Name: solvothermal synthesis of mil-96 and uio-66-nh2 on atomic layer deposited metal oxide coatings on fiber mats
Uploaded: 2018-06-13T14:45:00.000+00:00
Duration: 6 min
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。更换反应堆盖并打开闸阀。关闭排气口并打开托架氮气。关闭手动控制。</li>
	<li>在布料上装载 Al2O3的配方。该食谱将交替剂量 trimethylaluminum (TMA) 1.2 s, 其次是三十年代干氮气清除或剂量水1秒后, 六十年代干氮清除。将食谱设置为运行1000个周期。</li>
	<li>将质量流量控制器设置为20立方和炉膛温度为90°c (炉接口84°c)。</li>
	<li>打开手动阀门的 TMA 和水。关闭压力表。更换反应堆盖上的扣。在接口上按 "开始"。</li>
	<li>配方完成后, 打开压力表。从反应堆盖上取下扣。在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>取下反应堆盖和样品船。重新密封反应堆。 注意: 此时可能暂停该过程。</li>
</ol>2. 在 Polyamide-6 (PA-6) 纤维垫上2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 PA-6 织物样品 (一个薄, 刚性, 金属网架)。</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。更换反应堆盖并打开闸阀。关闭排气口并打开托架氮气。关闭手动控制。</li>
	<li>在布料上装上2的食谱。该食谱将交替剂量 TiCl4为 1 s, 其次是四十年代干氮气清除或剂量水1秒后, 六十年代干氮气清除。将食谱设置为运行300个周期。</li>
	<li>将质量流量控制器设置为20立方和炉膛温度为90°c (炉接口84°c)。</li>
	<li>打开手动阀 TiCl4和水。关闭压力表。更换反应堆盖上的扣。在接口上按 "开始"。</li>
	<li>配方完成后, 打开压力表。从反应堆盖上取下扣。在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>取下反应堆盖和样品船。重新密封反应堆。 注意: 此时可能暂停该过程。</li>
</ol>3. 溶剂热合成合成 MIL-96
<ol><li>添加0.0878 克 H3BTC 到80毫升玻璃烧杯。</li>
	<li>在烧杯中加入12毫升的 H2O 和12毫升乙醇。</li>
	<li>将磁性搅拌10分钟或直到 H3BTC 完全溶解。</li>
	<li>将溶液放在聚四氟乙烯衬里压力容器中。</li>
	<li>将 Al2O3涂层聚丙烯添加到溶液中, 并在网格支撑上支撑织物, 这样它就不会平躺在容器的底部。</li>
	<li>密封压力容器并将其放在炉内110摄氏度, 24 小时。</li>
	<li>在允许样品冷却后, 将织物样品放在烧杯中的网篮中。用乙醇洗两次, 每人12小时。</li>
	<li>样品活化要求在真空下加热6小时85摄氏度, 然后在真空下加热110摄氏度12小时。 注意: 这个过程可以在这里停止。所有样品应存储在干燥中以保持样品激活。</li>
</ol>4. 溶剂热合成合成 UiO-66-NH2
<ol><li>添加0.08 克 ZrCl4到20毫升玻璃闪烁瓶。</li>
	<li>增加20毫升的 n-, n-甲基酰胺 (DMF) 到 ZrCl4 5 毫升的增量。把瓶子盖在增量之间, 让烟雾消散。</li>
	<li>油脂实验解决方案为1分钟。</li>
	<li>将0.062 克的 2-氨基对苯二甲酸酸添加到瓶中, 磁性搅拌溶液5分钟。</li>
	<li>将25µL 的去离子水添加到瓶子里。</li>
	<li>将1.33 毫升的盐酸浓缩到瓶子里。</li>
	<li>在溶液中浸泡2限期涂布色板, 并盖瓶。</li>
	<li>将样品放入炉内85摄氏度, 24 小时。</li>
	<li>在允许样品冷却后, 将织物样品放在烧杯中的网篮中。用80毫升的 DMF 洗两次, 每12小时洗3次, 用80毫升的乙醇洗涤, 每种都为 12 h。</li>
	<li>卸下织物色板后, 过滤残余的 MOF 粉末。用80毫升的 DMF 洗两次, 每12小时洗3次, 用80毫升的乙醇洗涤, 每种都为 12 h。</li>
	<li>样品活化要求在真空下加热6小时85摄氏度, 然后在真空下加热110摄氏度12小时。 注意: 这个过程可以在这里停止。所有样品应存储在干燥中以保持样品激活。</li>
</ol>

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作者没有什么可透露的。

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><tbody><tr><td>trimethylaluminum</td><td>Strem Chemicals</td><td>93-1360</td><td></td></tr><tr><td>home-built ALD reactor</td><td>N/A</td><td></td><td></td></tr><tr><td>nitrogen cylinder</td><td>Arc3</td><td>UN1066</td><td></td></tr><tr><td>trimesic acid</td><td>Sigma-Aldrich</td><td>482749-500G</td><td></td></tr><tr><td>ethanol</td><td>Koptec</td><td>V1001</td><td></td></tr><tr><td>teflon lined autoclave</td><td>PARR Instrument Company</td><td>4760-1211</td><td></td></tr><tr><td>isotemp furnace</td><td>Fisher Scientific</td><td>F47925</td><td></td></tr><tr><td>Zirconium (IV) chloride</td><td>Alfa Aesar</td><td>12104</td><td></td></tr><tr><td>2-aminoterephthalic acid</td><td>Acros Organics</td><td>278031000</td><td></td></tr><tr><td>N,N-dimethylformamide</td><td>Fisher Scientific</td><td>D119-4</td><td></td></tr><tr><td>Hydrochloric Acid</td><td>Fisher Scientific</td><td>A481-212</td><td></td></tr><tr><td>Polypropylene fiber mats</td><td>N/A</td><td></td><td></td></tr><tr><td>Polyamide fiber mats</td><td>N/A</td><td></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 ...

solvothermal-synthesis-mil-96-uio-66-nh2-on-atomic-layer-deposited

Universidad de Cartagena UDEC

Research

JoVE Journal

Chemistry

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

11.4K 次观看.  North Carolina State University. 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。

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

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

单金属和双金属前过渡金属碳化物和氮化物纳米粒子的反相微乳液介导的合成

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

科研

化学

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

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in combination with their outstanding thermal and chemical stability, and low densities. However, their insoluble nature causes problems in their processing since usually applied techniques such as spin coating are not available. Especially for membrane applications, where the processing of CMP as thin films is desirable, the processing problems have hindered their commercial application.
Here we describe the interfacial synthesis of CMP thin films on functionalized substrates via molecular layer-by-layer (l-b-l) synthesis. This process allows the preparation of films with desired thickness and composition and even desired composition gradients.
The use of sacrificial supports allows the preparation of freestanding membranes by dissolution of the support after the synthesis. To handle such ultra-thin freestanding membranes the protection with sacrificial coatings showed great promise, to avoid rupture of the nanomembranes. To transfer the nanomembranes to the desired substrate, the coated membranes are upfloated at the air-liquid interface and then transferred via dip coating.

In this paper we describe the interfacial synthesis of conjugated microporous polymers (CMP) on sacrificial substrates, and the dissolution of the substrate for the preparation of freestanding CMP nanomembranes. In addition, we will describe how the fragile nanomembranes can be transferred to other substrates.

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 ...

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 and a superhydrophobic agent were coated on the HGM surface in one step. TBT and PFOTES were selected as the Ti source and the superhydrophobic agent, respectively. They were both coated on the HGM, and after the hydrothermal process, the TBT turned to anatase TiO2. In this way, a PFOTES/TiO2-coated HGM (MCHGM) was prepared. For comparison, PFOTES single-coated HGM (F-SCHGM) and TiO2 single-coated HGM (Ti-SCHGM) were synthesized as well. The PFOTES and TiO2 coatings on the HGM surface were demonstrated through X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive detector (EDS) characterizations. The MCHGM showed a higher contact angle (153&#176;) but a lower sliding angle (16&#176;) than F-SCHGM, with a contact angle of 141.2&#176; and a sliding angle of 67&#176;. In addition, both Ti-SCHGM and MCHGM displayed similar IR reflectivity values, which were about 5.8% higher than the original HGM and F-SCHGM. Also, the PFOTES coating barely changed the thermal conductivity. Therefore, F-SCHGM, with a thermal conductivity of 0.0479 W/(m&#183;K), was quite like the original HGM, which was 0.0475 W/(m&#183;K). MCHGM and Ti-SCHGM were also similar. Their thermal conductivity values were 0.0543 W/(m&#183;K) and 0.0543 W/(m&#183;K), respectively. The TiO2 coating slightly increased the thermal conductivity, but with the increase in reflectivity, the overall heat-insulation property was enhanced. Finally, since the IR-reflecting property is provided by the HGM coating, if the coating is fouled, the reflectivity decreases. Therefore, with the superhydrophobic coating, the surface is protected from fouling, and its lifetime is also prolonged.

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

This manuscript proposes a soft-chemistry method to synthesize superhydrophobic, TiO2-coated hollow glass microspheres (HGM) with high IR-reflective properties.

二氧化钛<sub&gt; 2</sub与由软化学法合成的超疏水性和高IR反射属性&gt;涂覆的空心玻璃微球

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

通过纳米氧化钇稳定的二氧化锆（YSZ）的支架的高温加工<em&gt;原位</em&gt;碳模板干凝胶

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

工程学

Electrophoretic Crystallization of Ultrathin High-performance Metal-organic Framework Membranes

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and non-porous supports (polymer, ceramic, metal, carbon, and graphene). We developed a novel crystallization technique, which is termed the ENACT approach: the electrophoretic nuclei assembly for the crystallization of highly intergrown thin films (ENACT). This approach allows for a high density of heterogeneous nucleation of MOFs on a chosen substrate via the electrophoretic deposition (EPD) directly from the precursor sol. The growth of well-packed MOF nuclei leads to a highly intergrown polycrystalline MOF film. We show that this simple approach can be used for the synthesis of thin, intergrown zeolite imidazole framework (ZIF)-7 and ZIF-8 films. The resulting 500 nm-thick ZIF-8 membranes show a considerably high H2 permeance (8.3 x 10-6 mol m-2 s-1 Pa-1) and ideal gas selectivities (7.3 for H2/CO2, 15.5 for H2/N2, 16.2 for H2/CH4, and 2655 for H2/C3H8). An attractive performance for C3H6/C3H8 separation is also achieved (a C3H6 permeance of 9.9 x 10-8 mol m-2 s-1 Pa-1 and a C3H6/C3H8 ideal selectivity of 31.6 at 25 &#176;C). Overall, the ENACT process, owing to its simplicity, can be extended to synthesize intergrown thin films of a wide range of nanoporous crystalline materials.

A simple, reproducible, and versatile approach for the synthesis of intergrown, polycrystalline metal-organic framework membranes on a wide range of unmodified porous and non-porous supports is presented.

超薄高性能金属-有机骨架膜的电泳结晶

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous 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. ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared according to the methodology developed by surface organometallic chemistry (SOMC). In this framework, catalytic cycles can be determined by isolating crucial intermediates. All air-sensitive materials are handled under inert atmosphere (using gloveboxes or a Schlenk line) or high vacuum lines (HVLs, &#60;10-5 mbar). The preparation of SiO2-700 (silica dehydroxylated at 700 &#176;C) and subsequent applications (the grafting of complexes and catalytic runs) requires the use of HVLs and double-Schlenk techniques. Several well-known characterization methods are used, such as Fourier-transform infrared spectroscopy (FTIR), elemental microanalysis, solid-state nuclear magnetic resonance spectroscopy (SSNMR), and state-of-the-art dynamic nuclear polarization surface enhanced NMR spectroscopy (DNP-SENS). FTIR and elemental microanalysis permit scientists to establish the grafting and its stoichiometry. 1H and 13C SSNMR allows the structural determination of the hydrocarbon ligands coordination sphere. DNP SENS is an emerging powerful technique in solid characterization for the detection of poorly sensitive nuclei (15N, in our case). SiO2-700 is treated with about one equivalent of the metal precursor compared to the amount of surface silanol (0.30 mmol&#183;g-1) in pentane at room temperature. Then, volatiles are removed, and the powder samples are dried under dynamic high vacuum to afford the desired materials [(&#8801;Si-O-)Hf(&#951;2&#960;-MeNCH2)(&#951;1-NMe2)(&#951;1-HNMe2)]. After a thermal treatment under high vacuum, the grafted complex is converted into metal imido silica complex [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)]. [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] effectively promotes the metathesis of imines, using the combination of two imine substrates, N-(4-phenylbenzylidene)benzylamine, or N-(4-fluorobenzylidene)-4-fluoroaniline, with N-benzylidenetert-butylamine as substrates. A significantly lower conversion is observed with the blank runs; thus, the presence of the imido group in [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is correlated to the catalytic performance.

A new group IV metal catalyst for imine metathesis is prepared by grafting amine metal complex onto dehydroxylated silica. Surface metal fragments are characterized using FT-IR, elemental microanalysis, and solid-state NMR spectroscopy. Further dynamic nuclear polarization surface enhanced NMR spectroscopy experiments complement the determination of the coordination sphere.

利用表面有机金属化学方法，利用硅支持的催化剂进行Imine金属分析

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...

Metal Oxide Heterojunction for Photocatalytic Activities

There is a significant global demand for improvements in synthesis techniques and their optimal characteristics, especially for industrial-scale applications. Sol-gel-based solution combustion synthesis (SG-SCS) is a simple method to produce ordered porous materials. In this regard, Pearson&#39;s hard and soft acids and bases theory assists in selecting host-dopant reactivity to form a proper heterojunction.
The formation of a heterojunction also changes the essential properties of the materials, improving photocatalysis via charge transfer or synergistic activities. A calcination temperature of 500 &#176;C is ideal for this process based on the results of the stability assessment via a differential thermogravimetry ratio analysis (DTG).
The nanoscale dimensions of the nanoparticles (NPs) and nanocomposites (NCs) generated were validated using X-ray diffraction and high-resolution transmission electron microscopy (HRTEM). Furthermore, the scanning electron microscopy micrographs and BET analyses confirmed the porosity nature of the materials. HRTEM, X-ray photoelectron spectroscopy, and energy-dispersive X-ray investigations established the materials composition. The study found that NCs degraded the acid orange 8 (AO8) color more efficiently than bare ZnO.

The development of a heterojunction boosts the photocatalytic activities of solution combustion synthesis, which is a time-/energy-efficient process. Advanced analytical characterization techniques were used in this protocol to evaluate the materials&#39; characteristics, and nanocomposites demonstrated improved acid orange-8 dye degradation.

There is a significant global demand for improvements in synthesis techniques and their optimal characteristics, especially for industrial-scale ...

Synthesis of Single-Crystalline Core-Shell Metal-Organic Frameworks

Because of their designability and unprecedented synergistic effects, core-shell metal-organic frameworks (MOFs) have been actively examined recently. However, the synthesis of single-crystalline core-shell MOFs is very challenging, and thus a limited number of examples have been reported. Here, we suggest a method of synthesizing single-crystalline HKUST-1@MOF-5 core-shells, which is HKUST-1 at the center of MOF-5. Through the computational algorithm, this pair of MOFs was predicted to have the matched lattice parameters and chemical connection points at the interface. To construct the core-shell structure, we prepared the octahedral- and cubic-shaped HKUST-1 crystals as a core MOF, in which the (111) and (001) facets were mainly exposed, respectively. Via the sequential reaction, the MOF-5 shell was well-grown on the exposed surface, showing a seamless connect interface, which resulted in the successful synthesis of single-crystalline HKUST-1@MOF-5. Their pure phase formation was proved by optical microscopic images and powder X-ray diffraction (PXRD) patterns. This method presents the potential of and insights into the single-crystalline core-shell synthesis with different kinds of MOFs.

Here, we demonstrate a protocol for the two-step synthesis of single-crystalline core-shells using a non-isostructural metal-organic framework (MOF) pair, HKUST-1 and MOF-5, which have well-matched crystal lattices.

单晶核壳金属有机骨架的合成

Because of their designability and unprecedented synergistic effects, core-shell metal-organic frameworks (MOFs) have been actively examined recently. ...

三唑和四唑官能化 Zr-MOF 的合成和表征

Synthesis of Triazole and Tetrazole-Functionalized Zr-Based Metal-Organic Frameworks Through Post-Synthetic Ligand Exchange

Metal-organic frameworks (MOFs) are a class of porous materials that are formed through coordination bonds between metal clusters and organic ligands. Given their coordinative nature, the organic ligands and strut framework can be readily removed from the MOF and/or exchanged with other coordinative molecules. By introducing target ligands to MOF-containing solutions, functionalized MOFs can be obtained with new chemical tags via a process called post-synthetic ligand exchange (PSE). PSE is a straightforward and practical approach that enables the preparation of a wide range of MOFs with new chemical tags via a solid-solution equilibrium process. Furthermore, PSE can be performed at room temperature, allowing the incorporation of thermally unstable ligands into MOFs. In this work, we demonstrate the practicality of PSE by using heterocyclic triazole- and tetrazole-containing ligands to functionalize a Zr-based MOF (UiO-66; UiO = University of Oslo). After digestion, the functionalized MOFs are characterized via various techniques, including powder X-ray diffraction and nuclear magnetic resonance spectroscopy.

作者聚焦：金属有机框架功能化：合成后配体交换的进步、挑战和力量 

Post-synthetic ligand exchange (PSE) is a versatile and powerful tool for installing functional groups into metal-organic frameworks (MOFs). Exposing MOFs to solutions containing triazole- and tetrazole-functionalized ligands can incorporate these heterocyclic moieties into Zr-MOFs through PSE processes.

通过合成后配体交换合成三唑和四唑功能化Zr基金属有机骨架

Metal-organic frameworks (MOFs) are a class of porous materials that are formed through coordination bonds between metal clusters and organic ligands. ...

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

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