这项研究是由国防威胁减少局 (DTRA BA08PRO015) 和美国海军研究局通过海军研究实验室基地基金发起的。这里所表达的观点是作者的意见, 并不代表美国海军、美国国防部或美国政府。

1. 微波启动
<ol><li>用10毫升的氢氧化铵 (28-30%) 与184毫升异丙醇在玻璃烧杯中混合, 用一个在 150 rpm 上的磁力搅拌棒来制备初始溶液。将6毫升的四乙基硅酸 (TEOS) 加入氢氧化铵溶液5。 注意: 氢氧化铵是一种碱溶液, 在接触眼睛和皮肤时会引起刺激和燃烧危险, 吸入或摄取时也会产生毒性。 注意: 四乙基硅酸是易燃和有毒的。</li>
	<li>要启动样品, 将织物的基质完全浸入 TEOS 混合物中, 取出玻璃、微波安全盘。 注意: 这里使用的布料是重量轻, 未漂白的棉花从一个特殊工艺品和织品零售商获得。所述工艺适用于范围广泛的织物, 限制其必须有可用的羟基或胺类5。这道菜的尺寸不重要, 只要布料能平躺在里面。<ol>
<li>微波饱和织物样品使用 1200 W 三十年代。 注意: 面料的样品和菜将是热的后续治疗。微波样品有足够的透气性, 避免吸入产生的蒸气。</li>
		<li>重复浸泡和微波处理共三个周期。 注: TEOS 混合物随着降水的发生而迅速变多云。立即使用。</li>
		<li>干燥处理的织物在100°c 30 分钟在烘干烤箱。一旦干燥, 织物可以储存在环境条件下。 注: 在这里使用的烤箱是一个重力烤箱, 但任何足够大小的烤箱适合干燥的材料。</li>
	</ol>
</li>
</ol>2. 镀膜用溶胶的制备
<ol><li>为制备溶胶, 在室温15、16、17、18、20 的塑料瓶中混合1.9 克 Pluronic P123、0.5 克均三甲苯和2.12 克 12-双 (trimethyoxysilyl) 乙烷 (BTE)。 ,21。 注意:12-双 (trimethyoxysilyl) 乙烷是易燃和有毒的。避免皮肤接触和吸入。均三甲苯是易燃和有毒的。避免皮肤接触和吸入。<ol>
<li>加入2.0 克甲醇和一个磁力搅拌棒。密封容器, 搅拌150转。 注意: 甲醇是易燃和有毒的, 可能会带来其他健康危害。避免皮肤接触和吸入。 注: 在这种沉积物的变化中, 乙醇可以代替本议定书的甲醇。在讨论中提供了其他信息。</li>
		<li>当搅拌溶液出现均匀时, 加入6.07 克的0.1 米 HNO3滴状。 注意: 硝酸是腐蚀性的, 会引起皮肤、眼睛和呼吸系统的刺激。避免皮肤接触和吸入。</li>
		<li>继续搅拌6小时的混合物。 注: 在这一点上, 混合物在一夜之间是稳定的, 但只有在没有蒸发的情况下。如果甲醇在贮存过程中蒸发, 会发生对溶胶凝胶的改变。</li>
	</ol>
</li>
</ol>3. 浸渍涂布
<ol><li>以150毫米/分钟的速率将 TEOS 处理过的织物浸入所制备的溶胶中。 注: 更快的速度高达270毫米/分钟可以使用, 并没有负面影响的结果材料。在这里, 任何设备达到倾角和绘制率之间的150和270毫米/分钟是合适的。<ol>
<li>将样品转移到60摄氏度烤箱中晾干24小时。</li>
		<li>继续固化在80摄氏度额外的24小时。 注意: 在这一点上可以接受120摄氏度以上的固化温度。固化后, 织物可以储存在室温下, 允许以后提取。</li>
	</ol>
</li>
	<li>将织物样品浸泡在超过65摄氏度的乙醇中, 以提取表面活性剂。 注意: 乙醇是易燃的。 注: 确保容器能耐受必要的温度。<ol>
<li>用额外的乙醇冲洗织物。</li>
	</ol>
</li>
	<li>在 60-65 摄氏度处过夜。一旦干燥, 织物可以储存在环境条件下。</li>
</ol>4. 涂层织物的卟啉功能化
<ol><li>为了 functionalize 主要胺基团的吸附剂材料, 在0.5% 体积/体积15,16的情况下, 在甲苯中制备 3-aminopropyltriethoxy 硅烷 (APS) 溶液。 注意: 3-Aminopropyltriethoxy 硅烷具有腐蚀性和毒性。避免皮肤接触和吸入。甲苯是易燃、有毒和已知的致癌物质。避免皮肤接触和吸入。<ol>
<li>浸泡在溶液中的织物和孵化1小时, 覆盖。</li>
		<li>用甲苯彻底冲洗样品。</li>
		<li>干燥织物样品隔夜在100°c。</li>
	</ol>
</li>
	<li>为制备次卟啉 IX 24 双乙二醇 (迪克斯) 的铜络合物, 在2毫升二甲基亚砜22中溶解20毫克卟啉。 注意: 卟啉可能存在健康危害;遵循建议的预防程序。<ol>
<li>将卟啉溶液添加到100毫升水中, 用12.8 毫克的氯化铜在圆底烧瓶中加入。 注意: 氯化铜具有腐蚀性、毒性, 并对水生环境构成危害。避免皮肤接触和吸入。</li>
		<li>一夜之间回流解决方案。</li>
		<li>使用旋转蒸发将总试样体积减少到5毫升。 注: 卟啉可以用更大的数量制备, 供以后使用。制备的卟啉应在室温下储存在黑暗中。</li>
	</ol>
</li>
	<li>将所制备的卟啉溶液添加到15毫升的0.1 米 2-(n-吗啉代) ethansulfonic 酸 (MES) 缓冲 pH 值5.5。<ol>
<li>在溶液中加入5毫克 1-乙基 3-(3-dimethylaminopropyl) carbodiimide (EDC), 立即将织物样品浸泡。</li>
		<li>覆盖样品和孵化过夜。</li>
		<li>用清水冲洗样品。</li>
		<li>干燥织物样品隔夜在100°c。</li>
	</ol>
</li>
</ol>5. 织物的特性
<ol><li>根据制造商的协议, 使用任何商业上可用的氮气吸附特性系统来表征织物样品的孔隙度。 注: 在这里, 氮气吸附分析完成 77 k 根据所使用的系统, 可能需要权衡样品或德加在≥65°c 之前分析。<ol>
<li>使用布鲁诺尔 (下注) 法测定表面积。</li>
		<li>使用巴雷特-乔伊纳-Halenda (BJH) 法测定等温线吸附支路的孔隙大小。</li>
		<li>用单点法测定相对压力下的孔隙体积 (p/p0) 0.97。</li>
	</ol>
</li>
	<li>通过对 2-氯乙基硫化物 (塞斯·弗林特曼) 通过织物样品的渗透特性, 遵循试验操作程序 (顶部) 8-2-501 的指导, 通过化学试剂或模拟剂 (色板试验) 对材料进行渗透试验 (样本测试)23 ,24。 注意: 2-氯乙基乙硫醚易燃、耐腐蚀、有毒, 并对健康构成危害。避免皮肤接触和吸入。 注: 在本研究中, 采用内部探头驱动加热器, 控制了自定义环境中的温度。使用探头驱动的质量流量控制器解决了进入本会议厅的潮湿空气比。不锈钢气溶胶-蒸气-液体评估组 (AVLAG) 单元与 O 形环密封水平保持样品。扩散渗透试验使用氮气流。该色板上方的顶空, 其中的目标放置, 是停滞的, 没有压力差在色板之上和下方。样品在两个实心支持盘之间支持与被排列的 0.64 cm2圆的开头。该组件放置在 AVLAG 单元格中, 湿度为2小时平衡, 使用重复分配器将目标作为液滴引入。一个专用的氢裂允许连续监测目标浓度。</li>
	<li>遵循 ASTM E96 提供的指导, 水蒸气运输: 直立开杯法表征水汽输送通过织物样品4,24,25。<ol>
<li>修改孵化器以提供25摄氏度的此分析的外壳。</li>
		<li>用16.9 毫升去离子水填充闪烁瓶 (20 毫升)。把样品材料密封在这个瓶子上, 然后称量瓶子。使用干燥剂在孵化器中驱动湿度差异, 并使干氮气流保持在样品表面 (0.25 升/分钟) 的流动。</li>
		<li>用分析天平测量30到45分钟的样品盖瓶的重量。</li>
	</ol>
</li>
</ol>

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作者声明他们没有竞争的财政利益。

在这里, 我们已经表明, 微波引发的沉积 TEOS 可用于制备织物, 随后沉积的多孔 organosilicate 吸附剂。方法导致布料的装载与 1.12 g 吸附剂每 m2织品表面。用氮吸附法对涂层织物进行分析, 表明在充分处理的材料与所启动的织物之间存在显著差异的多孔涂层的沉积。然而, 表面面积比作为一个整体合成的类似组合材料所观察到的要少。单独的吸附剂降低了85% 塞斯·弗林特曼运输的速度。加入卟啉功能化对支持的吸附剂进一步减少运输 (93% 总减少)。卟啉官能化处理织物的初步突破发生在2分钟;初步突破棉织物为0.6 分钟。这种化学渗透的减少对织物的水汽输送影响不大。
所沉积的吸附剂不是连续薄膜。该方法产生的涂层, 更紧密的保形, 以纱线的面料。因此, 减少渗透是有限的织物编织。在这里, 用轻质棉布作为支撑材料。微波启动适用于其它提供胺类或羟基的织物进行改性。更密的梭织织物, 如美国陆军战斗制服使用的尼龙和棉混纺 (针灸), 将产生更大的减少目标运输简单的基础上的空隙空间内的编织。作为遮蔽材料使用的密被编织的织物将提供类似的优势。忆及吸附剂的处理不限于织物的表面, 也可望提供某种深度的羊毛或重针织织物的材料, 从而产生更多的渗透减少。这一概念也适用于空气过滤用的三维折叠材料。
此处概述的治疗不限于在传统织物上使用。它提供了可能修改的纸张, 分层和褶积材料更典型地应用于过滤方法和非织造纺织品。在某些情况下, 此处描述的条件可能需要温和, 以保持支持材料的完整性。减少碱的浓度 (氢氧化铵) 可能是必要的, 如聚乙烯织物的情况。缩短微波周期的时间可能是必要的, 以避免灼热 (纸张材料)。一些合成纤维, 例如聚丙烯, 需要减少使用的干燥温度。应避免对溶胶时效温度和持续时间的变化, 因为这些条件对产生的吸附剂的形貌有重大影响。
在浸渍涂层溶胶中, 乙醇可以取代甲醇。这在放大合成和使用更大体积的溶胶时是鼓励的, 因为乙醇对健康危害较小。溶胶可以相当稀释与酒精,例如, 4 到12克乙醇, 而不是2克甲醇), 以准备一个更大的体积的混合物, 没有比例增加 BTE, Pluronic P123, 均三甲苯和酸。相对量的反应物和溶剂也可以乘以以制备溶胶, 以生成更大的涂层材料样品。溶胶的稀释程度或浓度可能会影响到特定织物上的吸附剂材料的大量加载。多循环的浸入溶胶混合物也应导致总负荷的变化。
目前正在对其他支持材料的沉积方法进行优化。改性的针刺尼龙和棉混纺织物是特别感兴趣的日常磨损解决方案提供基线化学保护, 因为是泽西针织材料。其他吸附剂材料的沉积也正在探索中。例如, 为捕获杀虫剂目标而开发的苯桥吸剂, 使用与此处描述的17、20、27和催化不同的溶胶制备方法。卟 啉。最后, 对织物支持材料进行了对气溶胶、液体和蒸气目标的评估。

目前, 美国国防部 (DoD) 使用的化学防护服, 要么提供一个完整的屏障, 一级的化学防护服, 例如, 或使用多层织物保护, 如在联合服务轻量级综合套装技术 (JSLIST)。全垒服给用户造成了很大的负担。由于没有水蒸气通过材料输送, 热调节受到阻碍。因此, 使用期限 (任务长度) 受到限制;该服装适用于范围有限的方案。另一方面, JSLIST 在壳织物和舒适层之间使用一层碳吸附剂。由此造成的用户负担减少, 但没有消除, 并减少了防护能力相比, 屏障西装。除热负荷外, JSLIST 套装仅适用于连续使用24小时。这两种技术都不适合在长期的日常服装中提供基线保护能力。基线保护将用于低危险环境, 适用于 MOPP 0 至2的条件 (MOPP 以任务为导向的保护姿态) 和其他低风险条件。除了国防部的关注之外, 基线保护对于那些可能进入受污染环境但没有事先警告的急救人员是有用的。
寻求改进国防部防护服装的研究正在进行中, 连续1,2,3,4。以前的努力确定了微波启动过程的潜力, 以沉积 heptadecafluoro-11, 22-tetrahydrodecyl) 三氯织物, 以产生憎油行为5。目的是生产一种可以增强 JSLIST 服装外壳层的织物。虽然这种 oleophobicity 可以提高层状服装的耐化学性, 但它不会解决该套装所施加的热量负担。还有其他正在进行的工作侧重于吸附剂和催化剂的捕获和/或分解化学威胁6,7,8,9,10, 11,12,13,14。最近描述的方法使用多孔 organosilicate 吸附剂结合卟啉捕获和降解光气, 并使用类似的材料捕获有毒的工业化合物 (抽搐) 以及杀虫剂模拟剂和 nitroenergetics15 ,16,17,18,19,20。这些粉状材料虽然前景看好, 但并不直接适用于服装技术。
Organosilicate 系统广泛应用于浸渍和自旋涂层方法, 通常在玻璃和硅片上。上述微波沉积技术为这些材料在织物上的应用提供了一种机制。在这里, 我们使用所描述的过程与 tetraethylorthosilicate 结合, 以准备织物。然后通过浸渍涂层方法对其进行多孔吸附剂处理。形态学表征表明了多孔吸附剂在织物上的存在。对 2-氯乙基硫醚 (塞斯·弗林特曼) 在织物上的渗透和不经过这种处理, 对靶材的运输有很大的影响。

<table border="0" cellpadding="0" cellspacing="0" width="1345">
	<tbody>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">unbleached 100% cotton fabric</td>
			<td style="width:239px;">JOANN Stores</td>
			<td style="width:275px;">N/A</td>
			<td style="width:471px;">Protocol is suitable for use on a variety of fabrics</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">ammonium hydroxide</td>
			<td style="width:239px;">Aldrich</td>
			<td style="width:275px;">32,014-5</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">tetraethyl orthosilicate</td>
			<td style="width:239px;">Aldrich</td>
			<td style="width:275px;">13,190-3</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Pluronic P123</td>
			<td style="width:239px;">Aldrich</td>
			<td style="width:275px;">435465</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">mesitylene</td>
			<td style="width:239px;">Sigma-Aldrich</td>
			<td style="width:275px;">M7200</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">1,2-bis(trimethoxysilyl)ethane</td>
			<td style="width:239px;">Aldrich</td>
			<td style="width:275px;">447242</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">methanol</td>
			<td style="width:239px;">Fisher Chemical</td>
			<td style="width:275px;">A454SK-4</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">nitric acid</td>
			<td style="width:239px;">Sigma-Aldrich</td>
			<td style="width:275px;">438073</td>
			<td style="width:471px;">Prepare 0.1 M aqueous solution</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">3-aminopropyltriethoxysilane</td>
			<td style="width:239px;">Gelest</td>
			<td style="width:275px;">SIA0603.4</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">toluene</td>
			<td style="width:239px;">Sigma-Aldrich</td>
			<td style="width:275px;">650579</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Deuteroporphyrin IX bis ethylene glycol</td>
			<td style="width:239px;">Frontier Scientific</td>
			<td style="width:275px;">D630-9</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">dimethyl sulfoxide</td>
			<td style="width:239px;">Sigma-Aldrich</td>
			<td style="width:275px;">276855</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">copper chloride</td>
			<td style="width:239px;">Sigma-Aldrich</td>
			<td style="width:275px;">256528</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">2-(N-morpholino)ethansulfonic acid</td>
			<td style="width:239px;">Sigma-Aldrich</td>
			<td style="width:275px;">M3671</td>
			<td style="width:471px;">Prepare 0.1M buffer at pH 5.5</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">1-ethyl-3-(3-dimethylaminopropyl)carbodiimide</td>
			<td style="width:239px;">Sigma-Aldrich</td>
			<td style="width:275px;">E6383</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">ethyl alcohol</td>
			<td style="width:239px;">Warner-Graham</td>
			<td style="width:275px;">64-17-5</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Drierite</td>
			<td style="width:239px;">Sigma-Aldrich</td>
			<td style="width:275px;">737828</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Microwave</td>
			<td style="width:239px;">Daewoo</td>
			<td style="width:275px;">KOR-630A</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Nitrogen adsorption instrument</td>
			<td>Micromeritics</td>
			<td style="width:275px;">&#160;TriStar II Plus&#160;</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Environmental chamber</td>
			<td style="width:239px;">custom part</td>
			<td style="width:275px;">N/A</td>
			<td style="width:471px;">Here, a modified Thermolyne incubator, Compact Series 5000 was used</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Flame ionization detector (FID)</td>
			<td style="width:239px;">SRI Instruments</td>
			<td style="width:275px;">8690-0010</td>
			<td style="width:471px;">Model 110</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Humidity probe</td>
			<td style="width:239px;">Vaisala</td>
			<td>HMT3303E0A193BCAC100A0CCABEA1</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">AVLAG Cell</td>
			<td style="width:239px;">custom part</td>
			<td style="width:275px;">N/A</td>
			<td style="width:471px;">AERO-Space Tooling and Machining, P/N RS0010 Permeation cell</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Computer controlled heater</td>
			<td style="width:239px;">World Precision Instruments</td>
			<td>AIRTHERMY-ATX</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Mass flow controller</td>
			<td style="width:239px;">MKS Instruments</td>
			<td style="width:275px;">1179A01312CS</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Dipper mechanism Type D1L</td>
			<td style="width:239px;">NIMA Technology Ltd</td>
			<td style="width:275px;">D1L</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Gravity oven</td>
			<td style="width:239px;">Fisher Scientific</td>
			<td style="width:275px;">15-103-0520</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Stirring hotplate</td>
			<td style="width:239px;">Fisherbrand</td>
			<td style="width:275px;">S28482</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Octagon spinbar, magnetic stirring bar</td>
			<td style="width:239px;">Fisherbrand</td>
			<td style="width:275px;">14-513-82</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">PSI-Plot version 9.5</td>
			<td style="width:239px;">Poly Software International, Inc</td>
			<td style="width:275px;">N/A</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:363px;">Microsoft Office Professional Plus - Excel 2013 32-bit</td>
			<td style="width:239px;">Microsoft</td>
			<td style="width:275px;">N/A</td>
			<td style="width:471px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:363px;">MicroActive TriStar II Plus Software</td>
			<td>Micromeritics</td>
			<td style="width:275px;">packaged with the TriStar II nitrogen adsorption instrument</td>
			<td style="width:471px;"></td>
		</tr>
	</tbody>
</table>

deposition of porous sorbents on fabric supports

烷的微波沉积技术, 以前被描述为生产的憎油织物, 是为了提供一种织物支持材料, 可随后处理的浸渍涂层。采用溶胶制备的浸渍涂层在织物上提供了受支持的多孔层。在这种情况下, 多孔层是一种卟啉功能性吸附剂系统, 其基础是一种粉末材料, 此前已经证明了对光气的捕获和转化。在10毫克/克的负载水平上, 有代表性的涂层适用于棉织物。这种涂层对通过织物 (93% 的支撑织物速率) 的水汽输送影响极小, 同时通过材料 (7% 的支持织物率) 显著减少了 2-氯乙基硫醚 (塞斯·弗林特曼) 的运输。所述方法适用于其他提供胺类和羟基的织物进行改性, 可与其他溶胶制剂结合使用, 以产生不同的功能。

采用氮气吸附法对浸渍涂层工艺后的织物进行了评价。如图 1所示, 为多孔涂层获得了预期的等温线。这与未处理的织品和为微波开始的织品注意的行为对比。仅对织物和微波处理后的织物进行了可忽略的氮吸附。没有确定孔隙大小。多孔涂层产生的表面积为3.39 米2/克, 孔隙体积0.013 厘米3/克。该仪器报告的 BJH 吸附孔径为76Å, 但在孔隙大小分布上没有明显的特征。图 2提供了涂层过程中每个阶段的织物图像。根据样品在沉积前的差重和最终干燥后的重量, 从原来的织物中增重 1%, 在棉花支护上沉积的吸附剂的平均质量确定为0.01 克/克。如果测量的表面积和孔隙体积被改正, 只占材料的吸附剂质量分量, 则吸附剂的表面积为339米2/克, 孔隙体积1.3 厘米3/克。为比较, 当这个吸附剂被合成作为一个整体在一个闭合的反应器, 氮气压表明了赌注表面面积 1143年 m2/g 与孔容量 1.01 m2/g 和孔直径76Å26。观察了这种材料具有显著滞后的 IV. 型等温线 (图 3)。在培养皿中固化镀膜溶胶, 并根据涂层织物样品的处理工艺, 制备了厚薄膜试样。氮气压表示一个赌注表面面积 968 m2/g 与孔容量 0.78 cm3/g 和孔直径39Å为这材料 (图 3)。
用两个腔室细胞4、24、25对所处理织物的水蒸气传输 (WVT) 速率进行了评估。该评价使用了一个圆形织物样品, 总暴露面积为1.65 厘米2。如图 4所示, 与未经处理的棉花相比, 这种织物的微波起动引起的水汽输送略有减少。在吸附剂沉积或功能化与卟啉之后, 没有注意到水蒸气输送的额外变化。棉织物的 WVT 率定为121克/小时/米2。在微波启动时, WVT 率降低到112克/小时/米2 。WVT 率为113克/小时/米2被确定为完全卟啉功能治疗。
2-氯乙基硫醚 (塞斯·弗林特曼) 被用作模拟, 以确定是否沉积的多孔处理导致化学运输性能的变化的织物。塞斯·弗林特曼通常被用作模拟硫磺芥末, 一种化学战剂。这里使用的吸附剂材料由乙烷桥接组组成, 并具有铜次卟啉 IX 24 双乙二醇 (CuDIX) 卟的功能。这反映了以前用来捕获光气15,16的吸附剂系统的特性。化学气相输送是用气溶胶-蒸气-液体评估组 (AVLAG) 细胞23,24确定的。该方法在受控温度 (40 °c) 和相对湿度 (50%) 的情况下, 利用连续流进行火焰电离检测 (FID), 使总暴露面积为0.64 厘米2。图 5提供了与时间相关的 FID 响应。当对纯棉织物进行评估时, 注意到67克/小时/米2的峰值率没有保留目标 (214 µg)。多孔处理的结果大大降低了运输高峰期 (9.6 克/小时/米2) 和目标通过织物的总运输。最初应用的214µg 塞斯·弗林特曼中只有78µg 在83小时内恢复。卟啉功能化多孔处理进一步降低了峰值的运输到4.5 克/小时/米2 , 总运输39µg 塞斯·弗林特曼超过 83 h 实验。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/57331/57331fig1.jpg"> 图 1: 织物的形态表征.这里显示的是代表性的氮吸附等温线 (a) 和孔隙大小分布 (B) 为典型的织物色板 (红色), 一个类似的样本后, 微波启动过程 (蓝色), 织物后应用的吸附剂 (绿色), 和织物以下应用的全吸附剂系统 (黑色)。<a href="/files/ftp_upload/57331/57331fig1large.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/57331/57331fig2.jpg"> 图 2: 织物的照片.这里的照片显示了微波启动, 吸附剂涂层材料 (A), CuDIX 卟啉单独在棉花 (B), 和一个完整的卟啉功能涂层的棉花 (C)。处理过的色板覆盖在未经治疗的棉织物上。<a href="/files/ftp_upload/57331/57331fig2large.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/57331/57331fig3.jpg"> 图 3: 不受支持的吸附剂的形态学表征.这里显示的是代表性的氮气吸附等温线 (A) 和孔隙大小分布 (B) 的吸附剂当合成为一个整体 (黑色), 当合成为厚膜 (红色)26。<a href="/files/ftp_upload/57331/57331fig3large.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/57331/57331fig4.jpg"> 图 4: 水蒸气渗透.本文给出了全 CuDIX 卟啉功能化吸附剂 (黑色) 的水蒸气渗透分析结果。棉织物仅 (红色) 和棉织物以仅吸附剂组分 (蓝色) 被提供比较。<a href="/files/ftp_upload/57331/57331fig4large.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/57331/57331fig5.jpg"> 图 5: 塞斯·弗林特曼的渗透.本文介绍了塞斯·弗林特曼在棉织物上的完全卟啉功能性吸附剂涂层 (黑色) 的渗透。织物仅 (红色) 和织品与仅吸附剂组分 (蓝色) 被提供比较。该插图为三材料的初始突破期提供了一个放大的视图。<a href="/files/ftp_upload/57331/57331fig5large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

Watch this Scientific Journal Video about Deposition of Porous Sorbents on Fabric Supports at JoVE.com

Deposition of Porous Sorbents on Fabric Supports

本报告详细介绍了微波启动的方法, 以沉积卟啉功能性多孔 organosilicate 吸附剂在棉织物, 并表明减少 2-氯乙基硫醚 (塞斯·弗林特曼) 运输通过织物由此产生的治疗。

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 ...

deposition-of-porous-sorbents-on-fabric-supports

Research

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Chemistry

6.5K 次观看.  Naval Research Laboratory. 本报告详细介绍了微波启动的方法, 以沉积卟啉功能性多孔 organosilicate 吸附剂在棉织物, 并表明减少 2-氯乙基硫醚 (塞斯·弗林特曼) 运输通过织物由此产生的治疗。

视频: Deposition of Porous Sorbents on Fabric Supports

Supercritical Nitrogen Processing for the Purification of Reactive Porous Materials

Supercritical fluid extraction and drying methods are well established in numerous applications for the synthesis and processing of porous materials. Herein, nitrogen is presented as a novel supercritical drying fluid for specialized applications such as in the processing of reactive porous materials, where carbon dioxide and other fluids are not appropriate due to their higher chemical reactivity. Nitrogen exhibits similar physical properties in the near-critical region of its phase diagram as compared to carbon dioxide: a widely tunable density up to ~1 g ml-1, modest critical pressure (3.4 MPa), and small molecular diameter of ~3.6 &#197;. The key to achieving a high solvation power of nitrogen is to apply a processing temperature in the range of 80-150 K, where the density of nitrogen is an order of magnitude higher than at similar pressures near ambient temperature. The detailed solvation properties of nitrogen, and especially its selectivity, across a wide range of common target species of extraction still require further investigation. Herein we describe a protocol for the supercritical nitrogen processing of porous magnesium borohydride.

Nitrogen is an effective supercritical fluid for extraction or drying processes due to its small molecular size, high density in the near-liquid supercritical regime, and chemical inertness. We present a supercritical nitrogen drying protocol for the purification treatment 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. ...

科研

化学

Chemical Vapor Deposition of an Organic Magnet, Vanadium Tetracyanoethylene

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in traditional materials, including low cost and mechanical flexibility. In a similar vein, it would be advantageous to expand the use of organics into high frequency electronics and spin-based electronics. This work presents a synthetic process for the growth of thin films of the room temperature organic ferrimagnet, vanadium tetracyanoethylene (V[TCNE]x, x~2) by low temperature chemical vapor deposition (CVD). The thin film is grown at &#60;60 &#176;C, and can accommodate a wide variety of substrates including, but not limited to, silicon, glass, Teflon and flexible substrates. The conformal deposition is conducive to pre-patterned and three-dimensional structures as well. Additionally this technique can yield films with thicknesses ranging from 30 nm to several microns. Recent progress in optimization of film growth creates a film whose qualities, such as higher Curie temperature (600 K), improved magnetic homogeneity, and narrow ferromagnetic resonance line-width (1.5 G) show promise for a variety of applications in spintronics and microwave electronics.

We present the synthesis of the organic-based ferrimagnet vanadium tetracyanoethylene (V[TCNE]x, x~2) via low temperature chemical vapor deposition (CVD). This optimized recipe yields an increase in Curie temperature from 400 K to over 600 K and a dramatic improvement in magnetic resonance properties.

化学气相沉积的有机磁体，钒四氰

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in ...

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 ...

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr2+ act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air.

化学溶液沉积在硅外延大孔石英薄膜的制备

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

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 ...

Accessing Valuable Ligand Supports for Transition Metals: A Modified, Intermediate Scale Preparation of 1,2,3,4,5-Pentamethylcyclopentadiene

A reliable, intermediate scale preparation of 1,2,3,4,5-pentamethylcyclopentadiene (Cp*H) is presented, based on modifications of existing protocols that derive from initial 2-bromo-2-butene lithiation followed by acid mediated dienol cyclization. The revised synthesis and purification of the ligand avoids the use of mechanical stirring while still permitting access to significant quantities (39 g) of Cp*H in good yield (58%). The procedure offers other additional benefits, including a more controlled quench of excess lithium during the production of the intermediate heptadienols and a simplified isolation of Cp*H of sufficient purity for metallation with transition metals. The ligand was subsequently used to synthesize [Cp*MCl2]2 complexes of both iridium and ruthenium to demonstrate the utility of the Cp*H prepared and purified by our method. The procedure outlined herein affords substantial quantities of a ubiquitous ancillary ligand support used in organometallic chemistry while minimizing the need for specialized laboratory equipment, thus providing a simpler and more accessible entry point into the chemistry of 1,2,3,4,5-pentamethylcyclopentadiene.

Reliable, intermediate scale preparation of 1,2,3,4,5-pentamethylcyclopentadiene (Cp*H) is presented. The revised protocol for the synthesis and purification of the ligand minimizes the need for specialized laboratory equipment while simplifying reaction workups and product purification. Use of Cp*H in the synthesis of [Cp*MCl2]2 complexes (M = Ru, Ir) is also described.

访问有价值的配体为支持过渡金属:1,2,3,4,5-五甲基环戊二烯的一种改进，中级规模制备

A reliable, intermediate scale preparation of 1,2,3,4,5-pentamethylcyclopentadiene (Cp*H) is presented, based on modifications of existing protocols that ...

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, ...

Nanothermite with Meringue-like Morphology: From Loose Powder to Ultra-porous Objects

The goal of the protocol described in this article is to prepare aluminothermic compositions (nanothermites) in the form of porous, monolithic objects. Nanothermites are combustible materials made up of inorganic fuel and an oxidizer. In nanothermite foams, aluminum is the fuel and aluminum phosphate and tungsten trioxide are the oxidizing moieties. The highest flame propagation velocities (FPVs) in nanothermites are observed in loose powders and FPVs are strongly decreased by pelletizing nanothermite powders. From a physical standpoint, nanothermite loose powders are metastable systems. Their properties can be altered by unintentional compaction induced by shocks or vibrations or by the segregation of particles over time by settling phenomena, which originates from the density differences of their components. Moving from a powder to an object is the challenge that must be overcome to integrate nanothermites in pyrotechnic systems. Nanothermite objects must have both a high open porosity and good mechanical strength. Nanothermite foams meet both of these criteria, and they are prepared by dispersing a nano-sized aluminothermic mixture (Al/WO3) in orthophosphoric acid. The reaction of aluminum with the acid solution gives the AlPO4 &#34;cement&#34; in which Al and WO3 nanoparticles are embedded. In nanothermite foams, aluminum phosphate plays the dual role of binder and oxidizer. This method can be used with tungsten trioxide, which is not altered by the preparation process. It could probably be extended to some oxides, which are commonly used for the preparation of high performance nanothermites. The WO3-based nanothermite foams described in this article are particularly insensitive to impact and friction, which makes them far safer to handle than loose Al/WO3 powder. The fast combustion of these materials has interesting applications in pyrotechnic igniters. Their use in detonators as primers would require the incorporation of a secondary explosive in their composition.

This manuscript describes the synthesis of combustible aluminophosphate matrices by the reaction of orthophosphoric acid (H3PO4) with aluminum nanopowder. When this reaction is carried out with excess aluminum in the presence of tungsten trioxide nanopowder, it leads to a solid, porous nanothermite foam.

Nanothermite 与蛋白酥样形态学: 从松散的粉末到超多孔物体

The goal of the protocol described in this article is to prepare aluminothermic compositions (nanothermites) in the form of porous, monolithic objects. ...

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. Conductive polymers, poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-propylenedioxythiophene) (PProDOT), and a semiconducting polymer, poly(thieno[3,2-b]thiophene) (PTT), were deposited on unconventional highly-disordered and textured substrates with high surface areas, such as paper, towels and fabrics. This reported deposition chamber is an improvement of previous vapor reactors because our system can accommodate both volatile and nonvolatile monomers, such as 3,4-propylenedioxythiophene and thieno[3,2-b]thiophene. Utilization of both solid and liquid oxidants are also demonstrated. One limitation of this method is that it lacks sophisticated in situ thickness monitors. Polymer coatings made by the commonly used solution-based coating methods, such as spin-coating and surface grafting, are often not uniform or susceptible to mechanical degradation. This reported vapor phase deposition method overcomes those drawbacks and is a strong alternative to common solution-based coating methods. Notably, polymer films coated by the reported method are uniform and conformal on rough surfaces, even at a micrometer scale. This feature allows for future application of vapor deposited polymers in electronics devices on flexible and highly textured substrates.

This paper presents a protocol for reactive vapor deposition of poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene), and poly(thieno[3,2-b]thiophene) films on glass slides and rough substrates, such as textiles and paper.

任意基底上共轭聚合物薄膜的反应气相沉积

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. ...

The Effect of Ultraviolet Radiation on the Chemical Bath Deposition of Bis(thiourea) Cadmium Chloride Crystals and the Subsequent CdS Obtention

In this work, the effects on the preparation of bis(thiourea) cadmium chloride crystals when illuminated with ultraviolet (UV) light at a wavelength of 367 nm using the chemical bath deposition technique are studied comparatively. Two experiments are performed to make a comparison: one without UV light and the other with the aid of UV light. Both experiments are performed under equal conditions, at a temperature of 343 K and with a pH of 3.2. The precursors used are cadmium chloride (CdCl2) and thiourea [CS(NH2)2], which are dissolved in 50 mL of deionized water with an acidic pH. In this experiment, the interaction of electromagnetic radiation is sought at the moment the chemical reaction is carried out. The results demonstrate the existence of an interaction between the crystals and the UV light; the UV light assistance causes crystal growths in an acicular shape. Also, the final product obtained is cadmium sulfide and shows no evident difference when synthesized with or without the use of UV light.

The Effect of Ultraviolet Radiation on the Chemical Bath Deposition of Bisthiourea Cadmium Chloride Crystals and the Subsequent CdS Obtention

This article presents a protocol for the synthesis of bis(thiourea) cadmium chloride crystals by chemical bath deposition. Two experiments are described: one aided by ultraviolet light compared to one without ultraviolet light.

紫外辐射对双 (硫脲) 氯化镉晶体化学镀液沉积的影响及随后的 CdS 获得

In this work, the effects on the preparation of bis(thiourea) cadmium chloride crystals when illuminated with ultraviolet (UV) light at a wavelength of ...