化水水到管内。铂金比例较高的盐模板应产生更绿的颜色，而具有增加铂含量的模板在溶液中会产生更多的橙色、粉红色和棕色。要准备一至零至一盐比铜-铂盐针模板，在微烟管中加入0.5毫升100毫摩尔钾四氯酸盐，并强行将0.5毫升100毫摩尔四甲胺铜（II）硫酸盐加入水中的微烟管。要准备三至一至二盐比铜-铂盐针模板，将 0.167 毫升 100 毫升四甲酸酯（II）氯化水合水和 0.333 毫升 100 毫升四铵铜（II）硫酸盐加入水中。涡旋后，强行向管中加入0.5毫升100毫摩尔四氯酸钾。为准备二到一的盐比铜-铂盐针模板，加入0.25毫升100毫摩尔四甲酸酯铂（II）氯化水合水和0.25毫升100毫摩尔四甲胺可可（II）硫酸盐在水中的微烟管，并涡旋微烟管3至5秒。然后，用力将0.5毫升100毫升四氯钾的移液器压到管子上。为准备一至零盐比铜 - 铂盐针模板，移液器 0 . 5 毫升 100 毫升四甲酸铅铂（ II ）氯化水水到微富管，并强力移液器 0 . 5 毫升 100 毫摩尔钾四氯化氯板酸管中，获得 1 毫升盐针模板溶液。铜离子和铂离子的结合将导致形成紫色多云溶液，这种溶液不像铂和铂溶液那样不透明。要对铂-铂盐模板进行化学还原，请将 50 毫升 0.1 摩尔钠波罗氢溶液添加到四个 50 毫升锥形管中，并将一个铂金-铂盐模板溶液的一毫升体积添加到每个管中。要对铜-铂盐模板进行化学还原，请将 50 毫升 0.1 摩尔 DMAB 溶液添加到四个 50 毫升锥形管中，并将一个铜-铂盐模板溶液的整个 1 毫升体积添加到烟气罩下的每个管中。24 小时后，将每个减少溶液中的上经液慢慢去掉到废物容器中，小心，不要倒出样品，将沉淀物转移到新的 50 毫升管中。将每个管充满50毫升的去化水，用轻轻的摇动孵育紧盖的管子24小时。第二天，将管子直立在管架上15分钟，让样品沉淀，然后慢慢从上流液中倾泻而下。向每个管子补充50毫升的电离水，并再摇动样品24小时。在孵育结束时，将管子放在机架中 15 分钟，然后尽可能多地清除透明或灰色的超自然物。要准备宏管和宏波光膜，请使用移液器或铲子将沉淀材料从每个管轻轻地转移到单独的玻璃幻灯片上，并将样品整合到均匀的堆中，大约 0.5 毫米。然后将幻灯片放在 24 小时内不会受到气流干扰的位置。当样品干燥后，将第二个玻璃幻灯片放在每个干燥的减少样品上，并手动将大约 200 千帕的力施加到顶部幻灯片上，以创建宏管薄膜或底部幻灯片上的宏波。对于样品的电子显微镜扫描，使用碳胶带将薄膜固定到扫描电子显微镜样品存根上，将初始加速电压设置为 15 千伏，将光束电流设置为 2.7 至 5.4 皮安。然后缩小到较大的采样区域，并收集能量分散的 X 射线光谱，以量化样本的元素组成。对于 X 射线衍射-分型分析，将薄膜样品幻灯片放到扫描阶段，对 45 千伏的 5 度到 90 度衍射角度进行 X 射线衍射扫描，在铜 K-α 辐射下，每步为 0.0130 度和 20 秒。要使活性材料的电化学测量正常化，将样品转移到单个电化学小瓶中，并在室温下轻轻向每个样品中加入0.5摩尔硫酸，进行24小时的孵育。第二天，将漆涂线与每个电化学小瓶底部的薄膜顶部接触的单个三个电极电池的一毫米外露尖端放置。在零伏特下以 10 毫伏的 10 毫伏下弦波执行电化学阻抗光谱，从一兆赫到一毫赫。然后使用负 0.2 至 1.2 伏的电压范围执行循环电压测量，扫描速率为 10、25、50、75 和 100 毫伏/秒。添加相反带电的方形平面贵金属离子，导致高纵横比盐晶体几乎瞬时形成。Magnus盐的化学还原与铂正比和铂负离子的一比一形成，并且通过具有空心内腔和多孔侧壁的宏管减少波罗氢钠的结果。宏管通常符合盐针模板的几何形状，平面侧壁和方形横截面，DMAB减少铜铂宏管呈现最明显和最大的方形横截面，约三微米的两侧。DMAB 减少的铜铂宏管侧壁也表现出高度纹理的表面，没有显著的孔隙度。铂金和铂金-铂金宏管和宏束化学成分最初可以具有 X 射线衍射特征。DMAB 减少的宏管的 X 射线衍射分析显示，根据相对盐模板的三元测量，超强加的峰值转向铂金或铜，表明合金成分。波罗氢钠减少了铜-铂宏束，表现出明显的铜和铂X射线衍射峰值，表明是双金属成分。铂金大管的X射线光电子光谱表明几乎没有氧化物物种的证据，表明表面具有催化活性。铂金-铂金宏束的X射线光电子光谱也未显示金属氧化物含量。嗯，压膜可以用钳子操纵。将薄膜转移到电化学瓶中时，必须小心，以防止压裂。鉴于能够将宏波和宏管压入整片中，还可以执行机械特性来确定弹性和柔性模块化。盐模板，用于合成毛孔，高表面积材料应使研究人员能够探索更广泛的金属盐和由此产生的金属、合金和多金属材料。

Research

JoVE Journal

Chemistry

Seeded Synthesis of CdSe/CdS Rod and Tetrapod Nanocrystals

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

Synthesis and Purification of Iodoaziridines Involving Quantitative Selection of the Optimal Stationary Phase for Chromatography

合成和Iodoaziridines纯化涉及定量选择最优固定相的色谱

The highly diastereoselective preparation of cis-N-Ts-iodoaziridines through reaction of diiodomethyllithium with N-Ts aldimines is described. ...

Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials

超临界氮处理的活性多孔材料的净化

Supercritical fluid extraction and drying methods are well established in numerous applications for the synthesis and processing of porous materials. ...

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

根据环境条件的金纳米粒子的稳定低聚簇的大小控制合成的一种简便方法

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

Synthesis and Exfoliation of Discotic Zirconium Phosphates to Obtain Colloidal Liquid Crystals

合成与盘状磷酸盐锆剥落获取胶体液晶

Due to their abundance in natural clay and potential applications in advanced materials, discotic nanoparticles are of interest to scientists and ...

Synthesis of Core-shell Lanthanide-doped Upconversion Nanocrystals for Cellular Applications

核壳镧系掺杂转换纳米晶的合成及其在蜂窝中的应用

Lanthanide-doped upconversion nanocrystals (UCNs) have attracted much attention in recent years based on their promising and controllable optical ...

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

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

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 ...

Deposition of Porous Sorbents on Fabric Supports

织物支架上多孔吸附剂的沉积

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material ...

Chemical Synthesis of Porous Barium Titanate Thin Film and Thermal Stabilization of Ferroelectric Phase by Porosity-Induced Strain

孔隙诱导应变法合成多孔钛酸钡薄膜及铁电相热稳定性

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its ...

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

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 ...