Name: graphene-assisted quasi-van der waals epitaxy of aln film on nano-patterned sapphire substrate for ultraviolet light emitting diodes
Uploaded: 2020-06-25T12:30:00
Description: Watch this Scientific Journal Video about Graphene-Assisted Quasi-van der Waals Epitaxy of AlN Film on Nano-Patterned Sapphire Substrate for Ultraviolet Light Emitting Diodes at JoVE.com

这项工作得到了中国国家重点研发计划（2018YFB0406703）、中国自然科学基金（61474109、61527814、11474274、6142791）和北京自然科学基金（第4182063号）的财政支持。

注意：这些方法中使用的几种化学物质具有剧毒和致癌性。使用前请查阅所有相关材料安全数据表 （MSDS）。
1. 纳米印刷光刻（NIL）编制NPSS
<ol><li>SiO2 薄膜的沉积<ol>
<li>用乙醇清洗2英寸C平面蓝宝石基板，然后用去电化水三次。</li>
		<li>用氮气枪擦干基材。</li>
		<li>在300°C下通过等离子体增强化学气相沉积（PECVD）将200纳米SiO2薄膜沉积在扁平蓝宝石基材上。?...

<ol>
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R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Defect+and+Stress+Characterization+of+AlN+Films+by+Raman+Spectroscopy.">Defect and Stress Characterization of AlN Films by Raman Spectroscopy.</a> Appllied Physics Letters. 89, 2653 (2006).</li><li>Li, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Van+der+Waals+epitaxy+of+GaN-based+light-emitting+diodes+on+wet-transferred+multilayer+graphene+film.">Van der Waals epitaxy of GaN-based light-emitting diodes on wet-transferred multilayer graphene film.</a> Jappanese Journal of Applied Physics. 56, 085506 (2017).</li><li>Chang, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Graphene-assisted+quasi-van+der+Waals+epitaxy+of+AlN+film+for+ultraviolet+light+emitting+diodes+on+nano-patterned+sapphire+substrate.">Graphene-assisted quasi-van der Waals epitaxy of AlN film for ultraviolet light emitting diodes on nano-patterned sapphire substrate.</a> Applled Physics Letters. 114, 091107 (2019).</li></ol>

如图1 Figure 1A所示，NIL 技术制备的 NPSS 说明了具有 400 nm 深度、1 μm 图案周期和 300 nm 宽度的纳米凹锥形图案。在石墨烯层的APCVD生长之后，图1B显示了石墨烯-NPSS。B拉曼光谱图1C中N等离子体处理石墨烯的D峰显著增加，表明在RIE工艺16期间产生的悬垂键增加。在AlN直接MOCVD增长...

AlN和AlGaN是DUI-LED1、2,中最重要的材料，广泛应用于灭菌、聚合物固化、生化检测、非视线通信、特殊照明3等领域。由于缺乏内在基材，MOCVD蓝宝石基材上的AlN异质基已成为最常见的技术路线4。然而，AlN和蓝宝石基板之间的大晶格不匹配会导致应力积累5,5、6、高密度错位和堆叠故障7。因此，LED的内部量子效率降低了8。近几十年来，人们提出使用图案蓝宝石作为基材（PSS）来诱导AlN外延性横向过度生长（ELO）来解决这个问题。此外，AlN模板,,9、10、11的成长9也取得了很大进展。然而，由于表面粘附系数高，粘附能高（AlN为2.88 eV），Al原子表面流动性低，AlN的生长往往具有三维岛生长模式12。因此，NPSS 上的 AlN 薄膜的外延生长是困难的，并且需要比平蓝宝石基材更高的粘结厚度（超过 3 μm），这会导致更长的生长时间，并且需要高成本 9。
最近，石墨烯显示出巨大的潜力，用于作为一个缓冲层作为AlN增长，由于其六边排列的sp2杂交碳原子13。此外，AlN的准范德瓦尔斯外延（QvdWE）可以减少不匹配效应，并为AlN生长14，15,铺平了一条新路。为了增加石墨烯的化学反应性，陈等人使用N 2等离子体处理石墨烯作为缓冲层，确定了优质AlN和GaN膜8的QvdWE，证明了石墨烯作为缓冲层的利用。
结合N2等离子处理石墨烯技术与商用NPSS基板，该协议提出了一种在石墨烯-NPSS基材上快速生长和合并AlN的新方法。石墨烯-NPSS上AlN的完全合并厚度确认小于1μm，外延AlN层具有高质量和释放应力。该方法为AlN模板批量生产铺平了一条新路，在基于AlGaN的DUILED的应用上显示出了巨大的潜力。

<table>
	<tbody>
		<tr>
			<td>Acetone,99.5%</td>
			<td>Bei Jing Tong Guang Fine Chemicals company</td>
			<td>1090</td>
			<td></td>
		</tr>
		<tr>
			<td>APCVD</td>
			<td>Linderberg</td>
			<td>Blue M</td>
			<td></td>
		</tr>
		<tr>
			<td>EB</td>
			<td>AST</td>
			<td>Peva-600E</td>
			<td></td>
		</tr>
		<tr>
			<td>Ethonal,99.7%</td>
			<td>Bei Jing Tong Guang Fine Chemicals company</td>
			<td>1170</td>
			<td></td>
		</tr>
		<tr>
			<td>HF,40%</td>
			<td>Beijing Chemical Works</td>
			<td>1789</td>
			<td></td>
		</tr>
		<tr>
			<td>ICP-RIE</td>
			<td>AST</td>
			<td>Cirie-200</td>
			<td></td>
		</tr>
		<tr>
			<td>MOCVD</td>
			<td>VEECO</td>
			<td>P125</td>
			<td></td>
		</tr>
		<tr>
			<td>PECVD</td>
			<td>Oerlikon</td>
			<td>790+</td>
			<td></td>
		</tr>
		<tr>
			<td>Phosphate,85%</td>
			<td>Beijing Chemical Works</td>
			<td>1805</td>
			<td></td>
		</tr>
		<tr>
			<td>Sulfuric acid,98%</td>
			<td>Beijing Chemical Works</td>
			<td>10343</td>
			<td></td>
		</tr>
	</tbody>
</table>

graphene-assisted quasi-van der waals epitaxy of aln film on nano-patterned sapphire substrate for ultraviolet light emitting diodes

该协议演示了一种在纳米片形蓝宝石基材 （NPSS） 上采用石墨烯辅助快速生长和粘聚 AlN 的方法。使用无催化剂的大气压力化学气相沉积 （APCVD） 直接在 NPSS 上生长石墨烯层。通过应用氮反应离子蚀刻（RIE）等离子体处理，在石墨烯薄膜中引入缺陷，以提高化学反应性。在AlN的金属-有机化学气相沉积（MOCVD）生长过程中，这种N等离子体处理石墨烯缓冲液使AlN能够快速生长，NPSS上的聚化通过横截面扫描电子显微镜（SEM）得到确认。然后，通过 X 射线摇摆曲线 （XRCs） 评估石墨烯-NPSS 上的高质量，在半最大值 （FWHM） 下，全宽为 267.2 弧秒和 503.4 弧秒。与裸 NPSS 相比，石墨烯-NPS 上的 AlN 增长显示，根据拉曼测量，残余应力从 0.87 GPa 显著减小到 0.25 Gpa。其次是AlGaN多量子井（MQWS）在石墨烯-NPSS上的生长，基于AlGaN的深紫外发光二极管（DUV LED）被制造出来。制造的 DUV LED 还表现出明显的增强发光性能。这项工作为高品质 AlN 的生长和高性能 DUV LED 的制造提供了新的解决方案，使用更短的工艺和更少的成本。

为外延AlN薄膜（图1，图2）和基于AlGaN的DUV-LED（图3）采集了扫描电子显微镜（SEM）图像、X射线衍射摇摆曲线（XRC）、拉曼光谱、透射电子显微镜（TEM）图像和电致发光（EL）光谱。SEM 和 TEM 用于确定石墨烯-NPSS 上的 AlN 形态。XRD 和拉曼用于计算错位密度和残余应力。EL 用于说明制造的 DUV LED 的照明。
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Watch this Scientific Journal Video about Graphene-Assisted Quasi-van der Waals Epitaxy of AlN Film on Nano-Patterned Sapphire Substrate for Ultraviolet Light Emitting Diodes at JoVE.com

Graphene-Assisted Quasi-van der Waals Epitaxy of AlN Film on Nano-Patterned Sapphire Substrate for Ultraviolet Light Emitting Diodes

提出了一种在纳米图案蓝宝石基材上生产高质量AlN薄膜的石墨烯辅助生长方案。

紫外发光二极管纳米图案蓝宝石基板的AlN薄膜的石墨烯辅助准范德瓦尔斯皮Taxy

This protocol demonstrates a method for graphene-assisted quick growth and coalescence of AlN on nano-pattened sapphire substrate (NPSS). Graphene layers ...

这种用于纳米图案蓝宝石基板和石墨烯层快速生长的亚硝酸盐新协议可用于快速、廉价地生成高性能深紫外 LED。以二鳗石墨烯为氮化铝模板，显示了铝、亚硝酸氧化铝应用的增长潜力。首先，用丙酮、乙醇和去压水冲洗NPSS三次。用氮枪擦干核动力源。将 NPSS 加载到三区高温炉中，具有长平的温度区。将炉子加热到1050摄氏度。将温度稳定在每分钟500标准立方厘米和每分钟300标准立方厘米的氢气分之一下下10分钟。然后将每分钟30个标准立方厘米的甲烷引入反应室，使NPSS上的石墨烯生长3小时。在生长反应结束时，关闭甲烷，让NPSS自然冷却。用去电化水冲洗冷却的基材。用氮枪擦干核动力源。然后，用氮等离子体蚀刻石墨烯NPSS，氮流速为每分钟300标准立方厘米，30秒。和50瓦的功率在无功离子蚀刻室。对于石墨烯 NPSS 上的 MOCVD 铝氮生长，编辑 MOCVD 铝氮生长配方。将石墨烯 NPSS 及其 NPSS 对应物装入自制的 MOCVD 腔室。加热12分钟后，温度将稳定在1200摄氏度。然后引入每分钟7000个标准立方厘米的氢气作为环境。每分钟 70 标准立方厘米三甲基铝。每分钟500标准立方厘米氨气两小时。根据手稿指示，继续进行铝氦氮量子井的MOCVD生长。完成后，将腔室温度降至800摄氏度，用氮气将P型层跪下20分钟。对于基于深紫外 LED 的铝氦氮制造，将光抗 4620 旋转到晶圆上，并执行光刻，具有 8 秒的紫外线照射、30 秒的开发时间和 2 分钟的冲洗时间。对于P-加仑氮的电感耦合等离子蚀刻，将蚀刻功率设置为450瓦，将蚀刻压力设置为4毫角，将蚀刻速率设置为5.6纳米/秒。将蚀刻样品放入80摄氏度的丙酮中5分钟。其次是用乙醇和去水清洗。旋转负光抗 NR9 和光刻，紫外线照射时间 12 秒，开发时间 20 秒，冲洗时间 2 分钟。用丙酮、乙醇和去维水清洗样品三次。并沉积钛铝钛金通过电子束蒸发。在相同设置下旋转负光电阻 NR9 和光刻。用丙酮、乙醇和去维化水洗三次，无需超声波。通过电子束蒸发沉积镍金。用乙醇和去水洗样品三次。在300摄氏度的沉积温度和每分钟100纳米的沉积速率下，通过等离子体增强的化学气相沉积沉积300纳米的二氧化硅。在紫外线照射时间8秒时旋转光抗304和光刻，开发时间为1分钟，冲洗时间为2分钟，然后将晶圆浸入23%的氢氟酸中15秒。用乙醇和去维水清洗样品三次。用氮枪擦干晶圆。以NR9为证明的光刻后，通过电子束蒸发沉积铝钛金。用乙醇和去维水洗样品三次。经过最后一次洗磨，通过机械抛光将蓝宝石抛光至130微米。用脱蜡溶液和去维化水清洗样品。然后使用激光将整个晶圆切成0.5由0.5毫米的器件片。并使用机械骰子将晶圆切成芯片。扫描和传输电子显微镜成像可用于确定石墨烯和NPSS铝氮的形态。拉面可用于计算错位密度和残余应力。电致发光用于说明制造的深度紫外线 LED 的照明。请记住，每次新修改之前，晶圆必须清洁。因此，在每一步之前彻底冲洗晶圆至关重要。

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A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex ...

A Fabrication and Measurement Method for a Flexible Ferroelectric Element Based on Van Der Waals Heteroepitaxy

基于范德华 Heteroepitaxy 的柔性铁电元件制备及测量方法

Flexible non-volatile memories have received much attention as they are applicable for portable smart electronic device in the future, relying on ...

Enhanced Electron Injection and Exciton Confinement for Pure Blue Quantum-Dot Light-Emitting Diodes by Introducing Partially Oxidized Aluminum Cathode

采用部分氧化铝阴极增强电子注入和激子约束的纯蓝色量子点发光二极管

Stable and efficient red (R), green (G), and blue (B) light sources based on solution-processed quantum dots (QDs) play important roles in next-generation ...

Film Control to Study Contributions of Waves to Droplet Impact Dynamics on Thin Flowing Liquid Films

薄膜控制研究波浪对液滴冲击动力学的影响薄流动液体薄膜

Droplet impact is a very common phenomenon in nature and attracts attention due to its aesthetic fascination and wide-ranging applications. Previous ...

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

矿物和岩石样品的同步辐射 x 射线 Microdiffraction 和荧光成像

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder ...

Fabrication of Schottky Diodes on Zn-polar BeMgZnO/ZnO Heterostructure Grown by Plasma-assisted Molecular Beam Epitaxy

等离子体辅助分子束外延法制备的锌极性 BeMgZnO/氧化锌异质结构肖特基二极管的制备

Heterostructure field effect transistors (HFETs) utilizing a two dimensional electron gas (2DEG) channel have a great potential for high speed device ...

Measurement of Dynamic Force Acted on Water Strider Leg Jumping Upward by the PVDF Film Sensor

PVDF 薄膜传感器对水黾腿跳起动力的测量

This study aimed to make an explanation for the phenomenon in nature that water strider usually jumps or glides on the water surface easily but quickly, ...