Name: solution-processed "silver-bismuth-iodine" ternary thin films for lead-free photovoltaic absorbers
Uploaded: 2018-09-27T14:45:00
Description: Watch this Scientific Journal Video about Solution-Processed "Silver-Bismuth-Iodine" Ternary Thin Films for Lead-Free Photovoltaic Absorbers at JoVE.com

这项工作得到了科学、信息和通信技术部 (18-01) Gyeongbuk 科技研究院 (DGIST) 研究与开发 (R & D) 项目的支持。这项工作还得到韩国能源技术评估和规划研究所 (KETEP) 和大韩民国贸易、工业 & 能源部 (MOTIE 20173010013200 号) 的支持。

1. 制备裸玻璃、掺氟氧化锡 (SnO2: F) 基材
<ol><li>要清洁裸玻璃, 掺杂氟氧化锡 (油脂实验) 基板, 它们依次在含2% 海卫、去离子水、丙酮和异丙醇 (IPA) 的水溶液中, 每15分钟。</li>
	<li>将清洗后的基体放在加热炉的70摄氏度, 以去除残留的 IPA。</li>
</ol>2. 制备紧凑型2层 (c.2) 以阻挡电子
<ol><li>为制备2前驱体溶液, 将0.74 毫升的钛异丙醇 (TTIP) 缓慢地转?...

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我们为银-双 I 三元半导体的溶液制备提供了一个详细的协议, 这将被利用介观器件体系结构作为薄膜太阳能电池中的无铅光伏吸收器。在基板上形成了2层, 以避免电子泄漏流入该电极。在 c-2涂层的基板上依次形成了2层, 以改善光伏吸收器 (即银-双 i 薄膜) 产生的电子萃取。用 TiCl4水溶液对2和2的钝化进行了处理, 以使其2表面陷井;这?...

解决方案处理的无机薄膜太阳能电池已被许多研究人员广泛研究, 试图将阳光直接转化为电力1,2,3,4,5。随着材料合成和器件体系结构的发展, 以卤化铅为基础的 perovskites 已被报道为最好的太阳能电池吸收器, 其功率转换效率 (四氯乙烯) 大于 22%5。然而, 人们越来越担心使用有毒铅, 以及铅卤化物钙钛矿本身的稳定性问题。
最近据报道, 铋基混合 perovskites 可以通过将单价阳离子纳入碘化铋复合单元而形成, 并且这些可作为介观太阳能电池体系结构中的光伏吸收剂6, 7,8。perovskites 中的铅可以用铋代替, 它具有 6s2外孤对;然而, 到目前为止, 只有传统的卤化铅方法已用于铋基混合 perovskites 与复杂的晶体结构, 尽管事实上, 他们有不同的氧化状态和化学性质9。此外, 这些 perovskites 的表面形貌较差, 在薄膜器件应用的背景下产生相对较厚的薄膜;因此, 它们的光伏性能较差, 高频带隙能量 (> 2 eV)6,7,8。因此, 我们试图寻找一种新的方法来生产铋基薄膜半导体, 这是环境友好, 空气稳定, 并有低频段能量 (< 2 eV), 考虑到材料的设计和方法。
我们目前的解决方案处理银-双 I 三元薄膜, 可以结晶为 AgBi2I7和 Ag2BiI5, 为无铅和空气稳定半导体10,11。在本研究中, AgBi2I7的组成, 正丁胺被用作溶剂, 同时溶解银碘化物 () 和碘化铋 (BiI3) 前体。该混合物是旋转铸造和退火在150°c 30 分钟, 在一个 N2填充手套盒;随后, 薄膜被淬火到室温。所合成的薄膜呈棕黑色。此外, 银-双 I 三元体系的表面形貌和晶体组成由 BiI3的退火温度和前驱比控制。由此产生的 AgBi2I7薄膜呈现一个立方相晶体结构, 致密和平滑的表面形貌与大颗粒 200-800 nm 的大小, 和一个光带隙的 1.87 eV 开始吸收光从波长的 740 nm.最近据报道, 通过优化晶体组成和器件结构, 银双 I 三元薄膜太阳能电池可以达到4.3% 的四氯乙烯。

<table>
	<tbody>
		<tr>
			<td>Bismuth(III) iodide, Puratronic, 99.999% (metals basis)</td>
			<td>Afa Aesar</td>
			<td>7787-64-6</td>
			<td>stored in N2-filled condition</td>
		</tr>
		<tr>
			<td>Silver iodide, Premion, 99.999% (metals basis)</td>
			<td>Afa Aesar</td>
			<td>7783-96-2</td>
			<td>stored in N2-filled condition</td>
		</tr>
		<tr>
			<td>Butylamine 99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>109-73-9</td>
			<td></td>
		</tr>
		<tr>
			<td>Triton X-100</td>
			<td>Sigma-Aldrich</td>
			<td>9002-93-1</td>
			<td></td>
		</tr>
		<tr>
			<td>Isopropyl alcohol (IPA)</td>
			<td>Duksan</td>
			<td>67-63-0</td>
			<td>Electric High Purity GRADE</td>
		</tr>
		<tr>
			<td>Titanium(IV) isopropoxide</td>
			<td>Sigma-Aldrich</td>
			<td>546-68-9</td>
			<td>&#8805;97.0%</td>
		</tr>
		<tr>
			<td>Ethyl alcohol</td>
			<td>Sigma-Aldrich</td>
			<td>64-17-5</td>
			<td>200 proof, ACS reagent, &#8805;99.5%</td>
		</tr>
		<tr>
			<td>Hydrochloric acid</td>
			<td>SAMCHUN</td>
			<td>7647-01-0</td>
			<td>Extra pure</td>
		</tr>
		<tr>
			<td>Titanium tetrachloride (TiCl4)</td>
			<td>sharechem</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>50nm-sized TiO2 nanoparticle paste</td>
			<td>sharechem</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>2-propanol</td>
			<td>Sigma-Aldrich</td>
			<td>67-63-0</td>
			<td>anhydrous, 99.5%</td>
		</tr>
		<tr>
			<td>Terpineol</td>
			<td>Merck</td>
			<td>8000-41-7</td>
			<td></td>
		</tr>
		<tr>
			<td>Heating oven</td>
			<td>WiseTherm</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Oxygen (O2) plasma</td>
			<td>AHTECH</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>X-ray diffraction (XRD)</td>
			<td>Rigaku</td>
			<td></td>
			<td>Rigaku Miniflex 600 diffractometer with a NaI scintillation counter and using monochromatized Cu-K&#945; radiation 
			(1.5406 &#197; wavelength).</td>
		</tr>
		<tr>
			<td>Fourier transform infrared (FTIR)</td>
			<td>Bruker</td>
			<td></td>
			<td>Bruker Tensor 27</td>
		</tr>
		<tr>
			<td>field-emission scanning electron microscope (FE-SEM)</td>
			<td>Hitachi</td>
			<td></td>
			<td>Hitachi SU8230</td>
		</tr>
		<tr>
			<td>UV-Vis spectra</td>
			<td>PerkinElmer</td>
			<td></td>
			<td>PerkinElmer LAMBDA 950 
			Spectrophotometer</td>
		</tr>
		<tr>
			<td>Ultraviolet photoelectron spectroscopy (UPS)</td>
			<td>RBD Instruments</td>
			<td></td>
			<td>PHI5500 Multi-Technique system</td>
		</tr>
	</tbody>
</table>

solution-processed "silver-bismuth-iodine" ternary thin films for lead-free photovoltaic absorbers

铋基混合 perovskites 被认为是有前景的光活性半导体, 用于环境友好和空气稳定的太阳能电池应用。然而, 表面形貌差和相对高的带隙能量限制了它们的潜能。银铋碘 (Ag 双 I) 是一种有前途的半导体光电器件。因此, 我们用材料溶液处理的方法演示了银-双 I 三元薄膜的制备。所产生的薄膜根据其热退火温度表现出受控的表面形貌和光学 bandgaps。此外, 据报道, 银双 I 三元系统结晶为 AgBi2I7, Ag2BiI5,等等, 根据前体化学品的比例。解决方案处理的 AgBi2I7薄膜显示一个立方相晶体结构, 致密, 无针孔表面形貌, 晶粒范围从200到800毫微米, 并间接带隙的 1.87 eV。结果 AgBi2I7薄膜显示良好的空气稳定性和能量带图, 以及表面形貌和光学 bandgaps 适合无铅和空气稳定的单结太阳能电池。最近, 通过优化银双 I 晶体组合物和太阳能电池器件体系结构, 获得了4.3% 功率转换效率的太阳能电池。

据报道, 银-双 I 三元体系, 被认为是有希望的半导体, 是结晶的各种组合, 如 AgBi2I7, AgBiI4, 银2BiI510, 根据BiI3的摩尔比。早先的研究表明, 银-双 I 三元体系的各种成分的块状晶体形式可以通过改变 BiI3的摩尔比和每个组合有一个不同的 XRD 模式10来进行实验合成。
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Watch this Scientific Journal Video about Solution-Processed "Silver-Bismuth-Iodine" Ternary Thin Films for Lead-Free Photovoltaic Absorbers at JoVE.com

Solution-Processed "Silver-Bismuth-Iodine" Ternary Thin Films for Lead-Free Photovoltaic Absorbers

在此, 我们提出了解决方案处理的银铋碘 (银双 I) 三元半导体薄膜制备的2涂层透明电极的详细协议及其作为空气稳定和无铅的潜在应用光电器件。

无铅光伏吸收剂的溶液处理 "银铋碘" 三元薄膜

Bismuth-based hybrid perovskites are regarded as promising photo-active semiconductors for environment-friendly and air-stable solar cell applications. ...

此方法可以帮助您回答有关如何为环保薄膜太阳能电池制造溶液可加工银-双碘三元半导体并采用应用等关键问题。该技术的主要优点是银-双碘溶液制造，然后用作薄膜太阳能电池中的无铅光伏吸收器，具有显微装置结构。该技术在生产环保薄膜太阳能电池方面具有潜在的应用潜力，因为银-二碘三元半导体是无铅、空气稳定的光伏吸收器。要开始为紧凑型二氧化钛层制备前体溶液，请将8毫升无水乙醇放在20毫升玻璃瓶中，然后开始大力搅拌。在搅拌乙醇滴中加入0.74毫升的异丙酰胺钛。然后迅速加入0.06毫升的浓缩盐酸。在室温下搅拌混合物12至24小时，形成前体溶液。接下来，用2%水性八氧醇-9、丙酮和异丙醇，对裸露的一英寸一英寸的FTO基板进行15分钟的声波处理。在70摄氏度的烤箱中干燥干净的基材一小时，让它在空气中冷却到室温。然后，将基板固定到旋转涂布夹上。用紧凑型二氧化钛层前体溶液填充 1 毫升或 3 毫升注射器，并连接 0.2 纳米注射器过滤器。将溶液过滤成小瓶。将过滤前体溶液的200微升涂在基材上，以完全覆盖基材。以 3000 RPM 的速度旋转基材 30 秒。在500摄氏度的烤箱中将薄膜放入一小时。然后关闭热量，让基板在空气中冷却到室温，这通常需要大约六个小时。接下来，将涂层基材浸入四氯化钛水性0.12摩尔溶液中。将基板浸泡在70摄氏度的烤箱中30分钟。之后，在去离子水中彻底冲洗基材，以去除残留的四氯化钛。将薄膜在500摄氏度下退去一小时，然后让薄膜冷却到空气中的室温。冷却后，将紧凑型二氧化钛涂层基板存放在氮气下，供以后使用。在5毫升玻璃瓶中开始制备中孔二氧化钛纳米颗粒层的前体溶液，将0.5克50纳米二氧化钛纳米颗粒膏与1.75克异丙醇和0.5克三氯苯酚混合。加入搅拌棒到小瓶中搅拌，直到糊状物完全溶解。这通常需要大约一个小时。接下来，在旋转涂布器上固定一个紧凑的二氧化钛涂层 FTO 基板，并在基板表面应用 200 微升的纳米颗粒溶液。以 5000 RPM 的速度旋转基材 30 秒。将涂层的基板在500摄氏度的烤箱中退去一小时，并允许其冷却至室温。然后在70摄氏度下将基板浸泡在水性0.12摩尔四氯化钛溶液中30分钟。用去电化水彻底冲洗基材。在500摄氏度下摄氏一小时，让它冷却到空气中的室温。将涂有紧凑和中孔二氧化钛层的基材存放在氮气下，供以后使用。开始制备银碘二溴二苯醚、银二比二甲酸酯薄膜，在低湿度下充满氮的手套箱中，结合0.3克二氧化二氮-三碘化物、0.06克碘化银和3毫升氮丁胺。大力涡旋混合物，直到固体大部分溶解，然后注射器通过0.2微米聚四氟乙烯过滤器过滤前体溶液。接下来，将所需的基板固定到旋转涂布器上，并应用过滤前体溶液的 200 微升。以 6000 RPM 的速度旋转基材 30 秒。将基板放在热板上，加热至 150 摄氏度。在该温度下将薄膜退去 30 分钟，然后快速将其从热板中取出以淬火。在充满氮气的手套箱中，将10毫克P3HT和1毫升氯苯混合。在 50 摄氏度下搅拌混合物 30 分钟，完全溶解 P3HT，然后用 0.2 微米 PTFE 注射器过滤器过滤混合物。接下来，在旋转涂布器上固定涂有银二比二氧化钛的 FTO 基板。将 100 微升的 P3HT 溶液涂抹到基材上，并在 4000 RPM 或 30 秒时旋转涂层基材。将 P3HT 薄膜放在热板上，预热至 130 摄氏度，10 分钟。让基板冷却到手套箱中的室温。最后，使用热蒸发器以0.5微秒的速度在基板上沉积100纳米的黄金，形成太阳能电池的顶级金接触。用这种方法制造了碘化银与二丁三丁的银-二丁-碘三层薄膜，1：2、1：1和2：1摩尔银比。1：2的影片显示了一个约42度的峰值，与一个立方结构有关。1：1 和 2：1 的胶片观察到峰分裂，表示六边形结构。1：2胶片吸收的波长比2：1胶片长。此外，1：2薄膜表面光滑，颗粒较大，而在2：1薄膜上观察到多余碘化银颗粒。因此，1：2电影被选定作进一步研究。X射线衍射表明，1：2薄膜在立方相完全结晶需要150摄氏度的退火温度。这部电影在空中稳定了至少10天。FTIR光谱表明，残留的n-丁胺在较低的退火温度下仍然与二氧化二丁和碘化银的微弱复杂，抑制了银-二丁胺-碘基块的形成。随着退火温度的升高，谷物变得更大，包装更密集。在150摄氏度下退火的薄膜也具有最适合用于太阳能电池的吸收特性。总体而言，在150摄氏度下退火的银二比质六溴二氮薄膜显示出适合太阳能电池使用的能量特性。这项技术为可溶液处理薄膜太阳能电池的研究人员铺平了道路，以进一步开发银-二碘三元半导体在无铅和空气稳定薄膜太阳能电池等应用中的方法。在尝试此程序时，您可能希望使用低于 20% 的受控湿度，使用银-双碘前体溶液对基材进行旋转涂层。如果在湿度达到或超过 30% 的湿度下旋转涂层前体溶液，则由于高度反应和照片而看到黄色，如果您无法控制旋转涂层中的湿度，您可以在 N 填充手套箱中旋转前体溶液。但是，请记住，您必须在手套箱完成后完全清除手套箱。

Research

JoVE Journal

Chemistry

Towards Biomimicking Wood: Fabricated Free-standing Films of Nanocellulose, Lignin, and a Synthetic Polycation

朝仿生学木：纳米纤维素，木质素的装配式自由站立电影和合成聚阳离子

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and ...

科研

化学

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 ...

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 ...

Construction and Systematical Symmetric Studies of a Series of Supramolecular Clusters with Binary or Ternary Ammonium Triphenylacetates

建筑和超分子集群与二元或三元铵Triphenylacetates一系列的体制性对称研究

Functions of clusters in nano or sub-nano scale significantly depend on not only kinds of their components but also arrangements, or symmetry, of their ...

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 ...

Capillary Electrophoresis to Monitor Peptide Grafting onto Chitosan Films in Real Time

毛细管电泳监视肽接枝壳聚糖膜实时

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. ...

Low Pressure Vapor-assisted Solution Process for Tunable Band Gap Pinhole-free Methylammonium Lead Halide Perovskite Films

可调谐带隙无针孔 Methylammonium 铅卤化物钙钛矿薄膜的低压蒸气辅助解决工艺

Organo-lead halide perovskites have recently attracted great interest for potential applications in thin-film photovoltaics and optoelectronics. Herein, ...

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. ...

Chemical Synthesis of Porous Barium Titanate Thin Film and Thermal Stabilization of Ferroelectric Phase by Porosity-Induced Strain

孔隙诱导应变法合成多孔钛酸钡薄膜及铁电相热稳定性

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its ...

Inkjet Printing All Inorganic Halide Perovskite Inks for Photovoltaic Applications

用于光伏应用的喷墨打印所有无机舱齐德 perovskite 油墨

A method for synthesizing photoactive inorganic&#160;perovskite quantum dot inks and an inkjet printer deposition method, using the synthesized inks, are ...