Name: niobium oxide films deposited by reactive sputtering: effect of oxygen flow rate
Uploaded: 2019-09-28T14:30:00
Description: Watch this Scientific Journal Video about Niobium Oxide Films Deposited by Reactive Sputtering: Effect of Oxygen Flow Rate at JoVE.com

这项工作得到了圣保罗埃斯塔多·埃斯奎萨基金会的支持，《圣保罗中心》（CDMF-FAPESP No 2013/07296-2， 2017/11072-3，2013/09963-6 和 2017/18916-2）。特别感谢Máximo Siu Li教授的PL测量。

1. 蚀刻和清洁基板
<ol><li>使用玻璃切割系统，形成 2.5 x 2.5 厘米的氟化物薄氧化物 （FTO） 基板。</li>
	<li>用热胶带保护基板表面的一部分，使一侧露出 0.5 厘米。</li>
	<li>将少量锌粉（足以覆盖待蚀区域）沉积在暴露的 FTO 顶部，并缓慢地将浓缩盐酸 （HCl） 滴在锌粉上，直到所有锌粉被反应消耗。紧接着，用去离子 （DI） 水冲洗基板。 注意：大量氢气是由锌和HCl反应产生的。</li>
	<li>取出胶?...

<ol>
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A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nb2O5+nanosize+powders+prepared+by+sol-gel+-+Structure,+morphology+and+dielectric+properties.">Nb2O5 nanosize powders prepared by sol-gel - Structure, morphology and dielectric properties.</a> Journal of Alloys and Compounds. 553, 177-182 (2013).</li><li>Kogo, A., Numata, Y., Ikegami, M., Miyasaka, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nb+2+O+5+Blocking+Layer+for+High+Open-circuit+Voltage+Perovskite+Solar+Cells.">Nb 2 O 5 Blocking Layer for High Open-circuit Voltage Perovskite Solar Cells.</a> Chemistry Letters. 44, 829-830 (2015).</li><li>Ueno, S., Fujihara, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+an+Nb2O5+nanolayer+coating+on+ZnO+electrodes+in+dye-sensitized+solar+cells.">Effect of an Nb2O5 nanolayer coating on ZnO electrodes in dye-sensitized solar cells.</a> Electrochimica Acta. 56, 2906-2913 (2011).</li><li>Fernandes, S. 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在这项工作中制备的氧化氮薄膜被用作在perovskite太阳能电池中的电子传输层。电子传输层最重要的特征是防止重组、堵塞孔和有效地传输电子。
在这方面，使用反应溅射技术是有利的，因为它产生密集和紧凑的薄膜。此外，如前所述，与溶胶、阳极氧化、热液和化学气相沉积合成方法14、21、22相比，活性溅射是最适合沉积大面积<s...

溅射技术被广泛用于沉积高质量的薄膜。其主要应用在半导体行业，虽然它也用于表面涂层，以改善机械性能，和反射层1。溅射的主要优点是有可能将不同的材料沉积在不同的基材上;良好的可重复性和对沉积参数的控制。溅射技术允许均匀薄膜沉积，与化学气相沉积 （CVD）、分子束外延 （MBE） 和原子层沉积 （ALD） 等其他沉积方法相比，在大面积且成本低。1，2.通常，由溅射沉积的半导体薄膜是无定形或多晶的，然而，有一些关于溅射3、4的外延生长的报告。然而，溅射过程非常复杂，参数范围宽5，因此，为了实现高质量的薄膜，必须对每种材料的过程和参数优化有良好的理解。
有几篇文章报道了氧化氮薄膜通过溅射沉积，以及氮化物6和碳化铀7。在Nb氧化物中，五氧化二氮（Nb2O5）是一种透明、空气稳定、水溶性的材料，具有广泛的多态性。它是一种 n 型半导体，带隙值范围从 3.1 到 5.3 eV，使这些氧化物具有广泛的应用范围8、9、10、11、12、13 ，14，15，16，17，18，19。Nb2O5作为一种有前途的材料，因其具有可比的电子注入效率和与二氧化钛 （TiO2）相比的化学稳定性，因此备受关注。此外，Nb2O5的带隙可以改善14单元的开路电压（Voc）。
在这项工作中，Nb2O5在不同的氧气流速下通过反应溅射沉积。在低氧流率下，薄膜的电导率增加，而不使用掺杂物，从而在系统内引入杂质。这些薄膜被用作在perovskite太阳能电池中的电子传输层，提高这些电池的性能。结果发现，减少氧气量会导致氧空位的形成，从而增加薄膜的导电性，使太阳能电池具有更高的效率。

<table>
	<tbody>
		<tr>
			<td>2-propanol</td>
			<td>Merck</td>
			<td>67-63-0</td>
			<td>solvent with maximum of 0.005% H2O</td>
		</tr>
		<tr>
			<td>4-tert-butylpyridine</td>
			<td>Sigma Aldrich</td>
			<td>3978-81-2</td>
			<td>chemical with 96% purity</td>
		</tr>
		<tr>
			<td>acetonitrile</td>
			<td>Sigma Aldrich</td>
			<td>75-05-8</td>
			<td>anhydrous solvent , 99.8% purity</td>
		</tr>
		<tr>
			<td>bis(trifluoromethane)sulfonimide lithium salt</td>
			<td>Sigma Aldrich</td>
			<td>90076-65-6</td>
			<td>chemical with &#8805;99.95% purity</td>
		</tr>
		<tr>
			<td>chlorobenzene</td>
			<td>Sigma Aldrich</td>
			<td>108-90-7</td>
			<td>anhydrous solvent , 99.8% purity</td>
		</tr>
		<tr>
			<td>ethanol</td>
			<td>Sigma Aldrich</td>
			<td>200-578-6</td>
			<td>solvent</td>
		</tr>
		<tr>
			<td>Fluorine doped tin oxide (SnO2:F) glass substrate</td>
			<td>Solaronix</td>
			<td>TCO22-7/LI</td>
			<td>substrate to deposit films</td>
		</tr>
		<tr>
			<td>Kaptom tape</td>
			<td>Usinainfo</td>
			<td>04227</td>
			<td>thermal tape used to cover the substrates</td>
		</tr>
		<tr>
			<td>Kurt J Lesker magnetron sputtering system</td>
			<td>Kurt J Lesker</td>
			<td>------</td>
			<td>Sputtering equipment used to deposit compact films</td>
		</tr>
		<tr>
			<td>Lead (II) iodide</td>
			<td>Alfa Aesar</td>
			<td>10101-63-0</td>
			<td>PbI2 salt- 99.998% purity</td>
		</tr>
		<tr>
			<td>methylammonium iodide</td>
			<td>Dyesol</td>
			<td>14965-49-2</td>
			<td>CH3NH3I salt</td>
		</tr>
		<tr>
			<td>N2,N2,N2&#8242;,N2&#8242;,N7,N7,N7&#8242;,N7&#8242;-octakis (4-methoxyphenyl)-9,9&#8242;-spirobi [9H-fluorene]-2,2&#8242;,7,7&#8242;-tetramine</td>
			<td>Sigma Aldrich</td>
			<td>207739-72-8</td>
			<td>Spiro-OMeTAD salt, 99% purity</td>
		</tr>
		<tr>
			<td>Niobium target of 3&#8221;</td>
			<td>CBMM- Brazilian Metallurgy and Mining Company</td>
			<td>------</td>
			<td>niobium sputtering target used in the sputtering system</td>
		</tr>
		<tr>
			<td>N-N dimethylformamide</td>
			<td>Merck</td>
			<td>68-12-2</td>
			<td>solvent with maximum of 0.003% H2O</td>
		</tr>
		<tr>
			<td>TiO2 paste</td>
			<td>Dyesol</td>
			<td>DSL 30NR-D</td>
			<td>titanium dioxide paste</td>
		</tr>
		<tr>
			<td>tris(2-(1H-pyrazol-1-yl)-4-tert-butylpyridine)cobalt(III) tri[bis(trifluoromethane)sulfonimide]</td>
			<td>Dyesol</td>
			<td>329768935</td>
			<td>FK 209 Co(III) TFSL salt</td>
		</tr>
	</tbody>
</table>

niobium oxide films deposited by reactive sputtering: effect of oxygen flow rate

反应溅射是一种多功能技术，用于形成具有极佳均匀性的紧凑型薄膜。此外，它还便于控制沉积参数，如气体流速，从而改变成分，从而改变薄膜所需的特性。在本报告中，反应溅射用于沉积氧化氮薄膜。镍靶作为金属源，不同的氧气流速沉积氧化氮薄膜。氧气流量从3sccm变为10 sccm。沉积在低氧流速率下的薄膜具有较高的导电性，当用作电子传输层时，可提供更好的超氧化物太阳能电池。

在溅射系统中，沉积速率受氧流速的影响很大。当氧气流量增加时，沉积速率降低。考虑到所用目标区域的现状和等离子体功率，从3至4sccm的沉积速率有表达性下降，然而，当氧气从4个增加到10sccm时，它变得不那么明显。在3 sccm的体制中，沉积速率为1.1 nm/s，在10 sccm中突然减小到0.1纳米/s，如图1所示。
形成的氧化氮相取决于氧气流速。对于小于3 sccm 的...

Watch this Scientific Journal Video about Niobium Oxide Films Deposited by Reactive Sputtering: Effect of Oxygen Flow Rate at JoVE.com

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

在这里，我们提出了一个协议，通过反应溅射以不同的氧气流速沉积氧化氮薄膜，作为在perovskite太阳能电池中的电子传输层。

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 ...

在反应溅射技术中，可以对参数进行精细控制，从而可以沉积具有不同的蒸馏计和偏好的氧化氮烟气。该技术的主要优点是沉积均匀烟雾，在大面积、成本低、阻碍生产上均匀。注意每一步，不要跳过任何步骤，这一点很重要。实现如何处理设备和烟雾的最终外观有助于实现良好的沉积。首先使用热胶带保护基板表面，使 0.5 厘米的一侧暴露在外。沉积足够的锌粉，覆盖在暴露的氟化物薄氧化物顶部蚀刻的区域。然后慢慢滴浓缩盐酸，直到所有的锌粉被反应消耗。立即用电离水清洗基材。取出磁带。用肥皂对基质进行15分钟的声波化，然后用水、丙酮和异丙醇酒精进行两次。通过金属阴影面罩固定基板后，将基板放入溅射室。密封腔室后，启动机械泵，然后打开涡轮分子泵。当真空达到负 5 倍 10 到负 5 托rr 时，打开水冷却器系统并打开基板加热系统。将温度设置为 500 摄氏度，每五分钟增加 100 摄氏度，直到达到预期值。将砷设置为 40 SCCM，将氧气设置为每分钟 3 个标准立方厘米。将阿贡引入房间。将压力设置为负 10 的 5 倍至负 3 托，将无线电频率设置为 120 瓦。打开无线电频率。使用阻抗匹配框调谐频率。如果等离子体不启动，请缓慢增加压力，直到达到负2 10到负2托。使用可打开或关闭的闸阀来改变泵送速率以设置压力。将等离子体保持 120 瓦 10 分钟，以清洁镍靶，并清除其表面存在的任何氧化物层。稳定后，将氧气引入腔室，将射频功率设置为 240 瓦，然后打开基板快门。开始沉积并设定沉积时间，达到100纳米的最终厚度。沉积完成后，请关闭快门，关闭射频，关闭气体，降低基板温度。当基板温度达到室温时，在打开腔室并拆下基板之前引入空气以重新建立环境压力。在太阳能电池结构中，用一块胶带保护基板的两侧，并使用旋转涂布器，每分钟旋转 4000 次，30 秒，将中孔二氧化钛层沉积到氧化钛层上。然后根据指示的加热顺序将基板放入烤箱中。当烤箱达到室温时，使用旋转涂布器将两层碘化铅以每分钟 6000 次旋转的速度沉积到二氧化钛层中，90 秒。将基板放在热板或 70 摄氏度上，每次沉积后 10 分钟。热处理后，将300毫升的碘化甲酸甲基胺溶液滴到碘化铅层上，等待20秒，然后以每分钟4000次旋转30秒的速度旋转。在旋转结束时，将基板在 100 摄氏度下放在热板上 10 分钟，然后将 Spiro OMetTAD 溶液以每分钟 4，000 次旋转的速度沉积在旋转涂器的 perovskite 层顶部，旋转 30 秒。然后将薄膜储存在干燥器中过夜，以氧化斯皮罗·奥梅特塔德。第二天早上，刮起佩罗夫斯基特的胶片，露出 FTO 。使用阴影面罩以 0.2 安格罗姆/秒的速度将金接触点沉积在蒸发器中，直到厚度达到 5 纳米，然后将金接触率提高至 17 纳米/秒。"然后，单元格即可进行测试。在溅射系统中，沉积速率受氧流速的强，当氧流量增加时，沉积速率会降低。例如，从 3 到 4 SCCM，沉积速率有表现力的下降。当氧气增加时，从4到10 SCCM，然而沉积率变得不那么明显。形成的氧化氧化硅阶段取决于氧气流速，而对于流量小于3的SCCM二氧化氮是形成的主要相。对于流量等于或高于 3.5 SCCM，氧气量过高，无法产生二氧化氮。相反，五氧化氮被观测为主要阶段。电子显微镜图像显示沉积在三点五、四和十 SCCM 的薄膜的纳米公制球形颗粒。相比之下，沉积在三个 SCCM 的薄膜会露出片状颗粒。反应溅射在不同氧流速中沉积的薄膜表现出不同的电气特性。当使用三个 SCCM 氧气时，薄膜的电导率会提高。当氧气流速增加到三点五、四或十 SCCM 时，电导率会降低。佩罗夫斯基特太阳能电池的性能也取决于使用的氧化二氮。作为一个用电子传输层沉积在三点五 SCCM的电池，具有最佳性能，短路电流最高。在开始沉积氧化氮薄膜之前，请记住所有参数是否设置正确。氧化氮薄膜也是推迟化学溶液的原因。然而，金属不允许沉积不同的测定。是分析氧化钛烟雾的电导率如何影响白化硅太阳能电池性能的部件的发展。使用化学品进行永久沉积时小心，并确保遵守所有实验室安全规则。

Research

JoVE Journal

Chemistry

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

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 ...

科研

化学

Fabrication of Large-area Free-standing Ultrathin Polymer Films

大面积的制造自立性的超薄聚合物薄膜

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films.  Typically, ultrathin films are prepared ...

Unraveling Entropic Rate Acceleration Induced by Solvent Dynamics in Membrane Enzymes

揭开熵率的加速溶剂动力学的膜酶诱导

Enzyme catalysis evolved in an aqueous environment. The influence of solvent dynamics on catalysis is, however, currently poorly understood and usually ...

Cooling Rate Dependent Ellipsometry Measurements to Determine the Dynamics of Thin Glassy Films

冷却率相关的椭偏仪测量确定薄膜玻膜的动力学

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements ...

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

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 ...

Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR

溶出动态核极化仪器用NMR实时酶反应速率测量

The main limitation of NMR-based investigations is low sensitivity. This prompts for long acquisition times, thus preventing real-time NMR measurements of ...

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

金属氧化物结构的气溶胶辅助化学气相沉积: 氧化锌棒

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

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

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. ...

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

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

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 ...

U2O5 Film Preparation via UO2 Deposition by Direct Current Sputtering and Successive Oxidation and Reduction with Atomic Oxygen and Atomic Hydrogen

U2O5 Film Preparation via UO2 Deposition by Direct Current Sputtering and Successive Oxidation and Reduction with Atomic Oxygen and Atomic Hydrogen

利用uo2沉积制备 u2o5 薄膜, 利用原子氧和原子氢连续氧化还原

We describe a method to produce U2O5 films in situ using the Labstation, a modular machine developed at JRC Karlsruhe. The Labstation, an essential part ...