Name: solvothermal synthesis of mil-96 and uio-66-nh2 on atomic layer deposited metal oxide coatings on fiber mats
Uploaded: 2018-06-13T14:45:00
Description: Watch this Scientific Journal Video about Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats at JoVE.com

作者感谢他们的合作者在 RTI 国际, 美国陆军内蒂克士兵 RD & E 中心, 埃奇伍德化学和生物中心。他们还感谢他们的资金来源, 即防务减少威胁机构。

1. 铝2O3在纤维垫上的原子层沉积 (限期)
<ol><li>在反应堆船上放置 2.54 x 2.54 厘米2聚丙烯织物样品 (一个薄, 刚性, 金属网架)。图 2给出了反应堆的示意图。</li>
	<li>打开压力表。从反应堆盖上取下扣。在 LabView 系统中打开手动控制。在限期反应堆上关闭托架氮气和闸阀。打开排气口氮气。</li>
	<li>拆除反应堆盖后, 将织物样品装入限期反应堆。更换反应...

<ol>
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限期涂敷对 MOF 的粘附和加载有很大影响。首先, 根据基材和限期前体的类型, 限期可在纤维周围形成一个独特的外壳, 或扩散到纤维中, 以形成一个渐进过渡到金属氧化物涂层20。在棉和尼龙基体上观察到了硬壳, 在适当的条件下, 在聚丙烯中可以观察到扩散层。第二, 扩散到纤维也可以通过改变沉积温度20,24来控制。较高的温度增加了限...

金属-有机框架是由由有机分子连接器桥接的活性金属星团中心组成的结晶结构, 可提供较大的孔隙度和表面积。它们的结构、孔隙度和功能可以通过选择适当的簇和连接器来设计, 导致表面面积高达7000米2/克MOF1,2。它们的高孔隙度和表面积使得 MOFs 在从能源生产到环境关注到生物过程1、3等领域的吸附、分离和异质催化方面具有多样化的适用性, 4,5,6。
许多 MOFs 在选择性地吸附挥发性有机化合物和温室气体或催化降解可能对人类健康或环境有害的化学物质方面取得了成功。特别是, MIL-96 (Al) 已经表明有选择地吸附含氮挥发性有机化合物 (挥发性有机化合物), 由于在氮气组中的孤对电子的可用, 以配合目前在金属簇7中的弱路易斯酸 Al。MIL-96 也被证明吸附气体, 如 CO2, 对二甲苯, 和m-二甲苯8,9。MOF 吸附选择性取决于金属簇的路易斯酸和孔隙大小。MIL-96 的孔隙大小随温度的增加而增大, trimethylbenzene 的吸附能力随温度的升高而增加, 并给出了吸附温度调节选择性的机会9。
在这里的第二个 MOF, UiO-66-NH2已经被证明催化降解化学战剂 (CWAs) 和模拟物。链接器上的胺组可在有辱人格的神经毒剂上提供协同作用, 同时防止剂降解产物不可逆转地与锆团簇结合并毒害 MOF10。UiO-66-NH2具有催化水解二甲基对硝基苯磷酸 (DMNP), 半衰期在缓冲条件下短至0.7 分钟, 比其基部 MOF UiO-6611、12快20倍。
虽然这些吸附和催化性能是有希望的, MOFs 的物理形式, 主要是散装粉, 可能难以纳入气体捕获和过滤平台, 而不增加大量的散装, 堵塞毛孔, 或减少 MOF灵活性。另一种方法是创建 MOF 功能性织物。MOFs 已被纳入多种方式的织物, 包括静电纺丝 MOF 粉末/聚合物浆料, 粘合剂混合, 喷涂, 溶剂热合成生长, 微波合成, 和逐层增长方法13,14,15,16,17,18. 在这些情况下, 静电纺丝和聚合物粘合剂会导致 MOF 上被堵塞的功能部位, 因为它们封装在聚合物中, 大大降低了吸附能力和反应性。此外, 许多这些技术无法在纤维上产生保形涂层, 因为视线困难或粘附/核化差, 以及对纯静电相互作用的依赖。另一种方法是先将织物涂上金属氧化物, 以允许与 MOF18,19的更强的表面相互作用。
金属氧化物沉积的一种方法是原子层沉积 (限期)。限期是一种沉积保形薄膜的技术, 可控于原子尺度。该工艺利用两个半反应, 只发生在基体表面被涂覆。第一步是对含金属的前驱体进行剂量反应, 它与表面上的羟基发生化学反应, 留下一个 metallated 表面, 而多余的反应物从系统中清除。第二反应物是含氧反应物, 通常是水, 与金属部位发生反应, 形成金属氧化物。再次, 过剩的水和任何反应产品从系统中清除。这些交替剂量和清洗可以重复, 直到达到预期的胶片厚度 (图 1)。原子层沉积是特别有用的, 因为小尺度的气相前体允许在每一个表面上的共形薄膜, 复杂的拓扑结构, 如纤维垫。此外, 对于聚丙烯等聚合物, 其限期条件可以使涂层扩散到纤维表面, 为未来 MOF 增长20提供了强有力的锚定。
在传统的溶剂热合成合成过程中, 通过增加功能基团和粗糙度18,20, 金属氧化物涂层可以增加纤维的成核部位。我们的小组先前已经表明, 限期金属氧化物基层是有效的 UiO-6X, HKUST-1, 和其他合成通过各种途径的溶剂热合成, 逐层, 和羟基双盐转换方法13,17, 18,21,22,23。这里我们演示了两种合成类型。通过将铝2O3的限期涂层直接转化为 MOF, 通过有机链接器的扩散, 形成了材料。通过在等表征方法酸溶液和加热中浸没一个 Al2O3的涂布纤维垫, 有机链接器扩散到金属氧化物涂层中, 形成 MIL-96。这导致在每个纤维表面强烈黏附, 保形 MOF 涂层。第二种合成方法要求使用金属和有机前体进行典型的 UiO-66-NH2热液合成, 但添加了一个金属氧化物涂层纤维垫, MOF nucleates。对于这两种合成方法, 产生的产物由 MOF 晶体的保形薄膜组成, 该薄膜强烈附着在支撑织物上。在 MIL-96 的情况下, 这些可以被纳入过滤器, 以吸附挥发性有机化合物或温室气体。对于 UiO-66-NH2 , 这些织物可以很容易地被纳入到轻型防护服装的军事人员, 第一反应, 和平民持续防御 CWA 攻击。

<table border="0" cellpadding="0" cellspacing="0" width="625">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">trimethylaluminum</td>
			<td style="width:123px;">Strem Chemicals</td>
			<td style="width:119px;">93-1360</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">home-built ALD reactor</td>
			<td style="width:123px;">N/A</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">nitrogen cylinder</td>
			<td style="width:123px;">Arc3</td>
			<td style="width:119px;">UN1066</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">trimesic acid</td>
			<td style="width:123px;">Sigma-Aldrich</td>
			<td style="width:119px;">482749-500G</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">ethanol</td>
			<td style="width:123px;">Koptec</td>
			<td style="width:119px;">V1001</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">teflon lined autoclave</td>
			<td style="width:123px;">PARR Instrument Company</td>
			<td style="width:119px;">4760-1211</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">isotemp furnace</td>
			<td style="width:123px;">Fisher Scientific</td>
			<td style="width:119px;">F47925</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Zirconium (IV) chloride</td>
			<td style="width:123px;">Alfa Aesar</td>
			<td style="width:119px;">12104</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">2-aminoterephthalic acid</td>
			<td style="width:123px;">Acros Organics</td>
			<td style="width:119px;">278031000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">N,N-dimethylformamide</td>
			<td style="width:123px;">Fisher Scientific</td>
			<td style="width:119px;">D119-4</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Hydrochloric Acid</td>
			<td style="width:123px;">Fisher Scientific</td>
			<td style="width:119px;">A481-212</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Polypropylene fiber mats</td>
			<td style="width:123px;">N/A</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Polyamide fiber mats</td>
			<td style="width:123px;">N/A</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
	</tbody>
</table>

solvothermal synthesis of mil-96 and uio-66-nh2 on atomic layer deposited metal oxide coatings on fiber mats

金属-有机框架 (MOFs), 其中含有活性金属簇和有机配体, 允许大孔隙和表面区域, 已证明有效的气体吸附, 分离和催化。MOFs 通常被合成为散装粉, 需要额外的工艺来将它们粘附在功能性设备和织物上, 从而降低粉末的孔隙度和吸附能力。在这里, 我们演示了一个方法的第一涂层织物的金属氧化物薄膜使用原子层沉积 (限期)。这个过程在每个纤维上创建可控厚度的保形薄膜, 同时为 MOF 成核提供了更具反应性的表面。在溶剂热合成 MOF 合成过程中, 通过淹没在溶液中的限期涂层织物, MOFs 在纤维上创建一个保形, 粘附涂层, 导致 mof 功能性织物, 没有附加的黏附材料, 可能会阻止 MOF 毛孔和功能网站。这里我们演示了两种溶剂热合成合成方法。首先, 我们在聚丙烯纤维上形成一个 96 (Al) 层, 使用合成条件将金属氧化物转化为 MOF。使用不同厚度的初始无机薄膜, 将有机连结剂扩散到无机, 使我们能够控制 MOF 在织物上的负载程度。其次, 我们执行溶剂热合成合成的 UiO-66-NH2 , 其中 mof nucleates 在保形金属氧化物涂层上 polyamide-6 (PA-6) 纤维, 从而产生一个统一的和保形薄膜的 mof 在织物上。所得材料可直接纳入过滤装置或防护服, 消除松散粉末的笨拙品质。

为了描述 MOF/织物材料, 我们描绘了两个与实测面积有关的术语。首先, 投影表面积, cm2预计, 是指的宏观大小的织物样本测量与标尺, i. e., 样本的投影阴影区域。第二表面积的利益是赌注表面积, 计算从一个氮气等温线获得的 77 K。这些值以 m2/克结构、m2/gmof或 m2/gmof + 织物的单位给出, 分别对应于在 MOF...

Watch this Scientific Journal Video about Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats at JoVE.com

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

金属-有机框架在储气和异质催化中是有效的, 但典型的合成方法导致了不易融入智能材料的松散粉末。我们演示了一种第一涂层织物与限期金属氧化物, 导致在织物上的 MOF 保角膜溶剂热合成合成。

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 ...

Research

JoVE Journal

Chemistry

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

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

对磷酸增强富集制备高度多孔配位聚合物涂层的孔聚合物石柱的

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

科研

化学

Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes

层 - 层的合成和独立式共轭微孔聚合物纳米薄膜的转移

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in ...

Improved Heterojunction Quality in Cu2O-based Solar Cells Through the Optimization of Atmospheric Pressure Spatial Atomic Layer Deposited Zn1-xMgxO

Improved Heterojunction Quality in Cu2O-based Solar Cells Through the Optimization of Atmospheric Pressure Spatial Atomic Layer Deposited Zn1-xMgxO

在铜改善异质结质量<sub&gt; 2</sub&gt; O型的太阳能电池通过大气压力的空间原子层沉积的优化<br /&gt;锌<sub&gt; 1-X</sub&gt;镁<sub系列&gt; X</sub&gt; 0

Atmospheric pressure spatial atomic layer deposition (AP-SALD) was used to deposit n-type ZnO and Zn1-xMgxO thin films onto p-type thermally oxidized Cu2O ...

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

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 ...

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

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 ...

Aerosol-assisted Chemical Vapor Deposition of Metal Oxide Structures: Zinc Oxide Rods

金属氧化物结构的气溶胶辅助化学气相沉积: 氧化锌棒

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, ...

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

原位金纳米粒子合成快速 Nanoprobe 信号增强

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity ...

Molten-Salt Synthesis of Complex Metal Oxide 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. ...

Niobium Oxide Films Deposited by Reactive Sputtering: Effect of Oxygen Flow Rate

活性溅射沉积的氧化氮薄膜：氧气流速效应

Reactive sputtering is a versatile technique used to form compact films with excellent homogeneity. In addition, it allows easy control over deposition ...

The Effect of Anodization Parameters on the Aluminum Oxide Dielectric Layer of Thin-Film Transistors

阳极化参数对薄膜晶体管氧化铝介电层的影响

Aluminum-oxide (Al2O3) is a low cost, easily processable and high dielectric constant insulating material that is particularly appropriate for use as the ...