这项工作得到了西班牙科学和创新部的支持, 其部分原因是 TEC2015-74329-金 (AEI/菲德、欧盟)、TEC2016-79898-C6-1-R (AEI/菲德、欧盟) 和 TEC-2013-48147-C6-6R (AEI/菲德、欧盟)。SV 承认欧洲联盟和南亚区域联合ﬁnanced SoMoPro 第二方案的支持, 通过赠款4SGA8678。jč承认 MEYS 提供的资金, 项目 No。LQ1601 (CEITEC 2020)。这项研究的一部分利用了六研究中心的基础设施, 通过捷克共和国教育、青年和体育部资助的 CEITEC 开放项目下的 CEITEC 的核心设备, 以及西班牙信通技术网络 MICRONANOFABS 部分支持的 MINECO。

备注: 出于安全原因, 反应单元和气溶胶发生器放置在通风罩内。使用镊子来处理样品, 戴手套, 实验室大衣和护目镜, 并遵循常见的实验室安全做法. 
 1。衬底的制备及沉积温度的设置 <ol> <li> 使用菱形笔尖剪切器切割 10 mm x 10 mm 的硅基板 (基板尺寸已适应我们的反应单元大小)。在本试验中, 使用自制的不锈钢圆柱反应单元, 其内部容积为 7000 mm 3 (直径:30 mm, 高度:10 mm), 适应于用于制造的硅微机械平台的尺寸的气体传感器. </li>
	<li> 用异丙醇清洗基体, 用去离子水冲洗, 用氮气吹干基体, 确保薄膜的附着力和基体的均匀覆盖. </li>
	<li> 将衬底放入反应单元。当使用硅基微机械平台, 而不是裸硅衬底制造气体传感器, 把微机械平台的反应细胞, 然后与阴影的面具, 以限制增长的材料的面积兴趣. </li>
	<li> 关闭反应单元。确保反应单元的盖子正确密封, 以避免活性物质的泄漏. </li>
	<li> 合闸温度控制系统, 包括与反应电池集成的电阻加热器、热电偶, 以感知基板的温度和比例积分导数 (PID) 控制器. </li>
	<li> 将温度设置为400和 #176; C 让它稳定 (这个过程大约需要30分钟, 但它可能会根据反应细胞的尺寸和温度控制系统的特性而变化). </li>
</ol> 2。气溶胶生成溶液的制备 <ol> <li> 添加50毫克的 ZnCl 2 到100毫升的玻璃瓶装有真空阱 (29/32 接头, 200 毫米长度, 5 毫米软管倒钩). </li>
	<li> 溶解 ZnCl 2 在5毫升乙醇中, 然后用真空阱将瓶子盖住。确保下管端坐60毫米以上的瓶子底部, 并没有淹没在解决方案。如果需要, 使用玻璃接头夹在 CVD 过程中将瓶子和真空阱固定在一起. </li>
	<li> 将小瓶夹紧到通用支架上。调整的高度, 以满足瓶底和超声雾化器的最佳焦点, 在1.6 兆赫运作, 并提供了平均大小的气溶胶雾滴和 #8764; 3 和 #181; m. </li>
	<li> 分别将真空阱的入口和排气连接到氮气管道和反应单元, 如 "气溶胶辅助 CVD 系统的简化方案" 中所示 图 1 . </li>
	<li> 对每种沉积物使用新的反应液. </li>
</ol> 3。cvd 过程 <ol> <li> 在启动 cvd 过程之前, 请验证反应单元中的温度是否已达到稳定状态. </li>
	<li> 将氮气流量调整到 200 cm 3 /分钟, 并允许它流经系统 (根据我们的实验中所用的反应单元的尺寸, 流量已经调节)。建议使用质量流量控制器, 以确保在沉积过程中恒定流动. </li>
	<li> 合闸气溶胶发生器, 并保持气溶胶常数在这个过程中, 直到包含锌前驱体的溶液完全交付到反应细胞 (这个过程需要大约120分钟, 考虑5毫升的溶液体积和流速200厘米 3 /分钟. </li>
	<li> 当解决方案已完全交付给反应单元, 断的气溶胶发生器和温度系统冷却反应细胞。同时保持氮气在整个系统中流动. </li>
	<li> 当温度降至室温时, 关闭氮气流, 打开反应单元, 并取出样品。基板将显示在表面上的灰哑光颜色, 不同于闪亮的裸硅片 (硅微机械平台在 CVD 步骤后显示类似的外观)。这种无光泽的颜色与柱状 ZnO 结构的存在有关, 如扫描电子显微镜观察到的那样 ( 图 2 ). </li>
</ol>

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作者没有透露

这里详述的气雾剂辅助 CVD 过程在10毫米 x 10 毫米的硅瓦片导致 ZnO 棒的形成。这个做法可以被扩大到外套更大的表面;然而, 注意到反应细胞体积的增加将需要调整参数, 如载流子流速和溶液体积。对于较大的反应电池, 也建议控制在基板的温度梯度, 由于微妙的梯度小于10° c 可能有强烈的影响, 由此产生的形态学的胶片, 如前所示氧化钨的气溶胶辅助 CVD8。为了重现在这里报告的结果, 我们建议使用与协议中描述的类似的工作频率的超声波雾化器, 因为气溶胶的平均雾滴大小和由此产生的薄膜形貌受到此参数7。
其他 ZnO 形貌的选择性沉积, 而不是棒, 也可以通过改变前驱体、沉积温度或载体溶剂来实现。例如, 使用前体, 如二乙锌14或醋酸锌的15 , 已被证明导致形成其他形态的形式, 而不是六角棒。我们还注意到, 在气溶胶辅助 CVD 过程中使用不同的沉积温度会产生薄膜的形貌变化, 从而在400° c 以下温度下形成多晶薄膜, 在当达到600° c 时, 基体上的温度超过400° c, 或退化且密度较低的结构。同样, 使用不同的溶剂会影响薄膜的形貌, 例如, 我们最近已经证明, 在400° c 的沉积温度下使用甲醇鼓励形成具有鳞片状形貌的结构, 而丙酮在相同温度下的使用鼓励了倒锥状结构的形成9。
温度和载体溶剂的作用以前也被注意了在其他金属氧化物结构的气雾剂辅助的 CVD (例如, 氧化钨的5和氧化锡6), 并且它一般归因于: 化学作用由反应性中间体引起, 在处理温度下成为活跃种类为沉积或反应均匀地形成固体微粒 (这更可能为溶剂例如甲醇和丙酮, 在低温可能分解如, #60; 500 ° c);和调制率的沉积 (通量) 和雾滴蒸发 (这是更有可能占主导地位的溶剂作为乙醇, 不形成活性的自由基物种的温度在我们的实验中使用)。
此处报告的协议与基于硅的电子器件的最先进的微细加工工艺相兼容, 并有可能在涉及高耐热柔性材料的过程中被纳入, 因为相对较低结构的气溶胶辅助 CVD 的温度。然而, 重要的是要提到, 使用阴影面具的选择增长的结构, 如在种子方法的基础上的蒸气-液体-固体机制16, 可能有限制在某些制造过程。另一方面, 通过这里提出的催化的方法来发展结构的可能性可能具有较少的光刻和金属化步骤的优势, 在芯片集成的结构。此外, 相对低温的合成 ZnO 棒也可能允许使用这种方法与局部加热, 一种技术, 用于限制所需的热环境分解的气相反应物和结构的生长动力学对一个微型区域, 极大地减少功率消耗量高温 (热壁) 反应器17。例如, 在催化气溶胶辅助的氧化钨燃料的 CVD 中, 使用局部加热已经证明是可行的18。在化学传感、光催化、光子学和能量等领域, 具有受控形态的柱状 ZnO 结构的生长, 使其易于集成到不同的基体和微细加工过程中, 具有共同的兴趣。收割, 除其他之外。

ZnO 是一种具有宽直带隙 (3.37 eV)、大激子结合能 (60 兆伏特)、自发极化和压电常数的 II-VI 半导体, 使其成为电子、光电子、能量发生器的极具吸引力的材料,光催化和化学传感。ZnO 的大部分有趣的功能与它的矿晶体结构及其非极性 (例如、{100}、{110}) 和极 (例如、{001}、{111}) 曲面相关, 与特定的结构化形态表 (例如:, 棒, 金字塔, 盘子)。这些形态形式的控制需要合成方法, 能够产生定义明确的晶体, 具有均匀的尺寸、形状和表面结构1,2,3,4。在这种情况下, 新的添加剂 (自下而上的合成) 制造策略, 特别是基于气相路线是工业上有吸引力的和潜在的优势, 因为它们提供的能力, 产生结构化的电影在连续而比具有高纯度和高吞吐量的间歇模式。这些路线以前显示了 ZnO 结构的影片的形成, 但通常使用催化剂种子例如金子并且/或者高处理温度 900-1300 ° c2 {Wang, 2008 #491} (这可能是不方便的某些制造过程由于需要额外的处理步骤和/或温度不兼容的芯片集成)。
最近, 我们使用了气相法, 基于气溶胶辅助 CVD 的无机或金属-有机前体, 以实现选择性沉积金属氧化物结构 (例如, 氧化钨的5或锡氧化物6), 没有需要的催化剂种子和在较低的温度比那些报告的传统 CVD。这种方法在大气压下工作, 可以使用比传统 CVD 更少的挥发性前体;溶解性是关键的前驱体要求, 因为前驱体溶液以气溶胶形式传递到反应区7。在气溶胶辅助 CVD 中, 结构材料和薄膜的成核和生长动力学受反应物种的合成温度和浓度的影响, 从而影响膜的形态形式的8。最近, 我们研究了 zno 对各种气溶胶辅助 CVD 条件 (包括前体、温度、载体溶剂和前驱体浓度) 的形貌依赖性, 并找到了结构化 zno 与棒的形成途径,片状或倒锥体状的形态, 在其他9中。
在本文中, 我们提出了由 {100} 表面组成的棒状 ZnO 结构的气溶胶辅助 CVD 的协议。该协议与各种衬底兼容, 包括硅, 硅基微机械平台, 石英, 或高耐热聚酰亚胺箔。在这份报告中, 我们专注于裸硅片的涂层和用于制造气体传感器的基于硅的微机械平台。氧化锌气溶胶辅助 CVD 由三处理步骤组成, 包括: 制备基底和沉积温度的设置、气溶胶生成溶液的制备和 cvd 过程。下面详细介绍了这些步骤, 并在图 1中显示了显示系统主要元素的示意图视图.

<table border="0" cellpadding="0" cellspacing="0" width="824">
	<tbody>
		<tr height="25">
			<td height="25" style="height:25px;width:272px;">ZnCl2 99,999 % trace metal basis</td>
			<td style="width:124px;">Sigma-Aldrich&#160;</td>
			<td style="width:121px;">229997</td>
			<td style="width:307px;">used as purchased from manufacturer</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Ethanol &#8805;96%</td>
			<td style="width:124px;">Penta</td>
			<td style="width:121px;">71430</td>
			<td style="width:307px;">used as purchased from manufacturer</td>
		</tr>
		<tr height="108">
			<td height="108" style="height:108px;width:272px;">Reaction cell&#160;</td>
			<td style="width:124px;">home-made</td>
			<td style="width:121px;"></td>
			<td style="width:307px;">stainless steel cylindrical reaction cell (7000 mm3, diameter: 30 mm, height: 10 mm) with integrated heaters to reach the temperature of deposition and provided with a PID controller</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Ultrasonic liquid atomizer</td>
			<td style="width:124px;">Johnson Matthey</td>
			<td style="width:121px;"></td>
			<td style="width:307px;">Operating frequency &#8764;1,6 MHz</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:272px;">Flowmeter</td>
			<td style="width:124px;"></td>
			<td style="width:121px;"></td>
			<td style="width:307px;">To have a better control of this step the use of a mass flow controller is recommended.&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Nitrogen</td>
			<td style="width:124px;">Linde Gas A.S.</td>
			<td style="width:121px;"></td>
			<td style="width:307px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:272px;">Silicon wafers&#160;&#160;</td>
			<td style="width:124px;">MicroChemicals</td>
			<td style="width:121px;"></td>
			<td style="width:307px;">&#60;100&#62;, p-type, 525 &#181;m thick, cut into pieces (10 mm &#215; 10 mm )</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Glass vial - 100 ml</td>
			<td style="width:124px;"></td>
			<td style="width:121px;"></td>
			<td style="width:307px;">29/32 joint, 200 mm lenght</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Vacuum trap</td>
			<td style="width:124px;"></td>
			<td style="width:121px;"></td>
			<td style="width:307px;">29/32 joint, 5 mm hose barbs&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Graduated cylinder - 10 ml</td>
			<td style="width:124px;"></td>
			<td style="width:121px;"></td>
			<td style="width:307px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Universal support&#160;</td>
			<td style="width:124px;"></td>
			<td style="width:121px;"></td>
			<td style="width:307px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Balance</td>
			<td style="width:124px;"></td>
			<td style="width:121px;"></td>
			<td style="width:307px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">Scanning Electron Microscopy (SEM)</td>
			<td style="width:124px;">Tescan</td>
			<td style="width:121px;">Mira II LMU</td>
			<td style="width:307px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:272px;">X-ray diffraction (XRD)</td>
			<td style="width:124px;">Rigaku&#160;</td>
			<td style="width:121px;">Smart Lab 3kW</td>
			<td style="width:307px;">Cu K&#945; radiation</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:272px;">X-ray Photoelectron spectroscopy (XPS)</td>
			<td style="width:124px;">Kratos</td>
			<td style="width:121px;">AXIS Supra</td>
			<td style="width:307px;">Monochromatic&#160; K&#945; radiatio, 300 W emission power, magnetic lens, and charge compensation&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:272px;">Transmission Electron Microscopy (TEM)</td>
			<td style="width:124px;">Jeol</td>
			<td style="width:121px;">JEM 2100F</td>
			<td style="width:307px;">operated at 200kV using Schottky cathode and equiped with EDX&#160;</td>
		</tr>
	</tbody>
</table>

aerosol-assisted chemical vapor deposition of metal oxide structures: zinc oxide rods

虽然柱状氧化锌 (ZnO) 结构以棒或线的形式在以前被不同的液体或气相路线合成, 它们的高成本生产和/或与微细加工技术的不相容, 由于使用pre-deposited 催化剂-种子和/或高处理温度超过900° c, 代表了普遍使用这些方法的一个缺点。然而, 在这里, 我们报告的合成氧化锌棒通过一个催化蒸气固体机制启用了使用气溶胶辅助化学气相沉积 (CVD) 方法在400° c 与氯化锌 (ZnCl2) 作为前体和乙醇作为载体溶剂。这种方法提供了 ZnO 棒的单步形成和与各种基材类型直接集成的可能性, 包括硅、硅微机械平台、石英或高耐热聚合物。这可能有助于在 large-scale 中使用此方法, 因为它与设备制造的最先进的微细加工工艺相兼容。本报告还描述了这些结构的性质 (例如、形态学、晶相、光带间隙、化学成分、电阻) 并验证其对一氧化碳的气体传感功能。

在乙醇中溶解的 ZnCl2的气溶胶辅助 CVD 导致在裸硅片上形成灰均匀的和附着的薄膜 (机械上相对容易磨损)。利用扫描电子显微镜 (SEM) 对薄膜进行表征, 8,000X 放大显示 quasi-aligned 六角形 ZnO 棒, 长度为∼1,600 和∼380 nm 直径 (图 2)。在设定点温度下的较大误差或在 CVD 过程中沿基底温度梯度的存在可能导致其他 ZnO 形貌的沉积 ,如 (图3) 或具有非均匀结构的薄膜。此外, 不均匀或换药的涂层可能部分地与温度控制差、流量的不正确调整和/或使用不同的载体溶剂, 而不是本议定书所规定的。
x 射线衍射 (XRD) 分析的棒显示与六角氧化锌相关联的衍射模式 (P63mc空间组, a = 3.2490 Å, b = 3.2490 Å, 和c = 5.2050 Å;iccd/cop No. 5-0664)。这些模式在 34.34°2θ上显示一个高强度的衍射峰值, 对应于六角氧化锌相的 (002) 平面, 与其他七低强度衍射峰在 31.75, 36.25, 47.54, 56.55, 62.87, 67.92, 和 72,61° 2θ, 对应于六角氧化锌相的 (100) (101) (102) (110) (103) (201) 和 (004) 平面。通过高分辨率透射电子显微镜 (TEM) 表征棒材, 显示出标出的平面间距 (0.26 nm) 与 x 射线衍射识别的 (002) 平面 (d = 0.26025 nm) 的内部晶格相一致。能量色散 X 射线 (EDX) 光谱学显示了锌的存在相对地低氯污秽 (发现为氯: 锌0.05 在%)。
通过薄膜的漫反射测量来估计杆的光带隙, 表示 3.2 eV 的光带隙, 与 ZnO10的文献值一致。用 X 射线光电子能谱 (XPS) 分析薄膜的特点是锌 2p1/2和 zn 2p3/2核心级峰值光谱分别为1045和 1022 eV, 一致与那些早先被观察的那些为 ZnO11,12。
该协议的使用, 在基于硅的微机械平台的气体传感, 导致直接集成的柱状 ZnO 棒限制在传感活动区 (400 x 400 µm2), 这是由阴影掩码定义。该薄膜的电阻ω (∼100ω) 在室温下, 使用指电极集成到硅微机械平台中进行测量。图4显示基于气溶胶辅助 CVD 棒的四微机械气体传感器阵列的图片。本文介绍了微机械平台的特点和制作过程, 并描述了13。这些微计算机系统是敏感的相对低浓度的一氧化碳, 最大的反应记录 (使用连续气体流量测试室13) 时, 传感器的操作在360° c 使用电阻 microheaters 集成在系统中 (图 5)。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/56127/56127fig1.jpg"> 
图1:气溶胶辅助 CVD 系统的示意图.
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/56127/56127fig2.jpg"> 
图2:顶部 (A) 和横截面 (B) 通过气溶胶辅助 CVD 沉积的 ZnO 棒的 SEM 图像。<a href="//ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/56127/56127fig2large.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/56127/56127fig3.jpg"> 
图3:ZnO 在 300 (A)、400 (B)、500 (C) 和600° c (D) 上沉积的via气雾剂辅助 CVD 的横断面 SEM 图像。<a href="//ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/56127/56127fig3large.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/56127/56127fig4.jpg"> 
图4:硅基微机械平台, 4 传感器安装在 TO8-package (a) 上, 并详细查看传感器 (B) 和沉积在电极边缘 (C) 的 ZnO 棒。<a href="//ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/56127/56127fig4large.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/56127/56127fig5.jpg"> 
图5:氧化锌棒对不同浓度 (25、20、10和 5 ppm) 的电阻变化.<a href="//ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/56127/56127fig5large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

Watch this Scientific Journal Video about Aerosol-assisted Chemical Vapor Deposition of Metal Oxide Structures: Zinc Oxide Rods at JoVE.com

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

金属氧化物结构的气溶胶辅助化学气相沉积: 氧化锌棒

在不使用 pre-deposited 催化剂-种子颗粒的情况下, 通过气溶胶辅助化学气相沉积法合成柱状氧化锌结构。这种方法是可伸缩和兼容的各种基板的基础上, 无论是硅, 石英或聚合物。

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

aerosol-assisted-chemical-vapor-deposition-metal-oxide-structures

Nanyang Technological University

Research

JoVE Journal

Chemistry

13.0K 次观看.  Instituto de Microelectrónica de Barcelona (IMB-CNM, CSIC). 在不使用 pre-deposited 催化剂-种子颗粒的情况下, 通过气溶胶辅助化学气相沉积法合成柱状氧化锌结构。这种方法是可伸缩和兼容的各种基板的基础上, 无论是硅, 石英或聚合物。

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

Preparation of Hydrophobic Metal-Organic Frameworks via Plasma Enhanced Chemical Vapor Deposition of Perfluoroalkanes for the Removal of Ammonia

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high surface area microporous materials, such as metal-organic frameworks (MOFs), unique challenges present themselves for PECVD treatments. Herein the protocol for development of a MOF that was previously unstable to humid conditions is presented. The protocol describes the synthesis of Cu-BTC (also known as HKUST-1), the treatment of Cu-BTC with PECVD of perfluoroalkanes, the aging of materials under humid conditions, and the subsequent ammonia microbreakthrough experiments on milligram quantities of microporous materials. Cu-BTC has an extremely high surface area (~1,800 m2/g) when compared to most materials or surfaces that have been previously treated by PECVD methods. Parameters such as chamber pressure and treatment time are extremely important to ensure the perfluoroalkane plasma penetrates to and reacts with the inner MOF surfaces. Furthermore, the protocol for ammonia microbreakthrough experiments set forth here can be utilized for a variety of test gases and microporous materials.

Herein the procedures for plasma enhanced chemical vapor deposition of perfluoroalkanes on microporous materials such as metal-organic frameworks to enhance their stability and hydrophobicity are described. Furthermore, breakthrough testing of milligram quantities of samples is described in detail.

增强型氟烷烃的化学气相沉积等离子通过疏水金属 - 有机骨架的制备氨的去除

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high ...

科研

化学

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

原子定义模板复合氧化物薄膜的外延生长

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

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 ...

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 ...

Highly Stable, Functional Hairy Nanoparticles and Biopolymers from Wood Fibers: Towards Sustainable Nanotechnology

Nanoparticles, as one of the key materials in nanotechnology and nanomedicine, have gained significant importance during the past decade. While metal-based nanoparticles are associated with synthetic and environmental hassles, cellulose introduces a green, sustainable alternative for nanoparticle synthesis. Here, we present the chemical synthesis and separation procedures to produce new classes of hairy nanoparticles (bearing both amorphous and crystalline regions) and biopolymers based on wood fibers. Through periodate oxidation of soft wood pulp, the glucose ring of cellulose is opened at the C2-C3 bond to form 2,3-dialdehyde groups. Further heating of the partially oxidized fibers (e.g., T = 80 &#176;C) results in three products, namely fibrous oxidized cellulose, sterically stabilized nanocrystalline cellulose (SNCC), and dissolved dialdehyde modified cellulose (DAMC), which are well separated by intermittent centrifugation and co-solvent addition. The partially oxidized fibers (without heating) were used as a highly reactive intermediate to react with chlorite for converting almost all aldehyde to carboxyl groups. Co-solvent precipitation and centrifugation resulted in electrosterically stabilized nanocrystalline cellulose (ENCC) and dicarboxylated cellulose (DCC). The aldehyde content of SNCC and consequently surface charge of ENCC (carboxyl content) were precisely controlled by controlling the periodate oxidation reaction time, resulting in highly stable nanoparticles bearing more than 7 mmol functional groups per gram of nanoparticles (e.g., as compared to conventional NCC bearing &#60;&#60; 1 mmol functional group/g). Atomic force microscopy (AFM), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) attested to the rod-like morphology. Conductometric titration, Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), dynamic light scattering (DLS), electrokinetic-sonic-amplitude (ESA) and acoustic attenuation spectroscopy shed light on the superior properties of these nanomaterials.

Synthesis schemes to prepare highly stable wood fiber-based hairy nanoparticles and functional cellulose-based biopolymers have been detailed.

高稳定性，功能性毛纳米粒子和木纤维生物聚合物:迈向可持续纳米技术

Nanoparticles, as one of the key materials in nanotechnology and nanomedicine, have gained significant importance during the past decade. While ...

In Situ Detection and Single Cell Quantification of Metal Oxide Nanoparticles Using Nuclear Microprobe Analysis

Micro-analytical techniques based on chemical element imaging enable the localization and quantification of chemical composition at the cellular level. They offer new possibilities for the characterization of living systems and are particularly appropriate for detecting, localizing and quantifying the presence of metal oxide nanoparticles both in biological specimens and the environment. Indeed, these techniques all meet relevant requirements in terms of (i) sensitivity (from 1 up to 10 &#181;g.g-1 of dry mass), (ii) micrometer range spatial resolution, and (iii) multi-element detection. Given these characteristics, microbeam chemical element imaging can powerfully complement routine imaging techniques such as optical and fluorescence microscopy. This protocol describes how to perform a nuclear microprobe analysis on cultured cells (U2OS) exposed to titanium dioxide nanoparticles. Cells must grow on and be exposed directly in a specially designed sample holder used on the optical microscope and in the nuclear microprobe analysis stages. Plunge-freeze cryogenic fixation of the samples preserves both the cellular organization and the chemical element distribution. Simultaneous nuclear microprobe analysis (scanning transmission ion microscopy, Rutherford backscattering spectrometry and particle induced X-ray emission) performed on the sample provides information about the cellular density, the local distribution of the chemical elements, as well as the cellular content of nanoparticles. There is a growing need for such analytical tools within biology, especially in the emerging context of Nanotoxicology and Nanomedicine for which our comprehension of the interactions between nanoparticles and biological samples must be deepened. In particular, as nuclear microprobe analysis does not require nanoparticles to be labelled, nanoparticle abundances are quantifiable down to the individual cell level in a cell population, independently of their surface state.

In Situ Detection and Single Cell Quantification of Metal Oxide Nanoparticles Using Nuclear Microprobe Analysis

We describe a procedure for the detection of chemical elements present in situ in human cells as well as their in vitro quantification. The method is well-suited to any cell type and is particularly useful for quantitative chemical analyses in single cells following in vitro metal oxide nanoparticles exposure.

原位金属氧化物纳米粒子的核探针检测与单细胞定量研究

Micro-analytical techniques based on chemical element imaging enable the localization and quantification of chemical composition at the cellular level. ...

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. ...

Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

The synthesis of 3,5-lutidine N-oxide dehydrate, 1, was achieved in the synthesis route of 2-amino-pyridine-3,5-dicarboxylic acid. Ochiai first used the methodology for non-substituted pyridines in 1957 in a 12 h process, but no X-ray suitable crystals were obtained. The substituted ring used in the methodology presented here clearly influenced the addition of water molecules into the asymmetric unit, which confers a different nucleophilic strength in 1. The X-ray suitable crystal compound 1 was possible due to the stabilization of the negative charge in the oxygen by the presence of two water molecules where the hydrogen atoms donate positive charge into the ring; such water molecules serve well to construct a supramolecular interaction. The hydrated molecules may be possible for the alkaline system that is reached by adjusting the pH to 10. Importantly, the double methyl substituted ring and a reaction time of 5 h, makes it a more versatile method and with wider chemical applications for future ring insertions.

Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

Herein, we report the synthesis and crystallization of 3,5-lutidine N-oxide dehydrate by a simple protocol that differs from the classical synthesis of pyridine N-oxide. This protocol utilizes different starting material and involves less reaction time to yield a new solvated supramolecular structure, which crystallizes under slow evaporation.

35-吡啶N-氧化物脱水的合成、结晶和光谱表征

The synthesis of 3,5-lutidine N-oxide dehydrate, 1, was achieved in the synthesis route of 2-amino-pyridine-3,5-dicarboxylic acid. Ochiai first used the ...

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

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven effective in gas adsorption, separations, and catalysis. MOFs are most commonly synthesized as bulk powder, requiring additional processes to adhere them to functional devices and fabrics that risk decreasing the powder porosity and adsorption capacity. Here, we demonstrate a method of first coating fabrics with metal oxide films using atomic layer deposition (ALD). This process creates conformal films of controllable thickness on each fiber, while providing a more reactive surface for MOF nucleation. By submerging the ALD coated fabric in solution during solvothermal MOF synthesis, the MOFs create a conformal, well-adhered coating on the fibers, resulting in a MOF-functionalized fabric, without additional adhesion materials that may block MOF pores and functional sites. Here we demonstrate two solvothermal synthesis methods. First, we form a MIL-96(Al) layer on polypropylene fibers using synthetic conditions that convert the metal oxide to MOF. Using initial inorganic films of varying thicknesses, diffusion of the organic linker into the inorganic allows us to control the extent of MOF loading on the fabric. Second, we perform a solvothermal synthesis of UiO-66-NH2 in which the MOF nucleates on the conformal metal oxide coating on polyamide-6 (PA-6) fibers, thereby producing a uniform and conformal thin film of MOF on the fabric. The resulting materials can be directly incorporated into filter devices or protective clothing and eliminate the maladroit qualities of loose powder.

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

Metal-organic frameworks are effective in gas storage and heterogeneous catalysis, but typical synthesis methods result in loose powders that are difficult to incorporate into smart materials. We demonstrate a method of first coating fabrics with ALD metal oxides, resulting in conformal films of MOF on the fabrics during solvothermal synthesis.

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 ...

Preparation of Polyoxometalate-based Photo-responsive Membranes for the Photo-activation of Manganese Oxide Catalysts

This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic polymers, with the aim of photo-activating oxygen-evolving manganese oxide catalysts, which are important components in artificial photosynthesis. The cross-linking technique was applied to obtain a self-standing membrane with a high PW12O403- content. Incorporation and structure retention of PW12O403- within the polymer matrix were confirmed by FT-IR and micro-Raman spectroscopy, and optical characteristics were investigated by UV-Vis spectroscopy, which revealed successful construction of the metal-to-metal charge transfer (MMCT) unit. After deposition of MnOx oxygen evolving catalysts, photocurrent measurements under visible light irradiation verified the sequential charge transfer, Mn &#8594; MMCT unit &#8594; electrode, and&#160;the photocurrent intensity was consistent with the redox potential of the donor metal (Ce or Co). This method provides a new strategy for preparing integrated systems involving catalysts and photon-absorption parts for use with photo-functional materials.

Here, we present a protocol to prepare charge transfer chromophores based on a polyoxometalate/polymer composite membrane.

氧化锰催化剂光活化 Polyoxometalate 基光响应膜的制备

This paper presents a method to prepare charge-transfer chromophores using polyoxotungstate (PW12O403-), transition metal ions (Ce3+ or Co2+), and organic ...