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期前体向纤维的扩散。最后, 金属氧化物涂层必须足够厚后, 扩散形成一个共形外层涂层, 并提供功能组和增加的表面粗糙度, MOF 到核18,20。虽然硅晶片用于监测限期增长和估计膜厚度, 聚合物自旋涂在 QCM 晶体可以作为一个更准确的手段来跟踪质量的吸收, 加上 FTIR 强度, 以估计薄膜厚度24。这些方法需要更多的时间和材料, 但可以解释聚合物薄膜的延迟或加速成核, 而不是根据硅的限期增长来估计。或者, TEM 横断面成像可以使用, 但这可能导致打破或压缩纤维涂层。
与常规 MOF 合成不同, 密被合成依赖于在纤维上锚定的金属源。在适当的条件下, 聚丙烯的 Al2O3涂层可以扩散到纤维中, 有助于在合成后锚定 MOF。然而, 如果金属氧化物是完全反应或如果限期扩散是有限的, 粘合力可能略有减少。一个例子, 这是目前的 MIL-96 增长使用500限期周期的 Al2O3, 如图 3a中的 SEM 图像所示。不完整的 mof 覆盖率和松散的碎片是在金属氧化物完全反应后, mof 层剥离出纤维的证据,图 4中的横断面图像证实了这一点。对于较厚的金属氧化物层, 这种剥离是没有观察到的。该材料的 MOF 负载受光纤中的金属源的限制。500周期样本上的 MOF 负载可能较低, 因为 Al 已完全耗尽。1000周期和2000周期样本的统一 MOF 粘附, 以及它们的横断面图像表明 Al2O3没有完全消耗。荷载受等表征方法酸有机连结剂的扩散速率限制为 al2o3 , 而较长的合成时间可能在较厚的铝2O3涂层上显示更高的 MOF 负载。
在 MIL-96 合成过程中, 分别用铝2o3粉末代替 al2o3的限期涂布, 并将其与在织物上的 MOF 合成分开。粉末没有反应。为了了解粉末与薄膜的反应性差异, 比较了介电常数。在薄膜上使用椭偏测量, 折射率为 1.63, 使介电常数为 2.66, 而 Al2O3的文献价值为 1025。这表明, 限期电影更有可能形成一个偶极, 使其更具反应性。考虑到低限期的温度, 这可能是由于羟基留在影片造成的缺陷。
2000循环样品有最高的赌注表面区域, 与更大的质量装载一致比在500个周期样品。MIL-96 的小赌注表面区域在被涂上500个限期周期的纤维反射小大量装载。合成 MIL-96 下注表面积的文献价值约为600米2/gMOF7、8.利用质量测量和表面积, 计算出的布尔特表面面积仅为文献价值的 1/10, 但随着较厚的限期基层的提高, 这一点得到了改进。这个估计可能人为地低由于被夸大的质量测量和不足的材料在赌注。
对于 UiO-66-NH2的合成, PA-6 纤维上的2光纤与纤维的主干相互作用, 改变结构性能, 同时在纤维20、26上形成硬外壳。由于低温限制了前驱体在纤维中的扩散, 沉积在50°c 的涂层导致了 MOF 合成后的 pealing 和附着力差。对于沉积在90摄氏度的金属氧化物, 由于沉积温度的升高, 这种剥离基本上被消除了, 尽管在薄膜中仍能观察到一些裂缝。在200°c, 扩散到纤维中消除剥离和开裂, 但以牺牲稀释可利用的2在纤维表面。沉积在50和90°c 的厚外壳仍然导致 mof 的增长, 但 mof 的增长非常有限, 在2沉积在200°c, 可能是因为最外层的外壳是如此之薄。这些样品的下注面积反映了2层的生长。UiO-66-NH2粉末表面区域是 1325 m2/gMOF与文献报告的价值一致。返回计算 mof 表面积从质量测量和样品表面区域显示 mof 粉末在织品有至多一半表面面积每克 MOF。在所有情况下, 虽然质量负荷可能是误导性的, 但较厚的外部限期与更大的下注表面积相关, 在 mof 增长后, 可能会导致更好的 mof 结晶性, 因为 mof 前体与纤维的交互作用较小。
未来的研究可能会检查原子层沉积的各种金属氧化物, 包括氧化锌, ZrO2和 HfO2, 这可能适用于替代 MOF 合成27。然而, 这些过程中的一些需要更高的沉积温度, 限制了可行的沉积织物。此外, MOFs 与更复杂的金属中心, 如锆6簇, 可能会更难以实现, 由于电影的流动性有限。然而, 在选择适当的限期前体和温度时, 薄膜的流动性可能在更高的 MOF 合成温度28中实现。

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 之前对织物的每克样品的测量或估计总表面积。在使用 mof 加载后加载、mof 本身或结构。对于限期涂布织物和 MIL-96 涂层织物, 表面面积计算从0.05 到0.3 的部分压力范围。对于含 UiO-66-NH2的样品, 由于存在微孔率, 计算出的表面面积为0.02 至0.08 的分压范围。所有样品的相关系数均为0.995 或更高。表 1中的每个示例都列出了适合的参数。在织物上的 mof 的特定表面积 (m2/gmof) 是使用在织物上的 mof 的实测质量和表面积计算的:
<img alt="Equation" src="/files/ftp_upload/57734/57734eq1v2.jpg">
涂布后1000周期的铝2O3的限期, 聚丙烯织物出现视觉不变, 虽然一些额外的刚度可以用手来感受。显示器硅片的椭偏椭圆显示1100±15Å2O3增长使用柯西模型。限期涂层导致1.16 毫克Al2O3/cm2的质量增益预测。这个过程是重复的500和2000周期 Al2O3, 导致600±15和2010±40Å在显示器硅片上。质量增加是0.65 毫克Al2O3/cm2预测和2.26 毫克Al2O3/cm2预测的500和2000循环样品分别。铝2O3(1000) 涂层聚丙烯的下注表面积为4.7 米2/克织物。
在 mof 综合之后, 由此得到的解决方案是明确的, 没有松散的 mof 粉末, 表明在纤维上的强 mof 和限期粘连。在洗涤和干燥之后, 样品大量增加在 500, 1000 和2000个周期样品分别是 40, 73 和77% 质量的最初的样品。铝2O3涂层织物样品平行曝光在没有 MOF 链接器或金属簇前体的情况下, 发现其固有的质量增益为 10-20%, 表明质量测量夸大了 mof 的加载。扫描电镜检查 (SEM) 显示了在所有纤维上的保形 MOF 晶体薄膜, 类似鹅卵石图案 (图 3b-3c)。当 Al2O3被减少到500个周期, 影片开始打破分开, 当 MOF 形成, 导致一个不完整的涂层 (图 3a)。无 Al2O3涂层的裸聚丙烯样品也暴露在 MIL-96 合成条件下 (图 3d), 但 XRD 显示纤维上没有可检测到的 MOF。这些样品的横断面图像显示, 500 周期 al2o3基层完全反应, 而铝2O3基层的一部分仍然为1000和2000周期样本 (图 4d– 4f)。原始 Al2O3的涂覆聚丙烯的剖面显示在图 4a-4c。在24小时反应时间, 大约80±20毫微米 Al2O3反应了或在酸性合成条件可能被蚀刻。电子色散光谱图像的剖面显示碳基聚丙烯芯和主要 Al2O3壳 (图 5)。与 MIL-96 模拟 PXRD 模式相匹配的 MOF 涂层织物的 X 射线衍射模式如图 6所示。MOF 增长后的实测表面积为19.9、2和500循环样本的6.0 米2/克mof + 结构、6.7 m2/克 mof + 结构和 1000 m2000/gmof + 结构。吸附和解吸等温线如图 7所示。
PA-6 纤维毡在300周期的2次沉积后出现轻微发黄, 但毡的刚度几乎不变。椭偏在显示器硅上显示175±15Å2用于50、90或200摄氏度的限期。0.17、0.20 和0.25 毫克TiO2/cm2预测面积 PA-6为50、90和200°c 样品的限期质量负荷。PA-6 织品的赌注表面区域涂有300个周期2在90°c 是 8.2 m2/g织品。
继溶剂热合成 MOF 合成后, XRD 模式显示 UiO-66-NH2存在于纤维上 (图 8)。50、90和200°c 样本的 MOF 质量增益为2.4、78和0%。在没有 MOF 金属簇或连接器前体的情况下,2涂层尼龙平行暴露在合成条件下, 其质量增益为10-20%。此外, 在 mof 合成过程中, 织物容易被撕裂, 酸性条件可能会蚀刻2膜, 导致 MOF 负载不确定。SEM 图象显示了 MOF 涂层在每个样品, 与片状涂层在50°c 样品, 密集的涂层在90°c 样品和稀疏涂层在200°c 样品 (图 9a-9c)。未涂覆的 PA-6 样品也暴露于 UiO-66-NH2合成条件, 导致了相对稀疏的 MOF 晶体涂层 (图 9d)。MOF 合成后的实测下注表面积分别为4.67、2和50 °c 样品的16.0 米2/克mof + 织物、19.8 米2/克 mof + 织物和90米200/克mof + 织物。吸附和解吸等温线如图 10所示。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/57734/57734fig1v2.jpg"> 图1。Al2O3的过程示意图:在第一步, 前体剂量, 三甲基铝前体反应与羟基终止表面。多余的前驱体然后从系统中清除, 导致一个统一的铝二甲基终止表面。在水剂量步期间水反应替换甲基小组, 导致新的羟基被终止的表面。在循环的最后一步, 多余的水从系统中清除。<a href="/files/ftp_upload/57734/57734fig1v2large.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/57734/57734fig2.jpg"> 图2。限期反应堆示意图:该系统是一个内置的, 热壁粘性流反应器与干氮气载体气体。前体线用热胶带包裹着, 而实际的沉积带则有网状试样船位于炉内。该系统在真空下运行1.8 乇。<a href="/files/ftp_upload/57734/57734fig2large.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/57734/57734fig3.jpg"> 图 3.SEM 图像的 PP 与(a) Al2O3(500)/毫米-96, (b) al2O3(1000)/毫米-96, (c) al2o3(2000)/毫米-96, 和(d)暴露于 MIL-96 后无限期涂层合成条件。<a href="/files/ftp_upload/57734/57734fig3large.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/57734/57734fig4.jpg"> 图 4.与(a) Al2O3 (500) 的 PP 截面的 SEM 图像, (b) al2O3 (1000), (c)铝2O3 (2000), (d) al2o 3 (500 )/毫米-96, (e)al2o3 (1000)/毫米-96, (f) al2O3 (2000)/毫米-96。<a href="/files/ftp_upload/57734/57734fig4large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 5" class="xfigimg" src="/files/ftp_upload/57734/57734fig5.jpg"> 图 5.PP/Al2o3 (500)/毫米-96 剖面的 EDS 图像显示了以铝2O3壳为主的碳基聚丙烯芯。<a href="/files/ftp_upload/57734/57734fig5large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 6" class="xfigimg" src="/files/ftp_upload/57734/57734fig6.jpg"> 图6。(黑色)模拟 PXRD MIL-96 (红色) XRD 模式的铝2o3涂层聚丙烯, (绿色) MIL-96 在铝3o3 (500) 涂覆聚丙烯, (但是) MIL-96 铝3O3 (1000)涂覆聚丙烯, (紫色) MIL-96 在 Al3O3 (2000) 涂覆聚丙烯和(灰色)裸 PP 暴露后 MIL-96 合成条件。<a href="/files/ftp_upload/57734/57734fig6large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 7" class="xfigimg" src="/files/ftp_upload/57734/57734fig7v2.jpg"> 图7。(灰色)N2 MIL-962o3环上的 MIL-96 吸附和解吸等温线在聚丙烯 (蓝色)上对铝1000o2循环上的500循环的吸附和解吸等温线(黑色)聚丙烯上铝2O3 MIL-96 的吸附和解吸等温线为2000循环。<a href="/files/ftp_upload/57734/57734fig7v2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 8" class="xfigimg" src="/files/ftp_upload/57734/57734fig8v2.jpg"> 图 8. (黑色)模拟 PXRD 模式的 UiO-66-NH2, (红色) XRD 模式的2涂覆 PA-6, (绿色) UiO-66-NH2在叔叔2(50 °c), 涂覆 PA-6 (蓝色) UiO-66-NH2在叔叔2(90 °c) 涂层PA-6, (紫色) UiO-66-NH2在2(200 °c) 涂覆的 PA-6 和(灰色) UiO-66-NH2在光秃的 PA-6。<a href="/files/ftp_upload/57734/57734fig8v2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 9" class="xfigimg" src="/files/ftp_upload/57734/57734fig9.jpg"> 图 9.扫描电镜图像的 PA-6/TiO2/UiO-66-NH2与限期沉积在 (a) 50 °c, (b) 90 °c 和 (C) 200 °c 和 (d) UiO-66-NH2在 PA-6 没有限期的基础大衣, 表明更高的限期温度导致将限期前体进一步扩散到纤维中, 改变了 MOF 的附着力。<a href="/files/ftp_upload/57734/57734fig9large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 10" class="xfigimg" src="/files/ftp_upload/57734/57734fig10v2.jpg"> 图 10.N2吸附和解吸等温线为 PA-6/TiO2/UiO-66-NH2与限期沉积在(灰色) 50 °c (蓝色) 90 °c 和(黑色) 200 °c。<a href="/files/ftp_upload/57734/57734fig10v2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always"><tbody>
<tr>
<td>样品</td>
			<td>C</td>
			<td>Y (g/毫摩尔)</td>
			<td>斜坡 (g/毫摩尔)</td>
			<td>质量管理 (毫摩尔/克)</td>
		</tr>
<tr>
<td>PP/Al2O3 (1000)</td>
			<td>6.61</td>
			<td>3.13</td>
			<td>17.59</td>
			<td>0.048</td>
		</tr>
<tr>
<td>PP/Al2O3 (500)/毫米-96</td>
			<td>7.01</td>
			<td>2.31</td>
			<td>13.588</td>
			<td>0.062</td>
		</tr>
<tr>
<td>PP/Al2O3 (1000)/毫米-96</td>
			<td>9.24</td>
			<td>1.58</td>
			<td>13.01</td>
			<td>0.069</td>
		</tr>
<tr>
<td>PP/Al2O3 (2000)/毫米-96</td>
			<td>4.06</td>
			<td>1.21</td>
			<td>3.69</td>
			<td>0。2</td>
		</tr>
<tr>
<td>尼龙/2 (90 °c)</td>
			<td>2.99</td>
			<td>3.97</td>
			<td>10.57</td>
			<td>0.072</td>
		</tr>
<tr>
<td>尼龙/2 (50 °c)/UiO-66-NH2
</td>
			<td>63.09</td>
			<td>0.096</td>
			<td>5.99</td>
			<td>0.16</td>
		</tr>
<tr>
<td>尼龙/2 (90 °c)/UiO-66-NH2
</td>
			<td>599</td>
			<td>0.0082</td>
			<td>4.92</td>
			<td>0。2</td>
		</tr>
<tr>
<td>尼龙/2 (200 °c)/UiO-66-NH2
</td>
			<td>32.43</td>
			<td>0.644</td>
			<td>20.24</td>
			<td>0.048</td>
		</tr>
</tbody></table>表1。每个示例的下注匹配参数列表。

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

Nanyang Technological University

Research

JoVE Journal

Chemistry

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

11.3K 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

Synthesis and Characterization of Functionalized Metal-organic Frameworks

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy.

Synthesis, activation, and characterization of intentionally designed metal-organic framework materials is challenging, especially when building blocks are incompatible or unwanted polymorphs are thermodynamically favored over desired forms. We describe how applications of solvent-assisted linker exchange, powder X-ray diffraction in capillaries and activation via supercritical CO2 drying, can address some of these challenges.

功能化的合成与表征金属 - 有机骨架

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

科研

化学

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

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

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 ...

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 ...

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

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 substrates outside vacuum at low temperature. The performance of photovoltaic devices featuring atmospherically fabricated ZnO/Cu2O heterojunction was dependent on the conditions of AP-SALD film deposition, namely, the substrate temperature and deposition time, as well as on the Cu2O substrate exposure to oxidizing agents prior to and during the ZnO deposition. Superficial Cu2O to CuO oxidation was identified as a limiting factor to heterojunction quality due to recombination at the ZnO/Cu2O interface. Optimization of AP-SALD conditions as well as keeping Cu2O away from air and moisture in order to minimize Cu2O surface oxidation led to improved device performance. A three-fold increase in the open-circuit voltage (up to 0.65 V) and a two-fold increase in the short-circuit current density produced solar cells with a record 2.2% power conversion efficiency (PCE). This PCE is the highest reported for a Zn1-xMgxO/Cu2O heterojunction formed outside vacuum, which highlights atmospheric pressure spatial ALD as a promising technique for inexpensive and scalable fabrication of Cu2O-based photovoltaics.

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

Here we present a protocol for synthesizing Zn1-xMgxO/Cu2O heterojunctions in open-air at low temperature via atmospheric pressure spatial atomic layer deposition (AP-SALD) of Zn1-xMgxO on cuprous oxide. Such high quality conformal metal oxides can be grown on a variety of substrates including plastics by this cheap and scalable method.

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

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide (CdSe@CdS) nanorod photocatalysts. Seeded rods are grown using a colloidal hot-injection method and then moved to an aqueous medium by ligand exchange. CdSe@CdS nanorods, an iridium precursor and other salts are mixed and illuminated. The deposition process is initiated by absorption of photons by the semiconductor particle, which results with formation of charge carriers that are used to promote redox reactions. To insure photochemical oxidative growth we used an electron scavenger. The photogenerated holes oxidize the iridium precursor, apparently in a mediated oxidative pathway. This results in the growth of high quality crystalline iridium oxide particles, ranging from 0.5 nm to about 3 nm, along the surface of the rod. Iridium oxide grown on CdSe@CdS heterostructures was studied by a variety of characterization methods, in order to evaluate its characteristics and quality. We explored means for control over particle size, crystallinity, deposition location on the CdS rod, and composition. Illumination time and excitation wavelength were found to be key parameters for such control. The influence of different growth conditions and the characterization of these heterostructures are described alongside a detailed description of their synthesis. Of significance is the fact that the addition of iridium oxide afforded the rods astounding photochemical stability under prolonged illumination in pure water (alleviating the requirement for hole scavengers).

A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

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

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 ...

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

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, their high cost production and/or incompatibility with microfabrication technologies, due to the use of pre-deposited catalyst-seeds and/or high processing temperatures exceeding 900 &#176;C, represent a drawback for a widespread use of these methods. Here, however, we report the synthesis of ZnO rods via a non-catalyzed vapor-solid mechanism enabled by using an aerosol-assisted chemical vapor deposition (CVD) method at 400 &#176;C with zinc chloride (ZnCl2) as the precursor and ethanol as the carrier solvent. This method provides both single-step formation of ZnO rods and the possibility of their direct integration with various substrate types, including silicon, silicon-based micromachined platforms, quartz, or high heat resistant polymers. This potentially facilitates the use of this method at a large-scale, due to its compatibility with state-of-the-art microfabrication processes for device manufacture. This report also describes the properties of these structures (e.g., morphology, crystalline phase, optical band gap, chemical composition, electrical resistance) and validates its gas sensing functionality towards carbon monoxide.

Columnar zinc oxide structures in the form of rods are synthesized via aerosol-assisted chemical vapor deposition without the use of pre-deposited catalyst-seed particles. This method is scalable and compatible with various substrates based on either silicon, quartz or polymers.

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

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity and convenient colorimetric readout. However, high densities of nanoparticles are typically needed for detection. The available synthesis-based enhancement protocols are either limited to gold and silver nanoparticles or rely on precise enzymatic control and optimization. Here, we present a protocol to enhance the colorimetric readout of gold, silver, silica, and iron oxide nanoprobes. It was observed that the colorimetric signal can be improved by up to a 10000-fold factor. The basis for such signal enhancement strategies is the chemical reduction of Au3+ to Au0. There are several chemical reactions that enable the reduction of Au3+ to Au0. In the protocol, Good&#39;s buffers and H2O2 are used and it is possible to favor the deposition of Au0 onto the surface of existing nanoprobes, in detriment of the formation of new gold nanoparticles. The protocol consists of the incubation of the microarray with a solution consisting of chloroauric acid and H2O2 in 2-(N-morpholino)ethanesulfonic acid pH 6 buffer following the nanoprobe-based detection assay. The enhancement solution can be applied to paper and glass-based sensors. Moreover, it can be used in commercially available immunoassays as demonstrated by the application of the method to a commercial allergen microarray. The signal development requires less than 5 min of incubation with the enhancement solution and the readout can be assessed by naked eye or low-end image acquisition devices such as a table-top scanner or a digital camera.

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

In this work, a protocol for signal enhancement of nanoprobe-based biosensing is presented. The protocol is based on the reduction of chloroauric acid onto the surface of existing nanoprobes that consist of gold, silver, silica or iron-oxide nanoparticles.

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

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. ...

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

Reactive sputtering is a versatile technique used to form compact films with excellent homogeneity. In addition, it allows easy control over deposition parameters such as gas flow rate that results in changes on composition and thus in the film required properties. In this report, reactive sputtering is used to deposit niobium oxide films. A niobium target is used as metal source and different oxygen flow rates to deposit niobium oxide films. The oxygen flow rate was changed from 3 to 10 sccm. The films deposited under low oxygen flow rates show higher electrical conductivity and provide better perovskite solar cells when used as electron transport layer.

Here, we present a protocol for niobium oxide films deposition by reactive sputtering with different oxygen flow rates for use as an electron transport layer in perovskite solar cells.

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 ...